CN117158419B - Cyhalothrin thiamethoxam microcapsule suspension and preparation method thereof - Google Patents
Cyhalothrin thiamethoxam microcapsule suspension and preparation method thereof Download PDFInfo
- Publication number
- CN117158419B CN117158419B CN202311445586.8A CN202311445586A CN117158419B CN 117158419 B CN117158419 B CN 117158419B CN 202311445586 A CN202311445586 A CN 202311445586A CN 117158419 B CN117158419 B CN 117158419B
- Authority
- CN
- China
- Prior art keywords
- thiamethoxam
- cyhalothrin
- microcapsule
- agent
- microcapsule suspension
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000005941 Thiamethoxam Substances 0.000 title claims abstract description 102
- NWWZPOKUUAIXIW-FLIBITNWSA-N thiamethoxam Chemical compound [O-][N+](=O)\N=C/1N(C)COCN\1CC1=CN=C(Cl)S1 NWWZPOKUUAIXIW-FLIBITNWSA-N 0.000 title claims abstract description 101
- 239000003094 microcapsule Substances 0.000 title claims abstract description 92
- ZXQYGBMAQZUVMI-UNOMPAQXSA-N cyhalothrin Chemical compound CC1(C)C(\C=C(/Cl)C(F)(F)F)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-UNOMPAQXSA-N 0.000 title claims abstract description 66
- 239000000725 suspension Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 40
- 239000002270 dispersing agent Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000375 suspending agent Substances 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000006229 carbon black Substances 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000000230 xanthan gum Substances 0.000 claims abstract description 14
- 229920001285 xanthan gum Polymers 0.000 claims abstract description 14
- 229940082509 xanthan gum Drugs 0.000 claims abstract description 14
- 235000010493 xanthan gum Nutrition 0.000 claims abstract description 14
- 241001124076 Aphididae Species 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 239000012071 phase Substances 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 13
- 239000001856 Ethyl cellulose Substances 0.000 claims description 11
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 11
- 229920001249 ethyl cellulose Polymers 0.000 claims description 11
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000012074 organic phase Substances 0.000 claims description 10
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 239000003995 emulsifying agent Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000004546 suspension concentrate Substances 0.000 claims description 4
- 230000000295 complement effect Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 25
- 231100000584 environmental toxicity Toxicity 0.000 abstract 1
- 239000000575 pesticide Substances 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 15
- 239000003814 drug Substances 0.000 description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 9
- 238000005507 spraying Methods 0.000 description 9
- 241000238631 Hexapoda Species 0.000 description 8
- 230000002265 prevention Effects 0.000 description 6
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 5
- 240000003768 Solanum lycopersicum Species 0.000 description 5
- 239000002775 capsule Substances 0.000 description 5
- 238000005538 encapsulation Methods 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 239000011162 core material Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000002917 insecticide Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000009931 harmful effect Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 241000238876 Acari Species 0.000 description 1
- 240000007124 Brassica oleracea Species 0.000 description 1
- 235000003899 Brassica oleracea var acephala Nutrition 0.000 description 1
- 235000011301 Brassica oleracea var capitata Nutrition 0.000 description 1
- 235000001169 Brassica oleracea var oleracea Nutrition 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 241000219146 Gossypium Species 0.000 description 1
- 240000005979 Hordeum vulgare Species 0.000 description 1
- 235000007340 Hordeum vulgare Nutrition 0.000 description 1
- 244000141359 Malus pumila Species 0.000 description 1
- 241000207836 Olea <angiosperm> Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 244000098338 Triticum aestivum Species 0.000 description 1
- 241000219094 Vitaceae Species 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 235000021016 apples Nutrition 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 210000003050 axon Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 235000021021 grapes Nutrition 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000003090 pesticide formulation Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000011197 physicochemical method Methods 0.000 description 1
- 244000000003 plant pathogen Species 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 235000012015 potatoes Nutrition 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000002728 pyrethroid Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The application discloses a cyhalothrin thiamethoxam microcapsule suspension and a preparation method thereof. On one hand, the application provides a cyhalothrin thiamethoxam microcapsule suspension suspending agent, which comprises cyhalothrin and thiamethoxam microcapsules, wherein the cyhalothrin thiamethoxam microcapsule suspension suspending agent comprises the following components in percentage by mass: 6-8% of cyhalothrin, 10-30% of thiamethoxam microcapsule, 4-8% of dispersing agent, 0.5-1.5% of xanthan gum, 1-3% of white carbon black, 0.1-0.5% of antifreezing agent and the balance of water; the effective content of thiamethoxam is 14-16%. On the other hand, the application also provides a preparation method and application of the cyhalothrin thiamethoxam microcapsule suspension. The aphid control method can be used for rapidly and permanently controlling aphids, and is low in environmental toxicity and good in control effect.
