阅读说明：本技术 一种吡唑醚菌酯霜脲氰复配杀菌剂及其制备方法 (Pyraclostrobin cymoxanil compound bactericide and preparation method thereof ) 是由 刘建华 薛云兰 董贤娴 张晓娟 刘巍 王亚妮 于 2021-08-31 设计创作，主要内容包括：本发明公开了一种吡唑醚菌酯霜脲氰复配杀菌剂及其制备方法,杀菌剂由以下质量百分比的组分制成：吡唑醚菌酯10-20％,霜脲氰20-40％,分散剂5-20％,润湿剂1-10％,崩解剂1-10％,渗透剂1-10％,pH调节剂1-5％,消泡剂0.1-5％,余量为载体；制备方法包括以下步骤：S1、称取上述组分；S2、将吡唑醚菌酯和霜脲氰混合得到第一混合物,将第一混合物和其余原料混合得到预混合物料；S3、将预混合物料粉碎得到预处理物料；S4、将预处理物料搅拌均匀得到混合物料；S5、将混合物料与水按照1：4的质量比混合得到固液混合物料；S6、将固液混合物料造粒、干燥、筛分后得到成品。本发明公开的杀菌剂活性成分含量高、稳定性好,对作物病害的防治效果显著。(The invention discloses pyraclostrobin cymoxanil compound bactericide and a preparation method thereof, wherein the bactericide is prepared from the following components in percentage by mass: 10-20% of pyraclostrobin, 20-40% of cymoxanil, 5-20% of dispersant, 1-10% of wetting agent, 1-10% of disintegrating agent, 1-10% of penetrating agent, 1-5% of pH regulator, 0.1-5% of defoaming agent and the balance of carrier; the preparation method comprises the following steps: s1, weighing the components; s2, mixing pyraclostrobin and cymoxanil to obtain a first mixture, and mixing the first mixture and the other raw materials to obtain a premixed material; s3, crushing the premixed material to obtain a pretreated material; s4, uniformly stirring the pretreated materials to obtain mixed materials; s5, mixing the mixed material with water according to the ratio of 1:4 to obtain a solid-liquid mixed material; and S6, granulating, drying and screening the solid-liquid mixed material to obtain a finished product. The bactericide disclosed by the invention has the advantages of high content of active ingredients, good stability and obvious effect of preventing and treating crop diseases.)

1. The pyraclostrobin cymoxanil compound bactericide is characterized by being prepared from the following components in percentage by mass:

10-20% of pyraclostrobin, 20-40% of cymoxanil, 5-20% of dispersant, 1-10% of wetting agent, 1-10% of disintegrating agent, 1-10% of penetrating agent, 1-5% of pH regulator, 0.1-5% of defoaming agent and the balance of carrier.

2. The pyraclostrobin cymoxanil compound fungicide according to claim 1, wherein the dispersant is one or more of polycarboxylate and naphthalene sulfonate.

3. The pyraclostrobin cymoxanil compound fungicide according to claim 1, wherein said wetting agent is sodium dodecyl sulfate.

4. The pyraclostrobin cymoxanil compound fungicide according to claim 1, wherein said disintegrant is ammonium sulfate.

5. The pyraclostrobin cymoxanil compound bactericide as claimed in claim 1, wherein the penetrant is fatty alcohol-polyoxyethylene ether.

6. The pyraclostrobin cymoxanil compound fungicide according to claim 1, wherein said pH adjusting agent is monoammonium phosphate.

7. The pyraclostrobin cymoxanil compound bactericide as claimed in claim 1, wherein the antifoaming agent is sodium aliphatate.

8. The pyraclostrobin cymoxanil compound fungicide according to claim 1, wherein said carrier is one or more of corn starch and light calcium carbonate.

9. A preparation method of pyraclostrobin cymoxanil compound bactericide as claimed in claim 1, characterized by comprising the following steps:

s1, weighing the following raw materials in percentage by mass:

10-20% of pyraclostrobin, 20-40% of cymoxanil, 5-20% of dispersant, 1-10% of wetting agent, 1-10% of disintegrating agent, 1-10% of penetrating agent, 1-5% of pH regulator, 0.1-5% of defoaming agent and the balance of carrier;

s2, uniformly mixing the pyraclostrobin, cymoxanil and a carrier to obtain a first mixture, and uniformly mixing the first mixture with the rest raw materials to obtain a premixed material;

s3, crushing the premixed material at 0-10 ℃ until the particle size is less than or equal to 15 mu m to obtain a pretreated material;

s4, uniformly mixing the pretreated materials to obtain a mixed material;

s5, mixing water and the mixed material according to the mass ratio of 1:4, and stirring for 2min to obtain a solid-liquid mixed material;

s6, extruding and granulating the solid-liquid mixed material at the temperature of less than or equal to 30 ℃ at the rotating speed of 25r/min, drying the prepared granules at the temperature of 50-55 ℃ for 15min, and sieving to obtain the pyraclostrobin cymoxanil compound bactericide with the particle size of 1.0 mm.

