阅读说明：本技术 基于研磨补偿介质的热敏性原药研磨方法和农药制剂 (Grinding compensation medium-based thermosensitive original medicine grinding method and pesticide preparation ) 是由 谭葵 石伟贤 王爱臣 廖联安 于 2021-07-27 设计创作，主要内容包括：本申请提供一种基于研磨补偿介质的热敏性原药研磨方法和农药制剂。上述的基于研磨补偿介质的热敏性原药研磨方法包括如下步骤：获取研磨介质和钛白粉研磨补偿介质,其中,所述钛白粉研磨补偿介质为纳米级颗粒；将钛白粉研磨补偿介质和热敏性原药进行混合操作,得到待研磨混合物；对所述待研磨混合物和所述研磨介质投入研磨机中进行研磨操作,得到热敏性原药研磨物。上述的基于研磨补偿介质的热敏性原药研磨方法能有效减少研磨过程中原药发热以确保原药的研磨速度,进而提高农药制剂生产效率和降低生产成本。(The application provides a thermosensitive original drug grinding method based on grinding compensation media and a pesticide preparation. The grinding compensation medium-based thermosensitive original medicine grinding method comprises the following steps: obtaining a grinding medium and a titanium dioxide grinding compensation medium, wherein the titanium dioxide grinding compensation medium is nano-scale particles; mixing the titanium dioxide grinding compensation medium and the thermosensitive original medicine to obtain a mixture to be ground; and putting the mixture to be ground and the grinding medium into a grinding machine for grinding operation to obtain the thermosensitive original drug ground product. The grinding compensation medium-based thermosensitive original drug grinding method can effectively reduce the heating of the original drug in the grinding process so as to ensure the grinding speed of the original drug, thereby improving the production efficiency of the pesticide preparation and reducing the production cost.)

1. A grinding compensation medium-based thermosensitive original medicine grinding method is characterized by comprising the following steps:

obtaining a grinding medium and a titanium dioxide grinding compensation medium, wherein the titanium dioxide grinding compensation medium is nano-scale particles;

mixing the titanium dioxide grinding compensation medium and the thermosensitive original medicine to obtain a mixture to be ground;

and putting the mixture to be ground and the grinding medium into a grinding machine for grinding operation to obtain the thermosensitive original drug ground product.

2. The grinding compensation medium-based heat-sensitive technical grinding method according to claim 1, wherein before the step of feeding the mixture to be ground and the grinding medium into a grinding mill for a grinding operation and after the step of mixing the titanium dioxide grinding compensation medium and the heat-sensitive technical, the grinding compensation medium-based heat-sensitive technical grinding method further comprises the steps of:

adding a dispersion medium and a dispersant to the mixture to be milled.

3. The grinding compensation medium-based heat-sensitive bulk drug grinding method of claim 2, wherein prior to the step of feeding the mixture to be ground and the grinding medium into a grinding mill for a grinding operation, and after the step of adding a dispersion medium and a dispersant to the mixture to be ground, the grinding compensation medium-based heat-sensitive bulk drug grinding method further comprises the steps of:

a wetting or emulsifying agent is added to the mixture to be milled.

4. The method of grinding a thermally sensitive technical material based on grinding compensation media of claim 1 wherein the titanium dioxide grinding compensation media has a D50 of 0.5 to 1 μ ι η.

5. The grinding compensation medium-based thermosensitive bulk drug grinding method according to claim 1, wherein the addition amount of the titanium dioxide grinding compensation medium is greater than or equal to 3% of the total mass of the thermosensitive bulk drug.

6. The grinding compensation medium-based thermosensitive bulk drug grinding method according to claim 1, wherein the thermosensitive bulk drug is at least one of pyraclostrobin, metiram, difenoconazole, trifloxystrobin and glyphosate.

7. The method of grinding a thermally sensitive bulk drug based on a grinding compensation medium of claim 1, wherein the fill rate of the grinding medium is between 60% and 75%.

8. The method of grinding a heat sensitive bulk drug based on grinding compensation media of claim 1 wherein the grinding media comprises a first ellipsoidal sphere and a second ellipsoidal sphere, the first ellipsoidal sphere having a volume greater than the volume of the second ellipsoidal sphere.

9. The method of grinding a thermally sensitive bulk drug based on a grinding compensation medium of claim 1, wherein the grinding medium has a particle size of 0.3mm to 2.0 mm.

10. A pesticidal preparation comprising the heat-sensitive raw drug milled product obtained by the heat-sensitive raw drug milling method based on a milling compensation medium according to any one of claims 1 to 9.

Technical Field

The invention relates to the technical field of pesticide preparation processing, in particular to a thermosensitive original pesticide grinding method based on grinding compensation media and a pesticide preparation.

Background

In the pesticide preparation, a plurality of dosage forms at least need to grind raw drug particles to 1-5 mu m by a sand mill, such as suspending agent, dry suspending agent, dispersible oil suspending agent and the like, the adding amount of grinding medium zirconia beads in the sand mill and the grinding speed of the sand mill are key factors influencing the grinding efficiency of the sand mill, if the adding amount of the grinding medium zirconia beads is larger or the grinding speed of the sand mill is higher, the materials are ground to generate heat, and when the temperature of the raw medicine particles is overhigh during grinding, the raw medicine can be changed in quality or agglomerated, further affects the quality of the pesticide product, if the addition amount of the zirconium oxide beads as the grinding medium is small or the grinding speed of the sand mill is slow, the grinding efficiency of the raw pesticide is affected, further reducing the production efficiency of the pesticide preparation, and greatly improving the production cost of the pesticide preparation by the long-time operation of the equipment.

Disclosure of Invention

The invention aims to overcome the defects in the prior art and provide a thermosensitive original drug grinding method based on a grinding compensation medium and a pesticide preparation, wherein the thermosensitive original drug grinding method can effectively reduce the heat of original drugs in the grinding process so as to ensure the grinding speed of the original drugs, further improve the production efficiency of the pesticide preparation and reduce the production cost.