Description
Technical Field
The application relates to the technical field of pesticides, in particular to a cyhalothrin thiamethoxam microcapsule suspension and a preparation method thereof.
Background
Pests, diseases and weeds are major threats to the loss and degradation of crops. It is estimated that about 9000 insects and mites, 8000 weeds, 50000 plant pathogens can cause damage to crops worldwide. Therefore, the application of pesticides to protect crops and promote sustainable development of agriculture is essential. However, the long-term extensive and inefficient use of pesticides poses serious environmental and human health hazards. There are data showing that 80% of the pesticide is actually lost due to biodegradation, chemical degradation, photodecomposition and evaporation, and the actual application rate of the pesticide is extremely low. The pesticide microcapsule is a brand new pesticide formulation, and is expected to solve the problems.
The cyhalothrin is also called as high-efficiency cyhalothrin, is a broad-spectrum pyrethroid insecticide, has the function of avoiding and killing insects, is mainly applied to nerve axon parts of the insects, is widely applied to the fields of agriculture in China and the like, and is used for crops such as cotton, apples, potatoes, wheat, barley, rice, tomatoes, olives, cabbages, soybeans, grapes, corn and the like. Cyhalothrin is easy to dissolve in methanol, solvent oil, acetone and organic solvent and stable under illumination, but cyhalothrin has irritation to human skin and has pungent smell, so that the application of cyhalothrin is limited.
The pesticide microcapsule is prepared by wrapping the active ingredients of the pesticide with natural, semi-natural or artificial polymer materials by a chemical method, a physical method or a physicochemical method to form a microcapsule with a semipermeable or sealed capsule membrane, and adding other auxiliary agents to enable the microcapsule to be stably dispersed and suspended in water to form a uniform and stable solid-liquid dispersion system. The microcapsule particle size is generally 1-1000 μm, the film forming material is called capsule wall or capsule wall material, and the coated active ingredient is called capsule core or core material. The microcapsules are generally spherical in shape, or may be oval, kidney, valley, or amorphous, and may be single-core or multi-core. Traditional pesticides and pesticides with skin irritation or pungent odor to human bodies can overcome part of defects of the traditional pesticides by the technical means of pesticide microcapsules.
At present, pesticide agents compounded by cyhalothrin and thiamethoxam exist in the prior art; the method not only uses the cyhalothrin to prepare the microcapsule compound thiamethoxam, but also uses the thiamethoxam to prepare the microcapsule compound cyhalothrin. The existing medicines have limited control effects on aphids, and a certain dosage is needed to obtain a good control effect. And the large dosage of the medicine can certainly cause the problem of environmental pollution.
Disclosure of Invention
In order to solve at least one technical problem, a pesticide product which can quickly and permanently control aphids, has low environmental pollution and good control effect is developed.
On the one hand, the application provides a cyhalothrin thiamethoxam microcapsule suspension suspending agent, which comprises cyhalothrin and thiamethoxam microcapsules, wherein the mass fraction ratio of each component is as follows: 6-8% of cyhalothrin, 10-30% of thiamethoxam microcapsule, 4-8% of dispersing agent, 0.5-1.5% of xanthan gum, 1-3% of white carbon black, 0.1-0.5% of antifreezing agent and the balance of water; the effective content of thiamethoxam is 14-16%.
By adopting the technical scheme, the suspension suspending agent of the cyhalothrin and thiamethoxam microcapsules is prepared by adopting the cyhalothrin and thiamethoxam microcapsules with specific proportion, the effective content of the cyhalothrin is controlled within 8%, and the thiamethoxam exists in the microcapsules, so that the toxic and harmful effects on the environment during spraying can be effectively reduced; in the method, xanthan gum and white carbon black are used as stabilizers, and dispersing agents are used as auxiliary materials, so that the prepared suspending agent has good stability; the cyhalothrin and thiamethoxam microcapsule has a rapid and durable effect on aphid control through reasonable medicine compatibility, and the medicine effect can be more than 24 days.
Optionally, the thiamethoxam microcapsule adopts ethyl cellulose.
Optionally, the white carbon black adopts nanoscale powder.
