阅读说明：本技术 一种吡蚜酮·呋虫胺干悬浮剂及其制备方法 (Pymetrozine and dinotefuran dry suspending agent and preparation method thereof ) 是由 郑少伟 张宗俭 卢忠利 张鹏 魏光 于 2021-07-02 设计创作，主要内容包括：本发明涉及一种吡蚜酮·呋虫胺干悬浮剂及其制备方法,属于农药技术领域。上述干悬浮剂由以下质量百分比的组分组成：40％～60％吡蚜酮原药、5％～30％呋虫胺原药、1％～5％阴离子型分散剂、5％～10％液体润湿剂、5％～20％木质素、余量填料补足至100％；所述木质素为木质素磺酸钠和/或木质素磺酸钙；所述阴离子型分散剂包括乙氧基化的三苯乙烯基苯酚磷酸钾盐。本发明利用木质素、阴离子分散剂、液体润湿剂可以与吡蚜酮、呋虫胺原药发生协同作用,增加吡蚜酮·呋虫胺干悬浮剂的分散性,及悬浮性能不易沉淀分层、易崩解。(The invention relates to a pymetrozine-dinotefuran dry suspending agent and a preparation method thereof, belonging to the technical field of pesticides. The dry suspending agent comprises the following components in percentage by mass: 40 to 60 percent of pymetrozine technical, 5 to 30 percent of dinotefuran technical, 1 to 5 percent of anionic dispersant, 5 to 10 percent of liquid wetting agent, 5 to 20 percent of lignin and the balance of filler are complemented to 100 percent; the lignin is sodium lignosulfonate and/or calcium lignosulfonate; the anionic dispersant comprises an ethoxylated tristyrylphenol potassium phosphate salt. According to the invention, lignin, an anionic dispersant and a liquid wetting agent can generate a synergistic effect with raw pymetrozine and dinotefuran, so that the dispersibility of the pymetrozine and dinotefuran dry suspending agent is improved, and the suspending performance is not easy to precipitate, layer and disintegrate.)

1. The pymetrozine-dinotefuran dry suspending agent is characterized by comprising the following components in percentage by mass: 40 to 60 percent of pymetrozine technical, 5 to 30 percent of dinotefuran technical, 1 to 5 percent of anionic dispersant, 5 to 10 percent of liquid wetting agent, 5 to 20 percent of lignin and the balance of filler are complemented to 100 percent; the lignin is sodium lignosulfonate and/or calcium lignosulfonate; the anionic dispersant comprises an ethoxylated tristyrylphenol potassium phosphate salt.

2. The pymetrozine dinotefuran dry suspending agent as claimed in claim 1, which is characterized by comprising the following components in percentage by mass: 45-55% of pymetrozine technical, 10-25% of dinotefuran technical, 1-5% of anionic dispersant, 5-10% of liquid wetting agent, 10-15% of lignin and the balance of filler are complemented to 100%.

3. A pymetrozine dinotefuran dry suspension according to claim 1 or 2, wherein the anionic dispersant further comprises one or more of a polycarboxylate, a naphthalene sulfonate.

4. The pymetrozine dinotefuran dry suspension of claim 3, wherein the liquid wetting agent is one or more of sodium dodecylbenzene sulfonate, sodium dodecyl sulfate and sodium alkenyl sulfonate.

5. The pymetrozine dinotefuran dry suspension as claimed in claim 4, wherein the filler is one or more of kaolin, light calcium and barium sulfate.

6. The pymetrozine dinotefuran dry suspension as claimed in claim 5, wherein the weight ratio of the anionic dispersant is 1: 0.5 of a mixture of ethoxylated tristyrylphenol potassium phosphate salt and polycarboxylate.

7. A process for the preparation of a dry suspension of pymetrozine dinotefuran of any one of claims 1 to 6, which comprises:

step 1: pouring the anionic dispersant, the liquid wetting agent, the lignin and the filler into a shearing kettle filled with water, shearing and stirring uniformly, then adding raw pymetrozine and dinotefuran and stirring uniformly to form slurry;

step 2: sucking the slurry into a first-stage sand mill and a second-stage sand mill for primary sand milling and repeated sand milling,

And step 3: and pressing the sanded slurry into a pressure type spray drying granulator, a centrifugal spray dryer or a fluidized bed spray drying granulator through a peristaltic pump for spray drying granulation.

Technical Field

The invention relates to the technical field of pesticide auxiliary agents, and particularly provides a pymetrozine and dinotefuran dry suspending agent and a preparation method thereof.