The purpose of the invention is realized by the following technical scheme:

a grinding compensation medium-based thermosensitive original medicine grinding method comprises the following steps:

obtaining a grinding medium and a titanium dioxide grinding compensation medium, wherein the titanium dioxide grinding compensation medium is nano-scale particles;

mixing the titanium dioxide grinding compensation medium and the thermosensitive original medicine to obtain a mixture to be ground;

and putting the mixture to be ground and the grinding medium into a grinding machine for grinding operation to obtain the thermosensitive original drug ground product.

In one embodiment, before the step of feeding the mixture to be milled and the milling media into a milling machine for milling operation, and after the step of mixing the titanium dioxide milling compensation media and the heat-sensitive technical, the method for milling heat-sensitive technical based on milling compensation media further comprises the following steps:

adding a dispersion medium and a dispersant to the mixture to be milled.

In one embodiment, before the step of feeding the mixture to be milled and the milling media into a mill for milling operation, and after the step of adding a dispersion medium and a dispersant to the mixture to be milled, the method for milling a thermosensitive bulk drug based on a milling compensation medium further comprises the steps of:

a wetting or emulsifying agent is added to the mixture to be milled.

In one embodiment, the D50 of the titanium dioxide grinding compensation medium is 0.5-1 μm.

In one embodiment, the addition amount of the titanium dioxide grinding compensation medium is greater than or equal to 3% of the total mass of the heat-sensitive raw pesticide.

In one embodiment, the bulk drug thermo-sensitive compound is at least one of pyraclostrobin, metiram, difenoconazole, trifloxystrobin and glyphosate.

In one embodiment, the grinding media has a fill rate of 60% to 75%.

In one embodiment, the grinding media comprises a first ellipsoidal sphere and a second ellipsoidal sphere, the first ellipsoidal sphere having a volume greater than the volume of the second ellipsoidal sphere.

In one embodiment, the grinding media have a particle size of 0.3mm to 2.0 mm.

A pesticide formulation comprising a heat-sensitive bulk grind obtained by the heat-sensitive bulk grind method based on a grind-compensating medium of any of the above embodiments.

Compared with the prior art, the invention has at least the following advantages:

1. in the grinding method of the thermosensitive original drug based on the grinding compensation medium, the titanium dioxide grinding compensation medium is nano-scale particles, so that the contact area between the grinding medium and the thermosensitive original drug is greatly increased, and further when the titanium dioxide grinding compensation medium is matched with the grinding medium to grind the thermosensitive original drug, the grinding medium directly impacts the thermosensitive original drug in the process of impacting and crushing the thermosensitive original drug by the grinding medium, and an impact force is given to the titanium dioxide grinding compensation medium when impacting the thermosensitive original drug, so that the grinding compensation medium further impacts the thermosensitive titanium dioxide, the impact frequency of the thermosensitive original drug is effectively improved, and the grinding speed of the thermosensitive original drug is accelerated; in addition, in the process that the grinding medium and the titanium dioxide grinding compensation medium flow, the grinding medium extrudes and grinds the heat-sensitive raw pesticide, and simultaneously, the titanium dioxide grinding compensation medium further extrudes and grinds the heat-sensitive raw pesticide, so that the extrusion and grinding friction force of the heat-sensitive raw pesticide is effectively increased, the grinding speed of the heat-sensitive raw pesticide is further accelerated, the temperature rise degree of the heat-sensitive raw pesticide is smaller when the heat-sensitive raw pesticide is crushed to the required grain diameter, namely when the temperature of the heat-sensitive raw pesticide is at a lower temperature, the heat-sensitive raw pesticide is crushed to the required grain diameter, the problem that the raw pesticide is changed or agglomerated when the addition amount of zirconium oxide beads of the grinding medium is larger or the grinding speed of a sand mill is higher, the material is ground and heated to the high temperature of raw pesticide particles is solved, the quality of the pesticide product is further influenced, the problem that the grinding efficiency of the original pesticide is influenced if the adding amount of the grinding medium zirconia beads is small or the grinding speed of a sand mill is slow is solved, the production efficiency of the pesticide preparation is further reduced, the production cost of the pesticide preparation is greatly improved due to the long-time operation of equipment, the grinding speed of the thermosensitive original pesticide is further improved, and the quality change or agglomeration of the thermosensitive original pesticide is reduced;

2. in the heat-sensitive original medicine grinding method based on the grinding compensation medium, the titanium dioxide grinding compensation medium is used as the filler, so that the titanium dioxide is not required to be separated when the titanium dioxide grinding compensation medium is used for a pesticide preparation, the preparation procedures of the pesticide preparation are reduced, and the production efficiency of the pesticide preparation is improved;

3. in the heat-sensitive raw pesticide grinding method based on the grinding compensation medium, the titanium dioxide grinding compensation medium has high thermal stability, hydrophilicity, weaker hygroscopicity and viscosity, and can be well dispersed on the peripheral surface of the heat-sensitive raw pesticide, so that the heat stability of the heat-sensitive raw pesticide is improved, the quality change or agglomeration of the heat-sensitive raw pesticide is reduced, the hydrophilicity of the heat-sensitive raw pesticide is improved, and the pesticide effect of a pesticide preparation is improved.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.

Fig. 1 is a flow chart of a method for grinding a heat-sensitive bulk drug based on a grinding compensation medium according to an embodiment of the present invention;

figure 2 is a graph of the exit temperature of the heat sensitive raw drug grind of example 17 and comparative example 5.

Detailed Description

To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.

It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

The application provides a thermosensitive original drug grinding method based on grinding compensation media. The grinding compensation medium-based thermosensitive original medicine grinding method comprises the following steps: obtaining a grinding medium and a titanium dioxide grinding compensation medium, wherein the titanium dioxide grinding compensation medium is nano-scale particles; mixing the titanium dioxide grinding compensation medium and the thermosensitive original medicine to obtain a mixture to be ground; and putting the mixture to be ground and the grinding medium into a grinder for grinding operation to obtain the heat-sensitive original drug ground substance.