Optionally, the dispersing agent adopts Morwet D-425 dispersing agent, sodium lignosulfonate and polyvinyl alcohol compound dispersing agent.
Further alternatively, the mass ratio of the Morwet D-425 dispersant to the sodium lignosulfonate to the polyvinyl alcohol in the dispersant is 1:1: 2-3.
Further alternatively, the thiamethoxam microcapsule is prepared by dissolving thiamethoxam and ethyl cellulose serving as raw materials in ethyl acetate to prepare an organic phase; dissolving TWN-80 emulsifying agent in water to prepare water phase; injecting the organic phase and the water phase into a microchannel reactor, and mixing at normal temperature until the particle size is less than 2 mu m; and then introducing the mixed solution into a pipeline reactor, heating to 65-70 ℃ until the ethyl acetate is completely volatilized, and thus obtaining the thiamethoxam microcapsule.
By adopting the technical scheme, the micro-channel reactor is adopted to carry out the mixing reaction of the oil phase and the water phase, so that particles with smaller particle size can be prepared, and the particle size of the prepared thiamethoxam micro-capsule can be controlled within 1.2 mu m; the micro-channel reactor is used for mixing, so that the encapsulation rate of the micro-capsules is effectively improved, the decomposition rate is reduced, and the encapsulation rate can reach more than 99.5%.
Optionally, the mass fraction ratio of each component is as follows: 6.8% of cyhalothrin, 24% of thiamethoxam microcapsule, 5% of dispersing agent, 0.8% of xanthan gum, 2.2% of white carbon black, 0.2% of antifreezing agent and the balance of water; the effective content of thiamethoxam is 15.2%.
In a second aspect, the present application also provides a preparation method of the above cyhalothrin thiamethoxam microcapsule suspension, comprising the following steps:
s1, preparing thiamethoxam microcapsules by adopting the steps;
s2, adding dispersing agent, xanthan gum, white carbon black and antifreezing agent in the formula amount into the thiamethoxam microcapsule suspension obtained in the step S1 in sequence, and stirring and mixing to obtain a mixed solution;
s3, adding the cyhalothrin with the formula amount into the mixed solution prepared in the step S2, adding water to complement the formula amount of water, and magnetically stirring and fully mixing to prepare the cyhalothrin thiamethoxam microcapsule suspension suspending agent.
Optionally, in the step S2, the stirring rotation speed of stirring and mixing is controlled to be 100-200 rpm, and the time is 10-20 min.
In a third aspect, the application also provides an application of the cyhalothrin thiamethoxam microcapsule suspension in aphid control and field.
In summary, the present invention includes at least one of the following beneficial technical effects:
1. the suspension suspending agent of the cyhalothrin and thiamethoxam microcapsules is prepared by adopting the cyhalothrin and thiamethoxam microcapsules with specific proportion, the effective content of the cyhalothrin is controlled within 8%, and the thiamethoxam exists in the microcapsules, so that the toxic and harmful effects on the environment during spraying can be effectively reduced.
2. According to the preparation method, xanthan gum and white carbon black are used as stabilizers, and dispersing agents are used as auxiliary materials, so that the prepared suspending agent has good stability.
3. The cyhalothrin and thiamethoxam microcapsule has a rapid and durable effect on aphid control through reasonable medicine compatibility, and the medicine effect can be more than 24 days.
4. According to the method, the micro-channel reactor is adopted to carry out the mixing reaction of the oil phase and the water phase, so that particles with smaller particle sizes can be prepared, and the particle size of the prepared thiamethoxam micro-capsule can be controlled within 1.2 mu m; the micro-channel reactor is used for mixing, so that the encapsulation rate of the micro-capsules is effectively improved, the decomposition rate is reduced, and the encapsulation rate can reach more than 99.5%.
Drawings
FIG. 1 is a photograph of seedlings of the control effect test of the present application.
Detailed Description
The present application is described in further detail below with reference to the drawings and examples.
The application designs a cyhalothrin thiamethoxam microcapsule suspension suspending agent, which comprises cyhalothrin and thiamethoxam microcapsules, wherein the mass fraction ratio of each component is as follows: 6-8% of cyhalothrin, 10-30% of thiamethoxam microcapsule, 4-8% of dispersing agent, 0.5-1.5% of xanthan gum, 1-3% of white carbon black, 0.1-0.5% of antifreezing agent and the balance of water; the effective content of thiamethoxam is 14-16%.