Background

With the environmental and ecological challenges faced by traditional pesticide formulations, it is inevitable and certain to develop environmentally compatible pesticides, and is also a requirement for the sustainable development of environmental and pesticide first-class pesticides. The dry suspending agent is a micro-particle pesticide formulation product, and is prepared by the following steps of content, packaging and process after the suspending agent. The cost, quality and use technology are all obviously superior to the updated products of other dosage forms. The dry suspending agent has the advantages of quick disintegration, fine dispersion, high suspension rate, quick formation of stable suspension when meeting water, no precipitation, no blocking of a spray head when being used, and the like.

The dry suspending agent mainly comprises a dispersing agent, a wetting agent, a defoaming agent, a pH regulator, a filler and the like, and has the main properties: effective content, disintegration, dispersibility, suspension rate, persistent foaming property, pH value, normal temperature, heat storage stability and the like. The disintegration, the dispersibility and the suspension rate directly influence the drug effect, and are closely related to the properties of the effective components, the used dispersing agent, wetting agent and filler. In the same formulation, the use of different dispersing agents or wetting agents can obviously affect the performance of the preparation, and if the pesticide active ingredients, the dispersing agents, the wetting agents and the fillers are incompatible, the performance of the granule preparation is unstable, the granule preparation is agglomerated and can not be disintegrated, and the suspension rate is reduced, so that the drug effect is affected, and the dispersing agents, the wetting agents and the fillers need to be matched with the active ingredients for use.

Pymetrozine is a high-efficiency non-biocidal insecticide, and dinotefuran is a high-efficiency insecticide. Pymetrozine has a unique needle blocking effect, and once eating, pests can quickly inhibit eating; dinotefuran is an insecticide which acts on an insect deep environment transmission system and has contact killing and stomach poisoning effects, can be quickly absorbed by vegetation and is widely distributed in crops. The two have strong toxicity complementation and high co-toxicity coefficient, have strong synergistic effect and are high-efficiency and low-toxicity compound agents.

Disclosure of Invention

In order to solve the problems in the prior art, the invention provides a pymetrozine and dinotefuran dry suspending agent and a preparation method thereof.

In order to solve the technical problems, the invention provides the following technical scheme:

on one hand, the invention provides a pymetrozine-dinotefuran dry suspending agent which comprises the following components in percentage by mass: 40 to 60 percent of pymetrozine technical, 5 to 30 percent of dinotefuran technical, 1 to 5 percent of anionic dispersant, 5 to 10 percent of liquid wetting agent, 5 to 20 percent of lignin and the balance of filler are complemented to 100 percent; the lignin is sodium lignosulfonate and/or calcium lignosulfonate; the anionic dispersant comprises an ethoxylated tristyrylphenol potassium phosphate salt.

Preferably, the pymetrozine-dinotefuran dry suspending agent consists of the following components in percentage by mass: 45-55% of pymetrozine technical, 10-25% of dinotefuran technical, 1-5% of anionic dispersant, 5-10% of liquid wetting agent, 10-15% of lignin and the balance of filler are complemented to 100%.

Further, the anionic dispersant also comprises one or more of polycarboxylate and naphthalene sulfonate.

Further, the liquid wetting agent is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and sodium alkenyl sulfonate.

Further, the filler is one or more of kaolin, light calcium and barium sulfate.

Preferably, the anionic dispersant is a mixture of 1: 0.5 of a mixture of ethoxylated tristyrylphenol potassium phosphate salt and polycarboxylate.

On the other hand, the invention also provides a preparation method of the pymetrozine-dinotefuran dry suspending agent, which comprises the following steps:

step 1: pouring the anionic dispersant, the liquid wetting agent, the lignin and the filler into a shearing kettle filled with water, shearing and stirring uniformly, then adding raw pymetrozine and dinotefuran and stirring uniformly to form slurry;

step 2: sucking the slurry into a first-stage sand mill and a second-stage sand mill for primary sand milling and repeated sand milling,

And step 3: and pressing the sanded slurry into a pressure type spray drying granulator, a centrifugal spray dryer or a fluidized bed spray drying granulator through a peristaltic pump for spray drying granulation.

In the step 1, the solid content in the slurry is 20-40%; in the step 2, the sanding medium is pickaxe beads with the diameter of 0.3-1.6 mm.

Compared with the prior art, the invention has the following beneficial effects:

(1) the pymetrozine-dinotefuran dry suspending agent material is subjected to sand grinding, the particle size of slurry is less than or equal to 5 microns, the dispersion in water is good, the suspension performance is good, and the deposition and layering are not easy to occur;

(2) the dispersant and wetting agent used in the pymetrozine-dinotefuran dry suspending agent are both anionic, and are self-dispersible in water, so that the problem of difficult disintegration and dispersion is avoided;

(3) the pymetrozine and dinotefuran are added with lignin, so that the problems of poor disintegration and poor dispersion of the preparation are solved. The problem of dead particles is easily generated.