In the method for grinding the thermosensitive original drug based on the grinding compensation medium, the titanium dioxide grinding compensation medium is nano-scale particles, so that the contact area between the grinding medium and the thermosensitive original drug is greatly increased, when the titanium dioxide grinding compensation medium is matched with the grinding medium to grind the thermosensitive original drug, the grinding medium directly impacts the thermosensitive original drug in the process of impacting and crushing the thermosensitive original drug by the falling grinding medium, and an impact force is given to the titanium dioxide grinding compensation medium when impacting the thermosensitive original drug, so that the titanium dioxide grinding compensation medium further impacts the thermosensitive original drug, the impact frequency of the thermosensitive original drug is effectively improved, and the grinding speed of the thermosensitive original drug is accelerated; in addition, in the process that the grinding medium and the titanium dioxide grinding compensation medium flow, the grinding medium extrudes and grinds the heat-sensitive raw pesticide, and simultaneously, the titanium dioxide grinding compensation medium further extrudes and grinds the heat-sensitive raw pesticide, so that the extrusion and grinding friction force of the heat-sensitive raw pesticide is effectively increased, the grinding speed of the heat-sensitive raw pesticide is further accelerated, the temperature rise degree of the heat-sensitive raw pesticide is smaller when the heat-sensitive raw pesticide is crushed to the required grain diameter, namely when the temperature of the heat-sensitive raw pesticide is at a lower temperature, the heat-sensitive raw pesticide is crushed to the required grain diameter, the problem that the raw pesticide is changed or agglomerated when the addition amount of zirconium oxide beads of the grinding medium is larger or the grinding speed of a sand mill is higher, the material is ground and heated to the high temperature of raw pesticide particles is solved, further influencing the quality of pesticide products, and reducing the problems that the grinding efficiency of the raw pesticide can be influenced if the adding amount of the grinding medium zirconia beads is small or the grinding speed of a sand mill is slow, further reducing the production efficiency of the pesticide preparation, greatly improving the production cost of the pesticide preparation due to the long-time operation of equipment, further improving the grinding speed of the thermosensitive raw pesticide and reducing the quality change or agglomeration of the thermosensitive raw pesticide. Because the titanium dioxide grinding compensation medium is used as the filler, the titanium dioxide is not required to be separated when the titanium dioxide grinding compensation medium is used for the pesticide preparation, the preparation procedures of the pesticide preparation are reduced, and the production efficiency of the pesticide preparation is improved. The titanium dioxide grinding compensation medium has high thermal stability and hydrophilicity, but has weak hygroscopicity and viscosity, and can be well dispersed on the peripheral surface of the thermosensitive original drug, so that the thermal stability of the thermosensitive original drug is improved, the quality change or agglomeration of the thermosensitive original drug is reduced, the hydrophilicity of the thermosensitive original drug is improved, and the pesticide effect of the pesticide preparation is improved.

It should be noted that, the heat-sensitive raw drug is subjected to impact grinding by using the grinding medium, if the volume of the grinding medium is small, the mass is not enough to break the heat-sensitive raw drug, so that the grinding medium is required to reach a certain mass, that is, the grinding medium reaches a certain volume, and in order to increase the fluidity of the grinding medium, the edges and corners of the grinding medium are generally required to be trimmed, that is, the general grinding medium is spherical, so that more gaps exist between the grinding media, and the contact area between the grinding medium and the heat-sensitive raw drug is small, therefore, if only the grinding medium is used to perform impact grinding on the heat-sensitive raw drug, the heat-sensitive raw drug with a larger volume is preferentially subjected to impact grinding by the grinding medium, and along with the gradual reduction of the particle size of the heat-sensitive raw drug, the impact grinding strength between the heat-sensitive raw drug with a smaller particle size and the grinding medium is gradually increased, the time for crushing the thermosensitive original drug to the required particle size is greatly increased, the temperature of the thermosensitive original drug is continuously increased, and the thermosensitive original drug is further changed in quality or agglomerated to a greater extent.

It should be further noted that if the grinding compensation medium is nanoscale steel balls, zirconium dioxide beads or ceramic beads, the separation of the grinding compensation medium from the ground heat-sensitive raw pesticide is required, and since the grinding compensation medium is nanoscale particles, the separation is troublesome and time-consuming, and the preparation difficulty of the nanoscale steel balls, zirconium dioxide beads or ceramic beads is high, the preparation time and difficulty of the pesticide preparation are increased, and the preparation efficiency of the pesticide preparation is reduced, therefore, in the present application, the nanoscale titanium dioxide is used as the grinding compensation medium, which not only effectively increases the grinding speed of the heat-sensitive raw pesticide, but also avoids the separation of the grinding compensation medium from the ground heat-sensitive raw pesticide, and since the grinding compensation medium is nanoscale particles, the separation is troublesome and time-consuming, and the preparation difficulty of the nanoscale steel balls, zirconium dioxide beads or ceramic beads is high, the preparation time and difficulty of the pesticide preparation are increased, the problem of preparation efficiency of the pesticide preparation is reduced, and the preparation efficiency of the pesticide preparation is effectively improved; in addition, the titanium dioxide has high thermal stability and hydrophilicity, but has weak hygroscopicity and viscosity, and can be well dispersed on the peripheral surface of the thermosensitive original drug, so that the thermal stability of the thermosensitive original drug is improved, the quality change or agglomeration of the thermosensitive original drug is reduced, the hydrophilicity of the thermosensitive original drug is improved, and the pesticide effect of the pesticide preparation is improved.

To better understand the grinding compensation medium-based thermal-sensitive bulk drug grinding method of the present application, the grinding compensation medium-based thermal-sensitive bulk drug grinding method of the present application is further explained below, and one embodiment of the grinding compensation medium-based thermal-sensitive bulk drug grinding method includes the following steps:

s100, obtaining a grinding medium and a titanium dioxide grinding compensation medium, wherein the titanium dioxide grinding compensation medium is nano-scale particles. It can be understood that before the thermosensitive original drug is ground, the grinding medium and the titanium dioxide grinding compensation medium are obtained to continuously grind the thermosensitive original drug, wherein the obtained titanium dioxide grinding compensation medium is nano-scale particles, so that the contact area between the grinding medium and the thermosensitive original drug is greatly increased, and the grinding speed of the thermosensitive original drug can be effectively increased by matching with the obtained grinding medium.