The thiamethoxam microcapsule of the application is prepared in the following manner: dissolving thiamethoxam and ethyl cellulose serving as raw materials in ethyl acetate to prepare an organic phase; dissolving TWN-80 emulsifying agent in water to prepare water phase; injecting the organic phase and the water phase into a microchannel reactor, and mixing at normal temperature until the particle size is less than 2 mu m; and then introducing the mixed solution into a pipeline reactor, heating to 65-70 ℃ until the ethyl acetate is completely volatilized, and thus obtaining the thiamethoxam microcapsule.
The preparation method of the cyhalothrin thiamethoxam microcapsule suspension comprises the following steps:
s1, preparing thiamethoxam microcapsules by adopting the steps;
s2, adding the dispersing agent, the xanthan gum, the white carbon black and the antifreezing agent in the formula amount into the thiamethoxam microcapsule suspension obtained in the step S1 in sequence, stirring and mixing, wherein the stirring speed is controlled to be 100-200 rpm, and the time is 10-20 min, so as to obtain a mixed solution;
s3, adding the cyhalothrin with the formula amount into the mixed solution prepared in the step S2, adding water to complement the formula amount of water, and magnetically stirring and fully mixing to prepare the cyhalothrin thiamethoxam microcapsule suspension suspending agent.
The following is a preparation example of thiamethoxam microcapsule preparation in the present application.
Preparation example 1
The thiamethoxam microcapsule prepared by the preparation method comprises the following steps:
s1-1, dissolving the original medicine thiamethoxam and ethyl cellulose in ethyl acetate according to a feeding ratio of 1:1, and preparing an organic phase by taking the addition amount of the ethyl acetate as the standard of completely dissolving the original medicine thiamethoxam and the ethyl cellulose;
s1-2, dissolving TWN-80 emulsifying agent in water to prepare 0.5% solution, so as to obtain water phase;
s1-3, injecting the organic phase obtained in the step S1-1 and the water phase obtained in the step S1-2 into a micro-channel reactor according to a feeding ratio of 1:3 by volume, and mixing at normal temperature until the particle size is within 2 mu m to obtain a mixed solution;
s1-4, introducing the mixed solution obtained in the step S1-3 into a pipeline reactor, and heating to 70 ℃ until the ethyl acetate is completely volatilized, so as to prepare the thiamethoxam microcapsule preparation;
s1-5, filtering the thiamethoxam microcapsule preparation obtained in the step S1-4 by using a 0.22 mu m filter membrane to remove water, and airing to obtain the thiamethoxam microcapsule.
Preparation example 2
The thiamethoxam microcapsule prepared by the preparation method comprises the following steps:
s1-1, dissolving the crude drug thiamethoxam and ethyl cellulose in ethyl acetate according to a feeding ratio of 1:1.5, wherein the adding amount of the ethyl acetate is based on the complete dissolution of the crude drug thiamethoxam and the ethyl cellulose, and preparing an organic phase;
s1-2, dissolving TWN-80 emulsifying agent in water to prepare 0.5% solution, so as to obtain water phase;
s1-3, injecting the organic phase obtained in the step S1-1 and the water phase obtained in the step S1-2 into a micro-channel reactor according to a feeding ratio of 1:4 by volume, and mixing at normal temperature until the particle size is within 2 mu m to obtain a mixed solution;
s1-4, introducing the mixed solution obtained in the step S1-3 into a pipeline reactor, and heating to 65 ℃ until the ethyl acetate is completely volatilized, so as to prepare the thiamethoxam microcapsule preparation;
s1-5, filtering the thiamethoxam microcapsule preparation obtained in the step S1-4 by using a 0.22 mu m filter membrane to remove water, and airing to obtain the thiamethoxam microcapsule.
Preparation example 3
The difference between this preparation and preparation 1 is that this preparation replaces the ethylcellulose of preparation 1 with an equal amount of carboxymethyl cellulose.
Preparation example 4
This preparation differs from preparation 2 in that the same amount of carboxymethyl cellulose was used instead of ethyl cellulose of preparation 1.
Sampling and detecting when thiamethoxam microcapsule preparations are prepared in preparation examples 1-4, and calculating the encapsulation rate by detecting the content of free thiamethoxam; and (3) detecting the particle size distribution of the thiamethoxam microcapsules prepared in preparation examples 1-4 by using a laser particle size meter, and detecting the particle size distribution of the microcapsules.