10. The preparation method according to claim 9, wherein in S4, the operation of uniformly mixing the pretreated materials is specifically:

and (3) mixing the pretreated materials by using a double-cone mixer until the pretreated materials are uniform, wherein the revolution speed is 15r/min, the rotation speed is 60r/min, and the mixing time is 25-35 min.

Technical Field

The invention relates to the technical field related to crop fungicides, in particular to a pyraclostrobin cymoxanil compound fungicide and a preparation method thereof.

Background

Pyraclostrobin is a novel broad-spectrum methoxy acrylic acid snore bactericide, can finally cause cell death by inhibiting mitochondrial respiration, has the functions of protection, treatment and leaf penetration conduction, and is mainly used for preventing and treating various diseases caused by fungi on crops; cymoxanil is a highly effective, low toxicity fungicide effective against downy mildew fungi such as the genera pestilence, peronospora, and monobasic. The bactericide has low toxicity to human and livestock, is widely mixed with cymoxanil and other protective bactericides, and is used for cruciferous vegetables such as cucumbers, grapes, tomatoes, litchis, jucais and the like, tobaccos and the like. Pyraclostrobin and cymoxanil are compounded, so that the pyraclostrobin and the cymoxanil can be synergistic, and a better disease control effect is achieved for crops.

The existing pyraclostrobin cymoxanil compound bactericide has generally low content of effective components, the dosage forms are mainly wettable powder and dry suspending agent, the production cost of the wettable powder is low, but the dust often rises in the production and transportation process due to small particle size of the powder, so that the bactericide has the defects of flammability and explosiveness; the dry suspending agent has smaller particle size and higher suspension rate, but has the defects of large production energy consumption, high cost of used auxiliaries, poor drug effect durability, easy agglomeration of particles and the like.

The granulation method of the existing dry suspending agent is generally spray granulation, the spray granulation temperature needs more than 100 ℃ to dry the granules, the drying temperature is difficult to control, and the melting point of the pyraclostrobin is only 63 ℃, so that the pyraclostrobin is easy to change into a molten state during spray granulation, the dispersibility, stability and disintegration of the produced granules are poor, and the drug effect is greatly influenced; and the quality problems such as agglomeration and the like can be caused by the fact that the spray granulation particles are too fine. The water solubility of cymoxanil is high, so that the content of the cymoxanil in a finished product is reduced by spray granulation, the drug effect and the drug effect durability of the product are reduced, and the dilution times are reduced or the use times are increased to ensure the use effect in actual use.

Disclosure of Invention

Therefore, the invention provides pyraclostrobin cymoxanil compound bactericide and a preparation method thereof, and aims to solve the problems in the prior art.

In order to achieve the above object, the embodiments of the present invention provide the following technical solutions:

in a first aspect, the embodiment of the invention provides pyraclostrobin cymoxanil compound bactericide which is prepared from the following components in percentage by mass:

10-20% of pyraclostrobin, 20-40% of cymoxanil, 5-20% of dispersant, 1-10% of wetting agent, 1-10% of disintegrating agent, 1-10% of penetrating agent, 1-5% of pH regulator, 0.1-5% of defoaming agent and the balance of carrier.

Preferably, the dispersant is one or more of polycarboxylate, naphthalene sulfonate.

Preferably, the wetting agent is sodium lauryl sulfate.

Preferably, the disintegrant is ammonium sulfate.

Preferably, the osmotic agent is fatty alcohol polyoxyethylene ether.

Preferably, the pH adjusting agent is monoammonium phosphate.

Preferably, the antifoaming agent is sodium fatty acid.

Preferably, the carrier is one or more of corn starch and light calcium carbonate.