S200, mixing the titanium dioxide grinding compensation medium and the thermosensitive original medicine to obtain a mixture to be ground. The titanium dioxide grinding compensation medium and the heat-sensitive raw pesticide can be fully and uniformly mixed by mixing the titanium dioxide grinding compensation medium and the heat-sensitive raw pesticide, so that the titanium dioxide is uniformly dispersed at the periphery of the heat-sensitive raw pesticide, the heat-sensitive raw pesticide has better heat stability during grinding, and the quality change or agglomeration of the heat-sensitive raw pesticide is reduced, and particularly, the titanium dioxide grinding compensation medium is a filler, so that the titanium dioxide is not required to be separated when used for a pesticide preparation, the preparation procedures of the pesticide preparation are reduced, and the production efficiency of the pesticide preparation is improved; in addition, the titanium dioxide grinding compensation medium has high thermal stability and hydrophilicity, but has weak hygroscopicity and viscosity, and can be well dispersed on the peripheral surface of the thermosensitive original drug, so that the thermal stability of the thermosensitive original drug is improved, the qualitative change or agglomeration of the thermosensitive original drug is reduced, the hydrophilicity of the thermosensitive original drug is improved, and the pesticide effect of the pesticide preparation is improved.

And S300, putting the mixture to be ground and the grinding medium into a grinding machine for grinding operation to obtain the thermosensitive original drug ground substance. It can be understood that the titanium dioxide grinding compensation medium is nano-scale particles, which greatly increases the contact area between the grinding medium and the heat-sensitive raw pesticide, so that when the titanium dioxide grinding compensation medium is matched with the grinding medium to grind the heat-sensitive raw pesticide, the grinding medium directly impacts the heat-sensitive raw pesticide in the process of impacting and crushing the heat-sensitive raw pesticide by the falling grinding medium, and an impact force is given to the titanium dioxide grinding compensation medium when impacting the heat-sensitive raw pesticide, so that the titanium dioxide grinding compensation medium further impacts the heat-sensitive raw pesticide, the impact frequency of the heat-sensitive raw pesticide is effectively improved, and the grinding speed of the heat-sensitive raw pesticide is further increased; in addition, in the process that the grinding medium and the titanium dioxide grinding compensation medium flow, the grinding medium extrudes and grinds the heat-sensitive raw pesticide, and simultaneously, the titanium dioxide grinding compensation medium further extrudes and grinds the heat-sensitive raw pesticide, so that the extrusion and grinding friction force of the heat-sensitive raw pesticide is effectively increased, the grinding speed of the heat-sensitive raw pesticide is further accelerated, the temperature rise degree of the heat-sensitive raw pesticide is smaller when the heat-sensitive raw pesticide is crushed to the required grain diameter, namely when the temperature of the heat-sensitive raw pesticide is at a lower temperature, the heat-sensitive raw pesticide is crushed to the required grain diameter, the problem that the raw pesticide is changed or agglomerated when the addition amount of zirconium oxide beads of the grinding medium is larger or the grinding speed of a sand mill is higher, the material is ground and heated to the high temperature of raw pesticide particles is solved, further influencing the quality of pesticide products, and reducing the problems that the grinding efficiency of the raw pesticide can be influenced if the adding amount of the grinding medium zirconia beads is small or the grinding speed of a sand mill is slow, further reducing the production efficiency of the pesticide preparation, greatly improving the production cost of the pesticide preparation due to the long-time operation of equipment, further improving the grinding speed of the thermosensitive raw pesticide and reducing the quality change or agglomeration of the thermosensitive raw pesticide.

In the method for grinding the thermosensitive original drug based on the grinding compensation medium, the titanium dioxide grinding compensation medium is nano-scale particles, so that the contact area between the grinding medium and the thermosensitive original drug is greatly increased, when the titanium dioxide grinding compensation medium is matched with the grinding medium to grind the thermosensitive original drug, the grinding medium directly impacts the thermosensitive original drug in the process of impacting and crushing the thermosensitive original drug by the falling grinding medium, and an impact force is given to the titanium dioxide grinding compensation medium when impacting the thermosensitive original drug, so that the titanium dioxide grinding compensation medium further impacts the thermosensitive original drug, the impact frequency of the thermosensitive original drug is effectively improved, and the grinding speed of the thermosensitive original drug is accelerated; in addition, in the process that the grinding medium and the titanium dioxide grinding compensation medium flow, the grinding medium extrudes and grinds the heat-sensitive raw pesticide, and simultaneously, the titanium dioxide grinding compensation medium further extrudes and grinds the heat-sensitive raw pesticide, so that the extrusion and grinding friction force of the heat-sensitive raw pesticide is effectively increased, the grinding speed of the heat-sensitive raw pesticide is further accelerated, the temperature rise degree of the heat-sensitive raw pesticide is smaller when the heat-sensitive raw pesticide is crushed to the required grain diameter, namely when the temperature of the heat-sensitive raw pesticide is at a lower temperature, the heat-sensitive raw pesticide is crushed to the required grain diameter, the problem that the raw pesticide is changed or agglomerated when the addition amount of zirconium oxide beads of the grinding medium is larger or the grinding speed of a sand mill is higher, the material is ground and heated to the high temperature of raw pesticide particles is solved, further influencing the quality of pesticide products, and reducing the problems that the grinding efficiency of the raw pesticide can be influenced if the adding amount of the grinding medium zirconia beads is small or the grinding speed of a sand mill is slow, further reducing the production efficiency of the pesticide preparation, greatly improving the production cost of the pesticide preparation due to the long-time operation of equipment, further improving the grinding speed of the thermosensitive raw pesticide and reducing the quality change or agglomeration of the thermosensitive raw pesticide. Because the titanium dioxide grinding compensation medium is used as the filler, the titanium dioxide is not required to be separated when the titanium dioxide grinding compensation medium is used for the pesticide preparation, the preparation procedures of the pesticide preparation are reduced, and the production efficiency of the pesticide preparation is improved. The titanium dioxide grinding compensation medium has high thermal stability and hydrophilicity, but has weak hygroscopicity and viscosity, and can be well dispersed on the peripheral surface of the thermosensitive original drug, so that the thermal stability of the thermosensitive original drug is improved, the quality change or agglomeration of the thermosensitive original drug is reduced, the hydrophilicity of the thermosensitive original drug is improved, and the pesticide effect of the pesticide preparation is improved.