The thiamethoxam microcapsule prepared in preparation examples 1-4 has a capsule forming rate of over 99.5 percent and a particle size of 2 mu m. The particle size distribution of preparation example 1 was the most average as measured by a laser particle size meter, and thiamethoxam microcapsules prepared in preparation example 1 were used in the subsequent examples of the present application.
Examples 1 to 7 of the present application are as follows.
Example 1
The mass fraction ratio of each component in the embodiment is as follows: 6% of cyhalothrin, 10% of thiamethoxam microcapsule, 4% of dispersing agent, 0.5% of xanthan gum, 1% of white carbon black, 0.1% of antifreezing agent and the balance of water; the effective content of thiamethoxam is 14%.
The dispersing agent of the embodiment adopts sodium lignosulfonate, the white carbon black adopts micron-sized powder, and the antifreezing agent adopts glycerol.
The preparation of this example was carried out using the preparation method described previously herein.
Example 2
The mass fraction ratio of each component in the embodiment is as follows: 8% of cyhalothrin, 30% of thiamethoxam microcapsule, 8% of dispersing agent, 1.5% of xanthan gum, 3% of white carbon black, 0.5% of antifreezing agent and the balance of water; the effective content of thiamethoxam is 16%.
The dispersing agent of the embodiment adopts sodium lignosulfonate, the white carbon black adopts micron-sized powder, and the antifreezing agent adopts glycerol.
The preparation of this example was carried out using the preparation method described previously herein.
Example 3
The mass fraction ratio of each component in the embodiment is as follows: 6.8% of cyhalothrin, 24% of thiamethoxam microcapsule, 5% of dispersing agent, 0.8% of xanthan gum, 2.2% of white carbon black, 0.2% of antifreezing agent and the balance of water; the effective content of thiamethoxam is 15.2%.
The dispersing agent of the embodiment adopts sodium lignosulfonate, the white carbon black adopts micron-sized powder, and the antifreezing agent adopts glycerol.
The preparation of this example was carried out using the preparation method described previously herein.
Example 4
The difference between this example and example 3 is that the white carbon black of this example uses nano-sized powder.
Example 5
The difference between the present example and example 4 is that the dispersant of the present example adopts Morwet D-425 dispersant, sodium lignosulfonate and polyvinyl alcohol compound dispersant, and the mass ratio of the three is 1:1:1.
example 6
The difference between the present example and example 4 is that the dispersant of the present example adopts Morwet D-425 dispersant, sodium lignosulfonate and polyvinyl alcohol compound dispersant, and the mass ratio of the three is 1:1:3.
example 7
The difference between the present example and example 4 is that the dispersant of the present example adopts Morwet D-425 dispersant, sodium lignosulfonate and polyvinyl alcohol compound dispersant, and the mass ratio of the three is 1:1:2.
comparative example 1
Formula 3 of chinese patent publication No. CN113519545a provides an insecticide.
Comparative example 2
First, 24.7% efficient cyhalothrin-thiamethoxam microcapsule suspending agent produced by Zhengda company.
Comparative example 3
Based on the embodiment 3 of the application, the contents of the cyhalothrin and thiamethoxam microcapsules are only adjusted, and the contents of the other components are not changed at all.
The content of cyhalothrin is regulated to 12%, and the content of thiamethoxam microcapsule is regulated to 12% of thiamethoxam effective content.
The cyhalothrin thiamethoxam microcapsule suspension suspending agent of examples 1-7 and the insecticide of comparative examples 1-3 are subjected to a control effect detection experiment respectively, and the control effect is detected.
The control effect detection experiment adopts the following method:
in a greenhouse, transplanting tomato seedlings with 4 leaves, transplanting 11 groups of 10 plants each, and 110 tomato seedlings. Each seedling of each group was planted individually, and the planting of each group of seedlings was as shown in the photograph of fig. 1. The temperature of the greenhouse is maintained at 24+/-2 ℃ and the humidity is 75%, 12 hours of illumination is maintained every day, normal planting is carried out, and watering is carried out every 6 days. The experiment was set up with 10 dosing groups and 1 blank group.
And spraying the suspension concentrate of the cyhalothrin thiamethoxam microcapsules of the examples 1-7 and the pesticides of the comparative examples 1-3 on the tomato seedlings of 10 pesticide application groups according to the dosage of 0.3mL sprayed on each group, and manually spraying to ensure that the front and the back of the leaves of each seedling are sprayed on the pesticide.