Detailed Description

In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.

The reagents and materials used in the examples and comparative examples were commercially available unless otherwise specified.

The invention provides a pymetrozine-dinotefuran dry suspending agent and a preparation method thereof, and specific embodiments are as follows.

Example 1

The pymetrozine-dinotefuran dry suspending agent comprises the following components in percentage by mass: 60% of pymetrozine technical, 5% of dinotefuran technical, 5% of ethoxylated tristyrylphenol potassium phosphate, 8% of sodium dodecyl sulfate, 7% of sodium lignin sulfonate and 15% of kaolin.

The preparation method of the pymetrozine-dinotefuran dry suspending agent comprises the following steps:

step 1: 5kg of polycarboxylate, 8kg of sodium dodecyl sulfate and 7kg of sodium lignin sulfonate are poured into a shearing kettle containing 100kg of water, the materials are sheared and stirred uniformly, and then 60kg of pymetrozine raw material and 5kg of dinotefuran raw material are added.

Step 2: sucking the slurry into a primary sand mill, sanding the slurry in a secondary sand mill in sequence, and repeatedly sanding until the particle size of the slurry is less than or equal to 5 microns; the sanding medium is a pickaxe bead with the diameter of 0.6 mm;

and step 3: and pressing the sanded slurry into a pressure type spray drying granulator through a peristaltic pump for spray drying granulation, wherein the inlet temperature of hot air is 80 ℃, and the exhaust temperature is 50 ℃.

Example 2

The pymetrozine-dinotefuran dry suspending agent comprises the following components in percentage by mass: 50% of pymetrozine technical, 20% of dinotefuran technical, 3.3% of ethoxylated tristyrylphenol potassium phosphate, 1.7% of polycarboxylate, 4% of sodium dodecyl sulfate, 4% of sodium dodecyl benzene sulfonate, 10% of sodium lignin sulfonate and 7% of light calcium.

The preparation method is the same as example 1.

Example 3

The pymetrozine-dinotefuran dry suspending agent comprises the following components in percentage by mass: 50% of pymetrozine technical, 10% of dinotefuran technical, 2% of naphthalenesulfonate, 2% of ethoxylated tristyrylphenol potassium phosphate, 5% of sodium dodecyl sulfate, 5% of sodium lignosulfonate, 10% of calcium lignosulfonate and 16% of barium sulfate.

The preparation method is the same as example 1.

Example 4

The pymetrozine-dinotefuran dry suspending agent comprises the following components in percentage by mass: 40% of pymetrozine technical, 20% of dinotefuran technical, 1% of polycarboxylate, 1% of ethoxylated tristyrylphenol potassium phosphate, 10% of sodium alkenyl sulfonate, 18% of calcium lignosulfonate and 10% of kaolin.

The preparation method is the same as example 1.

Example 5

The pymetrozine-dinotefuran dry suspending agent comprises the following components in percentage by mass: 40% of pymetrozine technical, 30% of dinotefuran technical, 1% of polycarboxylate, 2% of ethoxylated tristyrylphenol potassium phosphate, 4% of sodium dodecyl sulfate, 20% of sodium lignin sulfonate and 3% of light calcium.

The preparation method is the same as example 1.

Example 6

The pymetrozine-dinotefuran dry suspending agent comprises the following components in percentage by mass: 45% of pymetrozine technical, 25% of dinotefuran technical, 1% of polycarboxylate, 1% of ethoxylated tristyrylphenol potassium phosphate, 10% of sodium dodecyl sulfate, 12% of sodium lignin sulfonate, 3% of kaolin and 3% of light calcium.

The preparation method is the same as example 1.

Example 7

The pymetrozine-dinotefuran dry suspending agent comprises the following components in percentage by mass: 55% of pymetrozine technical, 15% of dinotefuran technical, 1.33% of polycarboxylate, 2.67% of ethoxylated potassium tristyrylphenol phosphate, 4% of sodium dodecyl sulfate, 4% of sodium alkenyl sulfonate, 15% of sodium lignin sulfonate and 3% of kaolin.

The preparation method is the same as example 1.

To further illustrate the beneficial effects of the present invention, the following comparative examples were constructed, for reasons of space only, using example 7 as an example.

Comparative example 1

The same procedure as in example 7 was repeated except that the ethoxylated potassium tristyrylphenol phosphate salt was replaced with an equal amount of the polycarboxylate.

Comparative example 2

The same conditions as in example 7 were followed except that the sodium lauryl sulfate and sodium alkenylsulfonate were replaced with the same amount of ammonium sulfate.

Comparative example 3

The polycarboxylate and ethoxylated tristyrylphenol potassium phosphate salt were replaced with equal amounts of ammonium sulfate, and the other conditions were the same as in example 7.

Comparative example 4

The sodium lignosulfonate was replaced with an equal amount of kaolin and the remaining conditions were the same as in example 7.

Comparative example 5

The sodium lignosulfonate was replaced with an equal amount of ammonium sulfate and the remaining conditions were the same as in example 7.

Comparative example 6

The kaolin was replaced with an equal amount of ammonium sulfate and the remaining conditions were the same as in example 7.

1. Detection of wetting Properties

The determination method comprises the following steps: 500ml of water were added to a measuring cylinder, 1g of the pymetrozine dinotefuran dry suspension of the above examples and comparative examples was taken in a weighing dish and poured quickly into the measuring cylinder without shaking, and the time scale for 99% of the sample to sink to the bottom of the cylinder was determined, and the results are shown in Table 1.

TABLE 1 results of measurement of wetting Properties

As can be seen from the detection data in Table 1, the pymetrozine-dinotefuran dry suspending agent prepared by the invention has good dispersibility and wettability. The use of the dispersing agent, the liquid wetting agent, the lignin and the filler in the formula improves the dispersibility and wettability of the preparation in water.

2. Determination of disintegration Property

The determination method comprises the following steps: 250ml of standard hard water is added into a measuring cylinder, and 1g of pymetrozine dinotefuran dry suspension in the above examples and comparative examples is taken. Pouring into a measuring cylinder, taking the bottom of the measuring cylinder as the center, reversing up and down at the speed of 2 s/time, and recording the disintegration times when the granules are completely disintegrated. The results are shown in Table 2.

TABLE 2 results of disintegration measurement

As can be seen from the detection data in Table 2, the pymetrozine and dinotefuran dry suspending agent solves the problems of non-fine disintegration and dead granules, and has better disintegration.

3. Determination of the suspension Rate

The test method comprises the following steps: 250ml of standard hard water is added into a measuring cylinder, and 1g of pymetrozine dinotefuran dry suspension in the above examples and comparative examples is taken. Pouring into a measuring cylinder, covering a plug, turning upside down at the speed of 2 s/time for 30 times by taking the bottom of the measuring cylinder as an axis, and standing for 30 minutes. 9/10 (i.e. 225ml) suspension of the contents was removed with a pipette within 10s-15s without shaking or picking up the sediment in the graduated cylinder. Suspension ratio W of effective component in sample₁The test results are shown in Table 3.

TABLE 3 results of suspension ratio measurement

The suspension rate is high, the pymetrozine and dinotefuran dry suspending agent needs good compatibility of auxiliaries, and the obtained dry suspending agent has high suspension rate and good effect due to the matching of polycarboxylate, ethoxylated tristyrylphenol potassium phosphate, sodium dodecyl sulfate, sodium alkenyl sulfonate, sodium lignin sulfonate and kaolin. Missing one of the components, the auxiliary agent is not matched properly, and the suspension rate is reduced.

4. Field efficacy test of cabbage diamondback moth

Due to space limitation, only field tests of the pymetrozine dinotefuran dry suspension agent in example 7 and comparative examples 1-6 on cabbage plutella xylostella were determined.

In the field test, example 7 and comparative examples 1 to 6 were set, and 8 treatments were performed with clear water, each treatment was repeated 4 times, and 32 treatment cells were performed, and 5 points were checked in each cell to investigate the number of insects. The number of worms in the population is investigated 4 times before the drug is taken as an investigation period, the number of surviving worms is investigated 2d, 7d and 14d after the drug is taken as an investigation period, the test data adopts a Duncan test New redevelopment test method (DMRT), and the results are shown in Table 4

TABLE 4 field test results of efficacy

The control effect calculation formula is as follows:

control effect (%) - (number of live insects before application-number of live insects after application) × 100/number of live insects before application

As can be seen from the test results in Table 4, the pymetrozine dinotefuran dry suspending agent of the invention has better drug effect; the data of 7d and 14d after the medicine is taken show that the control effect of the dry suspending agent of the formula is better than that of the dry suspending agent of other auxiliary agents, which proves that the dry suspending agent prepared by the invention has the advantages of fine disintegration and fine dispersion, has continuous drug effect and has a slow release function.

In conclusion, the dispersant used in the pymetrozine-dinotefuran dry suspending agent is an anionic surfactant, and the wetting agent is an anionic liquid and is matched with lignin for use, so that the pymetrozine-dinotefuran dry suspending agent has better water-entering self-dispersibility, avoids the problem of difficult disintegration and dispersion, and has no dead particles.

While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.