In one embodiment, before the step of putting the mixture to be ground and the grinding medium into the grinding machine for the grinding operation, and after the step of mixing the titanium dioxide grinding compensation medium and the heat-sensitive technical material, the grinding compensation medium-based heat-sensitive technical material grinding method further comprises the following steps: the dispersion medium and the dispersant are added to the mixture to be milled. It can be understood that adding the dispersion medium into the thermosensitive original drug for grinding is beneficial to the grinding sufficiency of the thermosensitive original drug, and the dispersion medium is beneficial to taking away the heat of the thermosensitive original drug, so that the temperature of the thermosensitive original drug in the grinding process is reduced, and adding the dispersion medium into the thermosensitive original drug is more beneficial to coating the titanium dioxide grinding compensation medium on the peripheral surface of the thermosensitive original drug, so that the thermal stability of the thermosensitive original drug is more effectively improved, the qualitative change or agglomeration of the thermosensitive original drug is effectively reduced, wherein the wetting property of the thermosensitive original drug in the dispersion medium is improved by the dispersing agent, the dispersion uniformity of the thermosensitive original drug in the dispersion medium is better ensured, and the full grinding of the thermosensitive original drug is further facilitated.

In one embodiment, the dispersing medium is water or methyl oleate. It is understood that water as a dispersion medium for suspending agents and dry suspending agents, etc., and methyl oleate as a dispersion medium for dispersible oil suspending agents, etc., all ensure the dispersibility of the thermosensitive original drug.

In one embodiment, the method for grinding a heat-sensitive technical drug based on a grinding compensation medium further comprises the following steps before the step of putting the mixture to be ground and the grinding medium into a grinding mill for a grinding operation and after the step of adding the dispersion medium and the dispersing agent to the mixture to be ground: a wetting or emulsifying agent is added to the mixture to be milled. The grinding also has the effect of mixing the added substances, and is beneficial to increasing the mixing uniformity and dispersion stability of the added substances, so that the wetting agent or the emulsifying agent is added into the grinding machine to be ground together with the thermosensitive original medicine, the mixing uniformity is greatly higher than that of the later stirring and mixing, and the uniformity and the stability of the pesticide preparation are effectively improved; in addition, the wetting agent or the emulsifying agent further improves the wettability of the thermosensitive original drug in the dispersion medium, better ensures the dispersion uniformity of the thermosensitive original drug in the dispersion medium, and is favorable for fully grinding the thermosensitive original drug.

In one embodiment, the method for grinding a heat-sensitive technical drug based grinding compensation medium further comprises the steps of, before the step of feeding the mixture to be ground and the grinding medium into a grinding mill for a grinding operation, and after the step of adding a wetting or emulsifying agent to the mixture to be ground: adding a disintegration aid to the mixture to be milled. It can be understood that the disintegration aid is added into the grinding machine to be ground together with the thermosensitive original medicine, the mixing uniformity degree is greatly higher than that of the later stirring and mixing, and the uniformity and the stability of the pesticide preparation are effectively improved.

In one embodiment, the method for grinding a heat-sensitive technical drug based grinding compensation medium further comprises the steps of, before the step of feeding the mixture to be ground and the grinding medium into a grinding mill for a grinding operation, and after the step of adding a wetting or emulsifying agent to the mixture to be ground: a filler is added to the mixture to be milled. The filler is added into the grinding machine to be ground together with the thermosensitive original medicine, so that the mixing uniformity is greatly higher than that of the later stirring and mixing, and the uniformity and the stability of the pesticide preparation are effectively improved; in addition, the filler further improves the grinding effect of the thermosensitive original drug, and further improves the grinding speed of the thermosensitive original drug.

In one embodiment, the method for grinding a heat-sensitive technical drug based grinding compensation medium further comprises the steps of, before the step of feeding the mixture to be ground and the grinding medium into a grinding mill for a grinding operation, and after the step of adding a wetting or emulsifying agent to the mixture to be ground: an anti-freeze agent is added to the mixture to be milled. The antifreezing agent is added into the grinding machine to be ground together with the heat-sensitive raw pesticide, so that the mixing uniformity is greatly higher than that of the later stirring and mixing, and the uniformity and the stability of the pesticide preparation are effectively improved; in addition, the antifreezing agent plays an antifreezing role on the heat-sensitive raw pesticide in the grinding process, and the grinding effect of the heat-sensitive raw pesticide is ensured.

In one embodiment, the method for grinding a heat-sensitive technical drug based grinding compensation medium further comprises the steps of, before the step of feeding the mixture to be ground and the grinding medium into a grinding mill for a grinding operation, and after the step of adding a wetting or emulsifying agent to the mixture to be ground: an antifoaming agent is added to the mixture to be milled. It can be understood that the defoaming agent has the function of a surfactant, so that bubbles generated by a mixture to be ground in a grinding machine in the grinding process are effectively reduced, the uniform dispersion of the thermosensitive original medicine is improved, and the uniformity of the pesticide preparation is further improved. In one embodiment, the D50 of the titanium dioxide grinding compensation medium is 0.5-1 μm. It can be understood that when the D50 of the titanium dioxide grinding compensation medium is 0.5-1 μm, the grinding strength of the heat-sensitive raw pesticide is optimal, the quick grinding of the heat-sensitive raw pesticide is better realized, and the quality change or agglomeration caused by the large temperature increase of the heat-sensitive raw pesticide due to long-time grinding is further reduced.