After application, on days 1, 8, 16 and 24, each leaf of each tomato seedling was inoculated with a population of healthy aphids raised artificially; after each inoculation of the aphid population, the number of residual insects was checked after 48 hours, the rate of killing the insects was calculated, and then all the residual insects were manually removed.
The control effect is calculated by the following formula:
control efficiency = [ (insect killing rate of the group-blank group)/(insect killing rate of 100-blank group) ] × 100%
The results obtained in this experiment are shown in tables 1 and 2 below.
Table 1 pesticide application group and blank group deinsectization rate
| 1 day deinsectization rate (%) | Deinsectization rate in 8 days (%) | Deinsectization rate in 16 days (%) | Rate of deinsectization in 24 days (%) | |
| Example 1 | 100 | 97.0 | 91.9 | 83.0 |
| Example 2 | 100 | 97.3 | 92.3 | 84.1 |
| Example 3 | 100 | 97.7 | 92.6 | 84.8 |
| Example 4 | 100 | 98.4 | 93.5 | 86.3 |
| Example 5 | 100 | 98.5 | 93.8 | 86.9 |
| Example 6 | 100 | 98.5 | 93.8 | 87.1 |
| Example 7 | 100 | 98.7 | 94.0 | 87.3 |
| Comparative example 1 | 98.4 | 86.5 | 66.9 | 36.9 |
| Comparative example 2 | 100 | 91.2 | 76.7 | 56.7 |
| Comparative example 3 | 100 | 91.8 | 74.6 | 54.3 |
| Blank group | -9.6 | -34.8 | -71.4 | -114.6 |
Table 2 examples 1 to 7 and comparative examples 1 to 3 were found to be effective in controlling
| 1 day control effect (%) | 8 days prevention effect (%) | 16 days of preventive effect (%) | 24-day control effect (%) | |
| Example 1 | 100 | 97.8 | 95.3 | 92.1 |
| Example 2 | 100 | 98.0 | 95.5 | 92.6 |
| Example 3 | 100 | 98.3 | 95.7 | 92.9 |
| Example 4 | 100 | 98.8 | 96.2 | 93.6 |
| Example 5 | 100 | 98.9 | 96.4 | 93.9 |
| Example 6 | 100 | 98.9 | 96.4 | 94.0 |
| Example 7 | 100 | 99.0 | 96.5 | 94.1 |
| Comparative example 1 | 98.5 | 90.0 | 80.7 | 70.6 |
| Comparative example 2 | 100 | 93.5 | 86.4 | 79.8 |
| Comparative example 3 | 100 | 93.9 | 85.2 | 78.7 |
As can be seen from the data in tables 1 and 2, the cyhalothrin thiamethoxam microcapsule suspension suspending agent in examples 1-7 has the control effect reaching about 98% by the 8 th day and 92% by the 24 th day, the disinsection rate still can be maintained at more than 80%, and the spraying and watering once every 6 days has no great influence on the cyhalothrin thiamethoxam microcapsule suspension suspending agent. As can be seen from the data in tables 1 and 2, the spraying amount of the pesticide in comparative examples 1-3 is greater than or equal to the spraying amount of the pesticide in the application, however, the prevention effect on the 8 th day is less than 95%, the prevention effect on the 24 th day is less than 80%, and the disinsection rate is reduced to less than 60%. Therefore, the cyhalothrin thiamethoxam microcapsule suspension suspending agent has good blade adhesion performance, is not easily affected by watering, rain washing and the like, has relatively durable pesticide effect, and can still achieve about 92% of prevention effect on 24 days, which is far beyond that of the pesticide of comparative examples 1-3.
As can be seen from the data in tables 1 and 2, the cyhalothrin thiamethoxam microcapsule suspension suspending agent of example 4 of the present application has a significantly better control effect than the suspending agents of examples 1 to 3; the cyhalothrin thiamethoxam microcapsule suspension suspending agent of the embodiments 5-7 has better control effect than the suspending agent of the embodiment 4, so that the suspending agent of the embodiment 7 has optimal performance. The applicant speculates that the adoption of the nano-scale white carbon black can further enhance the adhesive property of the medicament and ensure the lasting effectiveness of the medicament; meanwhile, the compounded dispersing agent is adopted, and after a specific compounding ratio is adopted, the white carbon black can be effectively dispersed in the suspending agent, the effective components of the pesticide can be effectively dispersed, and the effective components and the white carbon black form physical complexation, so that the effective components of the suspending agent can be ensured to be attached to plant leaves as much as possible.