In a second aspect, an embodiment of the present invention provides a preparation method of the above fungicide, which includes the following steps:

s1, weighing the following raw materials in percentage by mass:

10-20% of pyraclostrobin, 20-40% of cymoxanil, 5-20% of dispersant, 1-10% of wetting agent, 1-10% of disintegrating agent, 1-10% of penetrating agent, 1-5% of pH regulator, 0.1-5% of defoaming agent and the balance of carrier;

s2, uniformly mixing pyraclostrobin, cymoxanil and a carrier to obtain a first mixture, and uniformly mixing the first mixture with all the other raw materials to obtain a premixed material;

s3, crushing the premixed material at 0-10 ℃ until the particle size is less than or equal to 15 mu m to obtain a pretreated material;

s4, uniformly mixing the pretreated materials to obtain a mixed material;

s5, mixing water and the mixed material according to the mass ratio of 1:4, and stirring for 2min to obtain a solid-liquid mixed material;

s6, extruding and granulating the solid-liquid mixed material at the temperature of less than or equal to 30 ℃ at the rotating speed of 25r/min, drying the prepared granules at the temperature of 50-55 ℃ for 15min, and sieving to obtain the pyraclostrobin cymoxanil compound bactericide with the particle size of 1.0 mm.

Preferably, in S4, the operation of uniformly mixing the pretreated material specifically includes:

and (3) mixing the pretreated materials by using a double-cone mixer until the pretreated materials are uniform, wherein the revolution speed is 15r/min, the rotation speed is 60r/min, and the mixing time is 25-35 min.

Compared with the prior art, the embodiment of the invention at least has the following beneficial effects:

(1) compared with the existing dry suspending agent and wettable powder, the pyraclostrobin cymoxanil compound bactericide provided by the embodiment of the invention has the advantages of low production cost and strong dispersibility, stability and disintegrability; in addition, because the solvent is not used, the processed granules are easy to flow freely, have certain strength and are easy to disintegrate, the suspension rate after dispersion is high, no dust is generated, and the use is very safe and efficient.

(2) The pyraclostrobin cymoxanil compound bactericide provided by the embodiment of the invention adopts low-temperature crushing, low-temperature drying and low-temperature extrusion granulation to replace the traditional high-temperature spray granulation and drying method during preparation, and solves the problems of particle agglomeration, poor dispersibility, poor disintegrability, pesticide effect loss and the like caused by denaturation and melting of pyraclostrobin at high temperature.

(3) The pyraclostrobin cymoxanil compound bactericide provided by the embodiment of the invention does not need to use a solvent during preparation, removes water in particles by low-temperature drying, and can prevent the problems of bactericide efficacy deterioration and the like caused by excessive dissolution of cymoxanil in water.

(4) The pyraclostrobin cymoxanil compound bactericide provided by the embodiment of the invention has the advantages of good dispersibility, high suspension rate, high product stability, convenience for storage and use, simple preparation process and convenience for realizing large-scale commercial production; the pesticide has strong pesticide effect and strong permeability, and particularly has excellent control effect on downy mildew, powdery mildew and the like; and because of high drug effect, agricultural workers can achieve the same or better effect with less dosage compared with the prior bactericide when using the product, thereby reducing the use cost and the pollution to the environment.

Detailed description of the invention

In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is further described in detail with reference to specific embodiments below. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.

In the description of the present invention, "a plurality" means two or more unless otherwise specified.

Furthermore, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements specifically listed, but may include other steps or elements not expressly listed that are inherent to such process, method, article, or apparatus or that are added to such process, method, article, or apparatus based on the optimization concepts of the present invention.

The specific conditions of the examples 1-3 are shown in tables 1 and 2, wherein the table 1 shows the mass percent of each component of the examples 1-3, and the table 2 shows the specific component conditions of each component of the examples 1-3 except for pyraclostrobin and cymoxanil.

TABLE 1-examples 1 to 3 percentages by mass of the respective components

TABLE 2 specific ingredients for each of the components of examples 1-3

The preparation of example 1 is as follows:

s1, weighing the following raw materials in percentage by mass:

20% of pyraclostrobin, 40% of cymoxanil, 8% of polycarboxylate, 7% of naphthalenesulfonate, 2% of sodium dodecyl sulfate, 5% of ammonium sulfate, 6% of fatty alcohol-polyoxyethylene ether, 1.5% of monoammonium phosphate, 1.5% of sodium fatty acid, 5% of corn starch and 8% of light calcium carbonate;

s2, uniformly mixing pyraclostrobin, cymoxanil, corn starch and light calcium carbonate to obtain a first mixture, and uniformly mixing the first mixture with all the other raw materials to obtain a premixed material;

s3, crushing the premixed material at 8 ℃ until the particle size is less than or equal to 15 mu m to obtain a pretreated material;

s4, placing the pretreated material in a double-cone mixer, and mixing the pretreated material for 30min at the revolving speed of the mixer of 15r/min and the self-transmission speed of 60r/min to obtain a mixed material;

s5, mixing water and the mixed material according to the mass ratio of 1:4, and stirring for 2min to obtain a solid-liquid mixed material;

s6, extruding and granulating the solid-liquid mixed material at the temperature of 25 ℃ at the rotating speed of 25r/min, drying the prepared granules at the temperature of 50 ℃ for 15min, and sieving to obtain the pyraclostrobin cymoxanil compound bactericide with the particle size of 1.0 mm.

Examples 2-3 were prepared in the same manner as in example 1.

Next, performance tests were performed on the pyraclostrobin cymoxanil compound fungicide provided in examples 1-3 to demonstrate the beneficial effects of the present invention.

Test 1: determination of performance parameters

The performance parameters of the fungicides provided in examples 1 to 3 were measured, and the results are shown in Table 3.

TABLE 3 examples 1-3 Performance parameters

Test item and superior standard	Example 1	Example 2	Example 3
				Pyraclostrobin mass fraction%	20.03	10.01	10.02
Cymoxanil in mass fraction%	40.02	20.04	40.03
				Water% (≦ 3.0)	1.2	1.5	1.6
PH range (6- - -9)	6.9	6.7	6.8
				Wetting time S (less than or equal to 90S)	26	33	31
Pyraclostrobin suspension% (≧ 75)	91	94	88
				Cymoxanil suspension% (≧ 75)	99	97	96
Particle size (mum) (≦ 44 μm)	11	13	13
				% dispersibility (not less than 75)	88	85	84
Lasting foam (after 1 min) is less than or equal to 60ml	22	34	17
				Wet sieve test (passing 75 μm test sieve)%	99.9	99.9	99.9
Particle size range (420-	98	97	94
				Heat storage stability (54 ℃ +/-2 ℃) for 14 days	Qualified	Qualified	Qualified

And (3) testing 2: prevention and efficacy test

Setting treatment groups 1-5, and respectively testing the control effect of the tester on cucumber downy mildew; the treatment groups 1 to 3 are experimental groups, all the bactericides are pyraclostrobin cymoxanil compound bactericides provided by the embodiment 1 of the application, the treatment groups 4 to 5 are control groups, wherein the bactericide used in the treatment group 4 is a commercially available pyraclostrobin single agent, and the bactericide used in the treatment group 5 is a cymoxanil single agent with the concentration of 66 wt%. The application rates for each treatment group are shown in table 4; at the early stage of the onset of cucumber downy mildew, the spraying method is used for first application, then the spraying method is used for applying the medicine once every 7-10 days, the application is carried out three times, the disease index and the control effect are measured 7 days after each application, 7 days after the last application, the control effect conditions of the groups 1-5 are statistically processed, and the results are shown in table 5.

TABLE 4-treatment groups 1-5 application rates

Process group numbering	The bactericide is	Application rate
			1	Example 1	10 g/mu
2	Example 1	15 g/mu
			3	Example 1	20 g/mu
4	Pyraclostrobin single agent	30 g/mu
			5	66 wt% cymoxanil monomer	45 g/mu

TABLE 5-treatment groups 1-5 control efficacy

Test results show that the control effects of the treatment groups 1-3 after the first, second and third medicines are all excellent in 7 days, particularly the treatment groups 2 and 3 are far superior to the treatment groups 4 and 5 in performance, and the drug effect is particularly prominent; from the control effect after 7 days of the third drug, the drug effect persistence of the treatment groups 1 to 3 is higher than that of the treatment groups 4 and 5. And the treatment groups 1 to 3 have no adverse effect on the growth of the cucumbers in the whole pesticide effect test process.

The conclusion fully proves that the bactericidal composition has good control effect on downy mildew, has lasting pesticide effect, and is safe and reliable to crops within the range of test dosage.

All the technical features of the above embodiments can be combined arbitrarily, and for simplicity of description, all possible combinations of the technical features of the above embodiments are not described; these examples, which are not explicitly described, should be considered to be within the scope of the present description.

The present invention has been described in considerable detail by the general description and the specific examples given above. It should be noted that it is obvious that several variations and modifications can be made to these specific embodiments without departing from the inventive concept, which falls within the scope of protection of the present application. Therefore, the protection scope of the present patent shall be subject to the appended claims.