In one embodiment, the addition amount of the titanium dioxide grinding compensation medium is greater than or equal to 3% of the total mass of the heat-sensitive raw pesticide. It can be understood that the usage amount of the titanium dioxide is further limited according to the content of the filler of the pesticide preparation containing the heat-sensitive raw pesticide, and the titanium dioxide can be matched with the grinding medium under the condition that the addition amount of the titanium dioxide grinding compensation medium is more than or equal to 3% of the total mass of the heat-sensitive raw pesticide so as to effectively improve the grinding speed of the heat-sensitive raw pesticide, and the titanium dioxide grinding compensation medium acts on the surface of the heat-sensitive raw pesticide, so that the heat stability of the heat-sensitive raw pesticide is improved, the quality change or agglomeration of the heat-sensitive raw pesticide is effectively reduced, and the pesticide effect of the pesticide preparation is improved.

In one embodiment, the titanium dioxide grinding compensation medium is rutile titanium dioxide. It can be understood that the rutile type titanium dioxide has higher hardness, and plays a better grinding effect when the grinding medium is matched with the titanium dioxide grinding compensation medium to grind the heat-sensitive raw pesticide, so that the grinding speed of the heat-sensitive raw pesticide is better improved, and the quality change or agglomeration of the heat-sensitive raw pesticide is reduced. It can also be understood that if other types of titanium dioxide grinding compensation media are selected, the extrusion grinding effect of the grinding media and the titanium dioxide grinding compensation media on the thermosensitive original drug is poor, the grinding speed of the thermosensitive original drug is difficult to be effectively increased, and the quality change or agglomeration of the thermosensitive original drug is difficult to be reduced.

In one embodiment, the bulk drug thermo-sensitive compound is at least one of pyraclostrobin, metiram, difenoconazole, trifloxystrobin and glyphosate. It can be understood that the thermosensitive technical is an effective component of pesticide sensitive to heat, the heat is that the pesticide preparation is easy to be decomposed by heat under the condition of higher temperature or the pesticide preparation is reduced by other modes under the condition of higher temperature, for example, agglomeration occurs under the condition of higher temperature, pyraclostrobin, metiram, difenoconazole, trifloxystrobin and glyphosate are all effective components of pesticide sensitive to heat, namely, the thermosensitive technical is easy to be influenced by temperature to reduce the control effect of crops, in the application, the thermosensitive technical grinding method based on grinding compensation medium is adopted to grind the pyraclostrobin, metiram, difenoconazole, trifloxystrobin and glyphosate, so that the grinding speed of the pyraclostrobin, metiram, difenoconazole, trifloxystrobin and glyphosate is effectively improved, and the grinding speed of the pyraclostrobin, metiram, difenoconazole and glyphosate is reduced, The quality change or agglomeration of the trifloxystrobin and the glyphosate further improves the pesticide effect of the pesticide preparation.

In one embodiment, the grinding media is at least one of steel balls, zirconia balls, and ceramic balls. It can be understood that, in order to ensure the quality of the grinding medium and improve the filling quantity of the grinding medium, in the heat-sensitive raw drug grinding method based on the grinding compensation medium, the steel balls, the zirconia balls and the ceramic balls with higher mass density are selected as the grinding medium, and the grinding effect of the grinding medium and the titanium dioxide grinding compensation medium on the heat-sensitive raw drug is better ensured.

In one embodiment, the grinding media has a fill rate of 60% to 75%. It can be understood that when the filling rate of the grinding medium is 60-75%, the grinding medium is matched with the titanium dioxide grinding compensation medium in an amount which is more than or equal to 3% of the total mass of the heat-sensitive raw pesticide, so that the grinding effect of the matching of the grinding medium and the titanium dioxide grinding compensation medium on the heat-sensitive raw pesticide is better ensured.

In one embodiment, the grinding media comprises a first ellipsoidal sphere and a second ellipsoidal sphere, the first ellipsoidal sphere having a volume greater than the volume of the second ellipsoidal sphere. It can be understood that the volume of the first oval sphere is larger than that of the second oval sphere, the gap of the first oval sphere is filled well, the stacking density of the grinding medium is improved, the impact force and the impact frequency of the grinding medium are effectively improved, the thermosensitive raw medicine in the gap of the grinding medium is extruded out of the impact area of the grinding medium, and the grinding effect of the grinding medium and the titanium dioxide grinding compensation medium on the thermosensitive raw medicine is better ensured. In one embodiment, the grinding media have a particle size of 0.3mm to 2.0 mm. It can be understood that, under the condition that the grinding medium is matched with the titanium dioxide grinding compensation medium to grind the heat-sensitive raw pesticide, if the particle size of the grinding medium is too large, the heat-sensitive raw pesticide is easy to stay in the gap of the grinding medium, so that the grinding effect of the grinding medium and the titanium dioxide grinding compensation medium on the heat-sensitive raw pesticide due to mutual extrusion is reduced, the grinding speed of the heat-sensitive raw pesticide is further reduced, the heat-sensitive raw pesticide is subjected to great qualitative change or agglomeration, and the pesticide effect of the pesticide preparation is reduced; if the particle size of the grinding medium is smaller, the impact capacity of the grinding medium is weaker, so that the grinding medium and the titanium dioxide grinding compensation medium are matched to have a poorer crushing and grinding effect on the thermosensitive raw pesticide, further the grinding speed of the thermosensitive raw pesticide is reduced, the thermosensitive raw pesticide is greatly changed in quality or agglomerated, and the pesticide effect of the pesticide preparation is reduced, therefore, in the thermosensitive raw pesticide grinding method based on the grinding compensation medium, the particle size of the grinding medium is 0.3-2.0 mm, the grinding medium and the titanium dioxide grinding compensation medium are effectively ensured to be matched to have a crushing and grinding effect on the thermosensitive raw pesticide, the grinding speed of the thermosensitive raw pesticide is improved, and the quality change or agglomeration of the thermosensitive raw pesticide is reduced.

In one embodiment, the particle size of the first oval sphere is 0.3 mm-0.4 mm, so that the grinding effect of the grinding medium and the titanium dioxide grinding compensation medium on the heat-sensitive raw pesticide is better ensured.

In one embodiment, the particle size of the first oval sphere is 0.6 mm-0.8 mm, so that the grinding effect of the grinding medium and the titanium dioxide grinding compensation medium on the heat-sensitive raw pesticide is better ensured.

In one embodiment, the particle size of the first oval sphere is 0.8 mm-1.0 mm, so that the grinding effect of the grinding medium and the titanium dioxide grinding compensation medium on the heat-sensitive raw pesticide is better ensured.

In one embodiment, the particle size of the second elliptical spheres is 1.0 mm-1.2 mm, so that the grinding effect of the grinding medium and the titanium dioxide grinding compensation medium on the heat-sensitive raw pesticide is better ensured.

In one embodiment, the particle size of the second elliptical spheres is 1.4 mm-1.6 mm, so that the grinding effect of the grinding medium and the titanium dioxide grinding compensation medium on the heat-sensitive raw pesticide is better ensured.

In one embodiment, the particle size of the second elliptical spheres is 1.8 mm-2.0 mm, so that the grinding effect of the grinding medium and the titanium dioxide grinding compensation medium on the heat-sensitive raw pesticide is better ensured.

The present application also provides a pesticide formulation. The pesticide preparation comprises a dispersing agent, a wetting agent, a filler, a disintegrating aid and the heat-sensitive raw pesticide ground product obtained by the heat-sensitive raw pesticide grinding method based on the grinding compensation medium in any one embodiment. In this embodiment, the method for grinding heat-sensitive raw pesticide based on grinding compensation medium comprises the following steps: obtaining a grinding medium and a titanium dioxide grinding compensation medium, wherein the titanium dioxide grinding compensation medium is nano-scale particles; mixing the titanium dioxide grinding compensation medium and the thermosensitive original medicine to obtain a mixture to be ground; and putting the mixture to be ground and the grinding medium into a grinder for grinding operation to obtain the heat-sensitive original drug ground substance.

In the pesticide preparation, the titanium dioxide grinding compensation medium is used as the filler, so that the titanium dioxide is not required to be separated when the titanium dioxide grinding compensation medium is used for the pesticide preparation, the preparation procedures of the pesticide preparation are reduced, and the production efficiency of the pesticide preparation is improved. In addition, the titanium dioxide grinding compensation medium has high thermal stability and hydrophilicity, but has weak hygroscopicity and viscosity, and can be well dispersed on the peripheral surface of the thermosensitive original drug, so that the thermal stability of the thermosensitive original drug is improved, the qualitative change or agglomeration of the thermosensitive original drug is reduced, the hydrophilicity of the thermosensitive original drug is improved, and the pesticide effect of the pesticide preparation is improved.

In one embodiment, the pesticide formulation further comprises a thickening agent, which improves the dispersion stability of the pesticide formulation.

Compared with the prior art, the invention has at least the following advantages:

1. according to the heat-sensitive raw drug grinding method based on the grinding compensation medium, the titanium dioxide grinding compensation medium is nano-scale particles, so that the contact area between the grinding medium and the heat-sensitive raw drug is greatly increased, when the titanium dioxide grinding compensation medium is matched with the grinding medium to grind the heat-sensitive raw drug, the grinding medium directly impacts the heat-sensitive raw drug in the process that the falling grinding medium impacts and breaks the heat-sensitive raw drug, and an impact force is given to the titanium dioxide grinding compensation medium when the heat-sensitive raw drug is impacted, so that the titanium dioxide grinding compensation medium further impacts the heat-sensitive raw drug, the impact frequency of the heat-sensitive raw drug is effectively improved, and the grinding speed of the heat-sensitive raw drug is accelerated; in addition, in the process that the grinding medium and the titanium dioxide grinding compensation medium flow, the grinding medium extrudes and grinds the heat-sensitive raw pesticide, and simultaneously, the titanium dioxide grinding compensation medium further extrudes and grinds the heat-sensitive raw pesticide, so that the extrusion and grinding friction force of the heat-sensitive raw pesticide is effectively increased, the grinding speed of the heat-sensitive raw pesticide is further accelerated, the temperature rise degree of the heat-sensitive raw pesticide is smaller when the heat-sensitive raw pesticide is crushed to the required grain diameter, namely when the temperature of the heat-sensitive raw pesticide is at a lower temperature, the heat-sensitive raw pesticide is crushed to the required grain diameter, the problem that the raw pesticide is changed or agglomerated when the addition amount of zirconium oxide beads of the grinding medium is larger or the grinding speed of a sand mill is higher, the material is ground and heated to the high temperature of raw pesticide particles is solved, the quality of the pesticide product is further influenced, the problem that the grinding efficiency of the original pesticide is influenced if the adding amount of the grinding medium zirconia beads is small or the grinding speed of a sand mill is slow is solved, the production efficiency of the pesticide preparation is further reduced, the production cost of the pesticide preparation is greatly improved due to the long-time operation of equipment, the grinding speed of the thermosensitive original pesticide is further improved, and the quality change or agglomeration of the thermosensitive original pesticide is reduced;

2. in the heat-sensitive original medicine grinding method based on the grinding compensation medium, the titanium dioxide grinding compensation medium is used as the filler, so that the titanium dioxide is not required to be separated when the titanium dioxide grinding compensation medium is used for a pesticide preparation, the preparation procedures of the pesticide preparation are reduced, and the production efficiency of the pesticide preparation is improved;

3. in the heat-sensitive raw pesticide grinding method based on the grinding compensation medium, the titanium dioxide grinding compensation medium has high thermal stability, hydrophilicity, weaker hygroscopicity and viscosity, and can be well dispersed on the peripheral surface of the heat-sensitive raw pesticide, so that the heat stability of the heat-sensitive raw pesticide is improved, the quality change or agglomeration of the heat-sensitive raw pesticide is reduced, the hydrophilicity of the heat-sensitive raw pesticide is improved, and the pesticide effect of a pesticide preparation is improved.

Some specific examples are listed below, and if mentioned%, all are expressed in weight percent. It should be noted that the following examples are not intended to be exhaustive of all possible cases, and that the materials used in the following examples are commercially available without specific recitation.

Example a

Respectively obtaining zirconia balls with filling rates of 60%, 65% and 70%, and obtaining titanium dioxide.

Mixing titanium dioxide and the thermosensitive original medicine;

respectively adding a dispersion medium and a dispersant into the thermosensitive original drug;

adding a wetting agent into the thermosensitive original medicine;

adding a disintegrating aid, a defoaming agent and a filler into the thermosensitive original medicine;

putting the thermosensitive original medicine mixture to be ground and zirconia balls into a grinding machine for grinding;

wherein the usage amounts of the thermosensitive original drug (hereinafter referred to as an active ingredient), the dispersing agent, the wetting agent, the disintegrating aid, the antifoaming agent, the titanium dioxide, the filler and the dispersion medium are respectively shown in examples 1 to 11 and comparative examples 1 to 3.

Example b

Obtaining zirconia balls with the filling rate of 75 percent and obtaining titanium dioxide.

Mixing titanium dioxide and the thermosensitive original medicine;

respectively adding a dispersion medium and a dispersant into the thermosensitive original drug;

adding an emulsifier into the thermosensitive original medicine;

putting the thermosensitive original medicine mixture to be ground and zirconia balls into a grinding machine for grinding;

the amounts of the thermosensitive original drug (hereinafter referred to as active ingredient), the dispersant, the emulsifier, the titanium dioxide and the dispersion medium used were as shown in examples 12 to 14 and comparative example 4, respectively.

Example c

Obtaining zirconia balls with the filling rate of 75 percent and obtaining titanium dioxide.

Mixing titanium dioxide and the thermosensitive original medicine;

respectively adding a dispersion medium and a dispersant into the thermosensitive original drug;

adding a wetting agent into the thermosensitive original medicine;

adding an antifreezing agent and a defoaming agent into the thermosensitive original medicine;

putting the thermosensitive original medicine mixture to be ground and zirconia balls into a grinding machine for grinding;

the amounts of the heat-sensitive technical material (hereinafter referred to as an active ingredient), the dispersant, the wetting agent, the antifreeze, the defoamer, the titanium pigment and the dispersion medium used are shown in examples 15 to 17 and comparative example 5, respectively.

The filling rate of the zirconia beads used in examples 1 to 5 and comparative example 1 was 60%;

table 1: the use amounts of the active ingredients, the dispersing agent, the wetting agent, the filler, the disintegrating aid, the defoaming agent, the titanium dioxide and the dispersion medium in examples 1 to 5 and comparative example 1

The filling rate of the zirconia beads used in examples 6 to 8 and comparative example 2 was 65%;

table 2: the use amounts of the active ingredients, the dispersing agent, the wetting agent, the filler, the disintegrating aid, the antifoaming agent, the titanium dioxide and the dispersion medium in examples 6 to 8 and comparative example 2

The filling rate of the zirconia beads used in examples 9 to 11 and comparative example 3 was 70%;

table 3: the use amounts of the active ingredients, the dispersing agent, the wetting agent, the filler, the disintegrating aid, the antifoaming agent, the titanium dioxide and the dispersion medium in examples 9 to 11 and comparative example 3

The filling rate of the zirconia beads used in examples 12 to 14 and comparative example 4 was 75%;

table 4: the use amounts of the active ingredient, dispersant, emulsifier, thickener, titanium dioxide and dispersion medium in examples 12 to 14 and comparative example 4

The filling rate of the zirconia beads used in examples 15 to 17 and comparative example 5 was 75%;

table 5: the use amounts of the active ingredients, the dispersing agent, the wetting agent, the antifreeze, the antifoaming agent, the titanium dioxide and the dispersion medium in examples 15 to 17 and comparative example 5

The performance tests were carried out on the heat-sensitive raw drug abrasives of examples 1 to 17 and the heat-sensitive raw drug abrasives of comparative examples 1 to 5 obtained by the preparation of examples as follows:

the test results are shown in table 6, table 7, table 8, table 9, table 10 and fig. 2, where fig. 2 is a graph of the discharge temperature of the heat-sensitive technical ground product of example 17 and comparative example 5.

Table 6: each property of the heat-sensitive raw drug abrasives of examples 1 to 5 and comparative example 1

Table 7: each property of the heat-sensitive raw drug abrasives of examples 6 to 8 and comparative example 2

Table 8: each property of the thermosensitive original drug ground products of examples 9 to 11 and comparative example 3

Table 9: each property of the heat-sensitive raw drug abrasives of examples 12 to 14 and comparative example 4

Table 10: each property of the thermosensitive original drug abrasives of examples 15 to 17 and comparative example 5

As can be seen from tables 1 to 10 and fig. 2, the discharge temperature of the heat-sensitive raw drug ground product of examples 1 to 17 is significantly lower than that of the heat-sensitive raw drug ground product of comparative examples 1 to 5, which indicates that the temperature rise of the heat-sensitive raw drug in the grinding process is effectively reduced by grinding the heat-sensitive raw drug by using the titanium dioxide grinding compensation medium in cooperation with the grinding medium in the present application, and the grinding flow rate of the heat-sensitive raw drug ground product of examples 1 to 17 is significantly higher than that of the heat-sensitive raw drug ground product of comparative examples 1 to 5, which indicates that the heat-sensitive raw drug is ground by using the titanium dioxide grinding compensation medium in cooperation with the grinding medium in the present application, and the grinding speed of the heat-sensitive raw drug is effectively increased.

The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.