From the data in tables 1 and 2, comparing the data in examples 1-7 with the data in comparative example 3, it can be seen that the total effective dose of the preparation is controlled at 26% after the content of cyhalothrin is increased and the effective content of thiamethoxam is reduced, but the prevention effect is obviously and greatly reduced. Thus, a large dose of cyhalothrin is not easily attached to the leaves for a long period of time for the present application, and thus the prevention effect is significantly reduced.
In addition, the dosage of the cyhalothrin is controlled within 8%, the optimal spraying amount of the medicament spraying is 60 mL/mu, the dosage of the cyhalothrin is extremely low, no pungent smell exists or the cyhalothrin is stimulated to a human body, and the environment pollution is small.
The foregoing are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in any way, therefore: all equivalent changes in structure, shape and principle of this application should be covered in the protection scope of this application.
Claims (6)
1. The suspension suspending agent is characterized by comprising cyhalothrin and thiamethoxam microcapsules, wherein the mass fraction ratio of the components is as follows: 6-8% of cyhalothrin, 10-30% of thiamethoxam microcapsule, 4-8% of dispersing agent, 0.5-1.5% of xanthan gum, 1-3% of white carbon black, 0.1-0.5% of antifreezing agent and the balance of water; the dispersing agent adopts Morwet D-425 dispersing agent, sodium lignosulfonate and polyvinyl alcohol compound dispersing agent; the effective content of thiamethoxam is 14-16%; the thiamethoxam microcapsule adopts ethyl cellulose; the thiamethoxam microcapsule is prepared by dissolving thiamethoxam serving as a raw material and ethyl cellulose in ethyl acetate to prepare an organic phase; dissolving TWN-80 emulsifying agent in water to prepare water phase; injecting the organic phase and the water phase into a microchannel reactor, and mixing at normal temperature until the particle size is less than 2 mu m; then, introducing the mixed solution into a pipeline reactor, heating to 65-70 ℃ until the ethyl acetate is completely volatilized, and obtaining thiamethoxam microcapsules; among the dispersing agents, the Morwet D-425 dispersing agent, sodium lignosulfonate and polyvinyl alcohol have the mass ratio of 1:1: 2-3.
2. The cyhalothrin thiamethoxam microcapsule suspension concentrate according to claim 1, wherein the white carbon black is nano-scale powder.
3. The cyhalothrin thiamethoxam microcapsule suspension suspending agent disclosed in claim 1 is characterized by comprising the following components in parts by mass: 6.8% of cyhalothrin, 24% of thiamethoxam microcapsule, 5% of dispersing agent, 0.8% of xanthan gum, 2.2% of white carbon black, 0.2% of antifreezing agent and the balance of water; the effective content of thiamethoxam is 15.2%.
4. A method for preparing the cyhalothrin thiamethoxam microcapsule suspension concentrate of claim 1, comprising the following steps:
s1, preparing thiamethoxam microcapsules by adopting the steps of claim 1;
s2, adding dispersing agent, xanthan gum, white carbon black and antifreezing agent in the formula amount into the thiamethoxam microcapsule suspension obtained in the step S1 in sequence, and stirring and mixing to obtain a mixed solution;
s3, adding the cyhalothrin with the formula amount into the mixed solution prepared in the step S2, adding water to complement the formula amount of water, and magnetically stirring and fully mixing to prepare the cyhalothrin thiamethoxam microcapsule suspension suspending agent.
5. The method for preparing the cyhalothrin thiamethoxam microcapsule suspension suspending agent according to claim 4, wherein in the step S2, the stirring rotation speed of stirring and mixing is controlled to be 100-200 rpm, and the time is controlled to be 10-20 min.
6. Use of a cyhalothrin thiamethoxam microcapsule suspension concentrate according to claim 1 in the field of aphid control.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311445586.8A CN117158419B (en) | 2023-11-02 | 2023-11-02 | Cyhalothrin thiamethoxam microcapsule suspension and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311445586.8A CN117158419B (en) | 2023-11-02 | 2023-11-02 | Cyhalothrin thiamethoxam microcapsule suspension and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN117158419A CN117158419A (en) | 2023-12-05 |
| CN117158419B true CN117158419B (en) | 2024-02-06 |
Family
ID=88939796
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311445586.8A Active CN117158419B (en) | 2023-11-02 | 2023-11-02 | Cyhalothrin thiamethoxam microcapsule suspension and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117158419B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102396508A (en) * | 2011-11-24 | 2012-04-04 | 陕西美邦农药有限公司 | Novel pesticide combination containing thiamethoxam |
| CN109452304A (en) * | 2018-11-13 | 2019-03-12 | 中国农业大学 | Dinotefuran microcapsule suspending agent and preparation method thereof |
| CN113519545A (en) * | 2021-07-15 | 2021-10-22 | 孟州市华丰生化农药有限公司 | Thiamethoxam microcapsule seed treatment suspending agent and application thereof |
| CN114600877A (en) * | 2022-03-29 | 2022-06-10 | 山东潍坊润丰化工股份有限公司 | Microcapsule suspension-suspending agent containing efficient cyhalothrin and chlorantraniliprole and preparation method thereof |
| CN115735917A (en) * | 2022-11-28 | 2023-03-07 | 江苏艾津作物科技集团有限公司 | Pesticide microcapsule suspending agent with degradable capsule wall and preparation method thereof |
-
2023
- 2023-11-02 CN CN202311445586.8A patent/CN117158419B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102396508A (en) * | 2011-11-24 | 2012-04-04 | 陕西美邦农药有限公司 | Novel pesticide combination containing thiamethoxam |
| CN109452304A (en) * | 2018-11-13 | 2019-03-12 | 中国农业大学 | Dinotefuran microcapsule suspending agent and preparation method thereof |
| CN113519545A (en) * | 2021-07-15 | 2021-10-22 | 孟州市华丰生化农药有限公司 | Thiamethoxam microcapsule seed treatment suspending agent and application thereof |
| CN114600877A (en) * | 2022-03-29 | 2022-06-10 | 山东潍坊润丰化工股份有限公司 | Microcapsule suspension-suspending agent containing efficient cyhalothrin and chlorantraniliprole and preparation method thereof |
| CN115735917A (en) * | 2022-11-28 | 2023-03-07 | 江苏艾津作物科技集团有限公司 | Pesticide microcapsule suspending agent with degradable capsule wall and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN117158419A (en) | 2023-12-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105557747A (en) | Stable pesticide microcapsule suspending agent | |
| CN106490026A (en) | A kind of storage pest insecticide and preparation method thereof | |
| CN101878766A (en) | Pesticidal composition containing methoxyfenozide and biogenic pesticide | |
| CN113519545B (en) | Thiamethoxam microcapsule seed treatment suspending agent and application thereof | |
| CN101919386A (en) | Insecticidal composition containing methoxyfenozide and synthetic pyrethroid insecticide | |
| CN109430259A (en) | A kind of pesticide powder and preparation method thereof | |
| CN117158419B (en) | Cyhalothrin thiamethoxam microcapsule suspension and preparation method thereof | |
| CN100355345C (en) | Traditional Chinese medicine composite biological pesticide using crusta as main material | |
| CN1107293A (en) | Multifunctional emulsified insecticide | |
| CN108719345B (en) | Origanum vulgaris essential oil preparation, preparation method and application thereof | |
| CN102027949B (en) | Brassinolide neem microcapsule | |
| CN107950564A (en) | A kind of composite insecticide and its preparation process containing phenthoate dimephenthoate cidial and dimethoate emulsifiable concentrate | |
| CN106818766A (en) | A kind of composition pesticide of the mite nitrile of azoles containing second and spirodiclofen | |
| AU2019321001B2 (en) | Use of a structural polypeptide for plant coating | |
| CN103918656B (en) | A kind of plant growth regulator composition and preparation thereof | |
| CN105104422A (en) | Micro-capsule suspending agent containing fosthiazate and pyraclostrobin | |
| CN101396026A (en) | Plant pesticide capable of preventing and treating stored grain insects and use thereof | |
| JPH0967220A (en) | Plant pest-controlling agent | |
| CN105053021B (en) | For preventing the preparation of rice water weevil and preparation method | |
| CN104304287B (en) | A kind of suspension seed-coating agent of containing fipronil and ZEN 90160 and application thereof | |
| CN1152397A (en) | Synergistic composite suspended emulsion of weedicide | |
| CN104041532A (en) | Efficient sterilization yield-increasing suspending agent and production method and application thereof | |
| CN108684723A (en) | A kind of preparation method of the special disease prevention composition of rice | |
| CN1217880A (en) | Biological pesticides with virus and biological pesticide compositions | |
| CN113749130B (en) | Sugarcane organism seed stem coating agent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |