CN115956572A - High-stability sulfoxaflor suspending agent and preparation method thereof - Google Patents
High-stability sulfoxaflor suspending agent and preparation method thereof Download PDFInfo
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- CN115956572A CN115956572A CN202211174531.3A CN202211174531A CN115956572A CN 115956572 A CN115956572 A CN 115956572A CN 202211174531 A CN202211174531 A CN 202211174531A CN 115956572 A CN115956572 A CN 115956572A
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- sulfoxaflor
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- 239000005934 Sulfoxaflor Substances 0.000 title claims abstract description 52
- ZVQOOHYFBIDMTQ-UHFFFAOYSA-N [methyl(oxido){1-[6-(trifluoromethyl)pyridin-3-yl]ethyl}-lambda(6)-sulfanylidene]cyanamide Chemical compound N#CN=S(C)(=O)C(C)C1=CC=C(C(F)(F)F)N=C1 ZVQOOHYFBIDMTQ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000000375 suspending agent Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 19
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 19
- -1 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine Chemical compound 0.000 claims abstract description 17
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 17
- 229920000570 polyether Polymers 0.000 claims abstract description 17
- 229920005646 polycarboxylate Polymers 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 9
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- ABPYVNPDRFJZEU-UHFFFAOYSA-N 2-(2,2,2-triphenylethyl)phenol Chemical compound OC1=CC=CC=C1CC(C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 ABPYVNPDRFJZEU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000002270 dispersing agent Substances 0.000 claims description 20
- 239000002562 thickening agent Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 11
- 239000002518 antifoaming agent Substances 0.000 claims description 9
- 239000000230 xanthan gum Substances 0.000 claims description 9
- 229920001285 xanthan gum Polymers 0.000 claims description 9
- 235000010493 xanthan gum Nutrition 0.000 claims description 9
- 229940082509 xanthan gum Drugs 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000010008 shearing Methods 0.000 claims description 8
- 150000002367 halogens Chemical group 0.000 claims description 7
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- 230000002528 anti-freeze Effects 0.000 claims description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 239000013530 defoamer Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- RZXLPPRPEOUENN-UHFFFAOYSA-N Chlorfenson Chemical compound C1=CC(Cl)=CC=C1OS(=O)(=O)C1=CC=C(Cl)C=C1 RZXLPPRPEOUENN-UHFFFAOYSA-N 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- 229920001732 Lignosulfonate Polymers 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 229940071826 hydroxyethyl cellulose Drugs 0.000 claims description 2
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 2
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 235000010981 methylcellulose Nutrition 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 239000003381 stabilizer Substances 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 239000000080 wetting agent Substances 0.000 claims description 2
- 239000003814 drug Substances 0.000 abstract description 41
- 239000002245 particle Substances 0.000 abstract description 25
- 239000007788 liquid Substances 0.000 abstract description 14
- GJISNVPLOICVDR-UHFFFAOYSA-N 2-chloro-5-[(4-phenoxyphenoxy)methyl]-1,3-thiazole Chemical compound S1C(Cl)=NC=C1COC(C=C1)=CC=C1OC1=CC=CC=C1 GJISNVPLOICVDR-UHFFFAOYSA-N 0.000 abstract description 13
- 230000002195 synergetic effect Effects 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 6
- 241000607479 Yersinia pestis Species 0.000 abstract description 5
- 239000000575 pesticide Substances 0.000 abstract description 5
- 206010059866 Drug resistance Diseases 0.000 abstract description 4
- 125000005843 halogen group Chemical group 0.000 abstract 1
- 229940079593 drug Drugs 0.000 description 12
- 238000012360 testing method Methods 0.000 description 8
- TVFWYUWNQVRQRG-UHFFFAOYSA-N 2,3,4-tris(2-phenylethenyl)phenol Chemical compound C=1C=CC=CC=1C=CC1=C(C=CC=2C=CC=CC=2)C(O)=CC=C1C=CC1=CC=CC=C1 TVFWYUWNQVRQRG-UHFFFAOYSA-N 0.000 description 6
- 241000238631 Hexapoda Species 0.000 description 6
- 238000003860 storage Methods 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 241001124076 Aphididae Species 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000857 drug effect Effects 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000008234 soft water Substances 0.000 description 2
- 230000005653 Brownian motion process Effects 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 240000008067 Cucumis sativus Species 0.000 description 1
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000005900 Flonicamid Substances 0.000 description 1
- VKEQBMCRQDSRET-UHFFFAOYSA-N Methylone Chemical compound CNC(C)C(=O)C1=CC=C2OCOC2=C1 VKEQBMCRQDSRET-UHFFFAOYSA-N 0.000 description 1
- 206010034133 Pathogen resistance Diseases 0.000 description 1
- 231100000674 Phytotoxicity Toxicity 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 240000006677 Vicia faba Species 0.000 description 1
- 235000010749 Vicia faba Nutrition 0.000 description 1
- 235000002098 Vicia faba var. major Nutrition 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003042 antagnostic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004166 bioassay Methods 0.000 description 1
- 239000003139 biocide Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005537 brownian motion Methods 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- RLQJEEJISHYWON-UHFFFAOYSA-N flonicamid Chemical compound FC(F)(F)C1=CC=NC=C1C(=O)NCC#N RLQJEEJISHYWON-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000003630 growth substance Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 231100000518 lethal Toxicity 0.000 description 1
- 230000001665 lethal effect Effects 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- WPALTCMYPARVNV-UHFFFAOYSA-N tolfenpyrad Chemical compound CCC1=NN(C)C(C(=O)NCC=2C=CC(OC=3C=CC(C)=CC=3)=CC=2)=C1Cl WPALTCMYPARVNV-UHFFFAOYSA-N 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 invention discloses a high-stability sulfoxaflor suspending agent, which at least comprises a first component and a second component as preparation raw materials, wherein the first component is a halogen-containing compound with a 4-p-phenoxy phenoxymethyl structure, and the second component is sulfoxaflor. The invention relates to a method for preparing 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole or 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine and sulfoxaflor by adopting a ratio of 2:1, the pesticide can achieve the highest synergistic effect, can also reduce the drug resistance of pests, and has certain sustainable effect. And the synergistic effect of the liquid polycarboxylate, the propylene glycol block polyether and the triphenylethylphenol polyoxyethylene ether sulfate is adopted, so that the suspending agent has excellent stability, can be stored for a long time, prevents the medicament particles from settling, and maintains the long-acting stability of the medicament.
Description
Technical Field
The invention relates to a high-stability sulfoxaflor suspending agent, relates to A01N, and particularly relates to the field of biocides.
Background
The compound containing the halogen 4-p-phenoxy phenoxymethyl structure is a brand new chitin synthesis inhibitor, can play a role in killing insects as an insect growth regulator, and can generate better pest control effect by synergistic action with sulfoxaflor. And the two have no cross resistance, so the pesticide is not easy to generate drug resistance when being applied to pest control, and the control effect is obvious. The suspending agent prepared from the original medicine has strong capability of adhering to the surface of a plant, is resistant to rain wash, has long drug effect time, avoids dust hazard in the preparation process compared with powder, has small environmental protection pressure, takes water as a medium, and has no flammability and phytotoxicity problems generated by organic solvents. However, the biggest problem to be solved by the suspended medicament is the suspension stability of the medicament, and some suspended medicaments are stored in a high-temperature and low-temperature environment for a long time, so that the medicament particles can be settled, the dispersion stability of the medicament is influenced, and the medicament effect is reduced, so that how to improve the storage stability of the suspended medicament and prolong the storage time is a problem to be solved urgently.
Chinese invention patent CN201410414404.5 discloses a dispersible oil suspending agent containing sulfoxaflor, which takes sulfoxaflor and tolfenpyrad or flonicamid as effective components, has the characteristics of environmental protection, good drug effect, rain wash resistance, long lasting period and safety to crops, but adopts an oil solvent as a dispersing agent, has larger environmental protection pressure, and can harm an environmental ecosystem after long-term use. The Chinese invention patent CN201711489477.0 discloses a bennserin ether derivative pesticide composition and an application thereof in pest control, a compound with a 4-p-phenoxy methyl structure and the bennserin ether derivative are synergistic, but the stability of an aqueous suspending agent is not tested, and the storage stability is unknown.
Disclosure of Invention
In order to prepare a stable suspending agent with good drug effect and difficult drug resistance, the invention provides a high-stability sulfoxaflor suspending agent, which is prepared from at least a first component and a second component, wherein the first component is a halogen-containing compound with a 4-p-phenoxy phenoxymethyl structure, and the second component is sulfoxaflor.
As a preferable embodiment, the halogen in the compound containing a halogen 4-p-phenoxy methyl structure is selected from one or a combination of two of chlorine, fluorine and bromine, and the compound is selected from one of pyridine or thiazole.
As a preferred embodiment, the first component is selected from one of 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine or 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole.
As a preferred embodiment, the weight ratio of the first component to the second component is (80-1): (1-80).
As a preferred embodiment, the weight ratio of the first component to the second component is (40-1): (1-40).
As a preferred embodiment, the weight ratio of the first component to the second component is (8-1): (1-8).
As a preferred embodiment, the weight ratio of the first component to the second component is 2:1.
as a preferred embodiment, the preparation raw material further comprises an auxiliary agent, wherein the auxiliary agent is one or a combination of several of a dispersing agent, an antifreezing agent, an antifoaming agent, a thickening agent, a stabilizing agent, a wetting agent, a filler, a pH regulator and water.
As a preferred embodiment, the preparation raw materials comprise the following components in percentage by weight: 10-20% of a first component, 10-20% of a second component, 5-10% of a dispersant, 3-8% of an antifreeze, 1-5% of a defoamer, 1-5% of a pH regulator, 1-3 parts of a thickener and the balance of water.
As a preferred embodiment, the preparation raw materials comprise the following components in percentage by weight: 30% of a first component, 15% of a second component, 8% of a dispersing agent, 5% of an antifreezing agent, 2% of a defoaming agent, 3% of a pH regulator, 1.2 parts of a thickening agent and the balance of water.
As a preferred embodiment, the dispersing agent is selected from one or a combination of several of polycarboxylate, lignosulfonate, fatty alcohol-polyoxyethylene ether, alkylphenol ethoxylate, aryl phenol ethoxylate sulfonate, alkylphenol ethoxylate phosphate and polyether dispersing agent.
As a preferred embodiment, the polyether dispersant is propylene glycol block polyether, the propylene glycol block polyether has a molecular weight of 1500-2500Da, an HLB value of 4-10, and a viscosity of 250-400cps at 25 ℃.
In a preferable embodiment, the aryl phenol polyoxyethylene ether sulfonate is triphenylethyl phenol polyoxyethylene ether sulfate, and the acid value is less than or equal to 10mg KOH/g.
As a preferred embodiment, the dispersant is a combination of a liquid polycarboxylate, a propylene glycol block polyether and a tristyrylphenol polyoxyethylene ether sulfate.
In a preferred embodiment, the weight ratio of the liquid polycarboxylate, the propylene glycol block polyether and the tristyrylphenol polyoxyethylene ether sulfate is (1-2): 1: (1-3).
As a preferred embodiment, the weight ratio of the liquid polycarboxylate, the propylene glycol block polyether and the tristyrylphenol polyoxyethylene ether sulfate is 2:1:1.
the applicant found in the experimental process that the combination of liquid polycarboxylate, propylene glycol block polyether and tristyrylphenol polyoxyethylene ether sulfate as the dispersant can maintain good suspension state of the original drug particles, and guessed the possible reason is: the original drug particles can obtain smaller particle size under the shearing force, but the original drug with small particle size is easy to agglomerate, so that the particle size is reversely increased, and the stability of a suspension system is not facilitated. The applicant adds liquid polycarboxylate to have better adsorbability on the original drug particles, the lipophilic group of the carboxylate coats the surface of the original drug particles, and the hydrophilic carboxylate ions increase the electrostatic repulsion between the particles after shearing, so that the agglomeration between the original drug particles is reduced. Applicants have further found that when the liquid polycarboxylate, propylene glycol block polyether and tristyrylphenol polyoxyethylene ether sulfate are used in the range of 2:1:1, the particles of the active ingredient in the formed suspension do not settle, and the particle diameter of the drug particles can be maintained at an appropriate size for a long period of time. The stable particle size of the medicament can be maintained in a long-term storage environment. The reasons may be: under the optimized weight ratio, the liquid polycarboxylate multi-branched comb-shaped structure has a hydrophobic framework and hydrophilic side chains, and forms micelles on the surfaces of original drug particles under the synergistic action with triphenylethylphenol polyoxyethylene ether sulfate, and the long-chain hydrophobic groups of the polyoxyethylene ether further increase the steric hindrance between the particles, so that the particles are prevented from being closed. The comb-shaped structure of the liquid polycarboxylate can be inserted into the polyoxyethylene ether chain, so that the stability of the micelle is further improved, and the suspension system can be stably stored for a long time.
As a preferred embodiment, the antifreeze is an alcohol antifreeze, and preferably, the antifreeze is propylene glycol.
As a preferred embodiment, the defoamer is a silicone defoamer.
As a preferred embodiment, the pH regulator is selected from one or a combination of citric acid, glacial acetic acid, diethylamine and sodium bicarbonate.
As a preferred embodiment, the thickener is selected from xanthan gum, hydroxymethyl cellulose, hydroxyethyl cellulose, magnesium aluminum silicate, methyl cellulose and one or more of acrylate.
As a preferred embodiment, the thickener is a combination of xanthan gum and magnesium aluminum silicate.
As a preferred embodiment, the weight ratio of xanthan gum to magnesium aluminum silicate is (0.1-0.5): 1.
as a preferred embodiment, the weight ratio of xanthan gum to magnesium aluminum silicate is 0.2:1.
this application adopts the combination of xanthan gum and magnesium aluminium silicate as the thickener, can further improve the stability of suspending agent, and xanthan gum and magnesium aluminium silicate adopt 0.2:1 can weaken the brownian motion of the raw drug particles and counteract the gravity sedimentation of the raw drug particles, so that the suspended medicament has better storage stability.
The water is soft water.
The second aspect of the invention provides a preparation method of a high-stability sulfoxaflor suspending agent, which comprises the following steps:
(1) Putting the first component, the second component, the dispersing agent, the antifreezing agent, the pH regulator, the antifoaming agent, the thickening agent and water into a shearing kettle, and shearing for 20-50min;
(2) And then the suspension enters a sand mill, and the high-stability sulfoxaflor is prepared after sand milling.
Compared with the prior art, the invention has the following beneficial effects:
(1) The high-stability sulfoxaflor-nitrile suspending agent disclosed by the invention has the advantages that 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole or 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine and sulfoxaflor are synergistic, a higher deinsectization effect can be realized by using less medicament amount, the using amount of the medicament is reduced, and the planting cost is reduced.
(2) The high-stability sulfoxaflor suspending agent adopts 2:1, the pesticide can achieve the highest synergistic effect, can also reduce the drug resistance of pests, and has certain sustainable effect.
(3) The high-stability sulfoxaflor suspending agent disclosed by the invention has excellent stability by adopting the synergistic effect of the liquid polycarboxylate, the propylene glycol block polyether and the triphenylethylphenol polyoxyethylene ether sulfate, can be stored for a long time, prevents the drug particles from settling, and maintains long-acting stability of the drug.
Detailed Description
Example 1
A medicinal preparation is prepared from 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine.
Example 2
A medicine is prepared from sulfoxaflor.
Example 3
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine and sulfoxaflor in a mass ratio of 40:1.
example 4
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine and sulfoxaflor in a mass ratio of 8:1.
example 5
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine and sulfoxaflor in a mass ratio of 2:1.
example 6
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine and sulfoxaflor in a mass ratio of 1:1.
example 7
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine and sulfoxaflor in a mass ratio of 1:4.
example 8
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine and sulfoxaflor in a mass ratio of 1:20.
example 9
A preparation is prepared from 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole.
Example 10
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole and sulfoxaflor in a mass ratio of 40:1.
example 11
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole and sulfoxaflor in a mass ratio of 8:1.
example 12
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole and sulfoxaflor in a mass ratio of 2:1.
example 13
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole and sulfoxaflor in a mass ratio of 1:1.
example 14
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole and sulfoxaflor in a mass ratio of 1:4.
example 15
A medicament is prepared from the combination of 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole and sulfoxaflor in a mass ratio of 1:20.
example 16
The high-stability sulfoxaflor suspending agent comprises the following preparation raw materials in percentage by weight: 30% of first component, 15% of second component, 8% of dispersing agent, 5% of antifreezing agent, 2% of defoaming agent, 3% of pH regulator, 1.2 parts of thickening agent and the balance of water.
The first component is 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole, and the second component is sulfoxaflor.
The dispersing agent is a combination of liquid polycarboxylate, propylene glycol block polyether and triphenylethylphenol polyoxyethylene ether sulfate, and the weight ratio is 2:1:1. the liquid polycarboxylate was purchased from Weichafang Ruifu chemical Co., ltd; the propylene glycol block polyether is purchased from Heian petrochemical plants of Jiangsu province, and has the model of L62, the molecular weight of 2500Da, the HLB value of 7 and the viscosity of 400cps at 25 ℃; the triphenylethylphenol polyoxyethylene ether sulfate has an acid value of less than or equal to 10mg KOH/g, is purchased from Heian petrochemical plants in Jiangsu province, and has the model number of 600-1.
The antifreezing agent is propylene glycol.
The defoaming agent is an organic silicon defoaming agent which is purchased from Dow Corning and has the model number of 7305.
The pH regulator is glacial acetic acid.
The thickening agent is a combination of xanthan gum and magnesium aluminum silicate, and the weight ratio is 0.2:1.
the water is soft water.
A preparation method of a high-stability sulfoxaflor suspending agent comprises the following steps:
(1) Putting the first component, the second component, the dispersing agent, the antifreezing agent, the pH regulator, the defoaming agent, the thickening agent and water into a shearing kettle, and shearing for 30min;
(2) And then the suspension enters a sand mill, and the high-stability sulfoxaflor is prepared after sand milling.
Example 17
A high-stability sulfoxaflor suspending agent, the specific procedure of which is the same as example 16, is different in that the propylene glycol block polyether is purchased from Haian petrochemical plant of Jiangsu province, the model is L31, the molecular weight is 1100Da, the HLB value is 3.5, and the viscosity is 200cps at 25 ℃.
Example 18
The specific steps of a high-stability sulfoxaflor suspending agent are the same as those in example 16, but the difference is that the dispersing agent is a combination of liquid polycarboxylate and tristyrylphenol polyoxyethylene ether sulfate, and the weight ratio is 2:1.
example 19
The specific procedure of a high-stability sulfoxaflor suspending agent is the same as that in example 16, except that the thickening agent is xanthan gum.
Performance testing
1. And (3) testing toxicity: the indoor bioassay method comprises the following steps: an indoor toxicity determination test is carried out by adopting an immersion method, and according to the pre-test condition, various medicaments are respectively dissolved by acetone and respectively prepared into 5 concentration gradients of 10 mug/mL, 15 mug/mL, 20 mug/mL, 25 mug/mL and 30 mug/mL. Selecting cucumber leaves with a proper amount of aphids, removing the uncomfortable individuals, soaking in the prepared determination liquid medicine, taking out after 5s, airing at room temperature, placing in a culture dish paved with filter paper, and sealing with a preservative film. The treated test insects were treated in a light incubator at 25 ℃ and L: d = 14. Repeating the treatment for 5 times, wherein each repetition is no less than 30 adult aphids, checking the mortality rate 48h after the pesticide application, slightly poking the insect body with a fine hair pen during the check, and recording the total number of the insects and the number of dead insects according to the judgment standard that the aphids cannot climb up to death by themselves. And (3) carrying out statistical processing on the data obtained by the test by using SPSS software to obtain a toxicity regression equation, lethal medium concentration, correlation coefficient and the like, and solving a cotoxicity coefficient (CTC) by using a Sun cloud Peel method. The judgment standard of the synergistic effect of the two effective components after compounding is as follows:
the CTC is synergistic when the CTC is more than 120, antagonistic when the CTC is less than 80, and additive when the CTC is 80-120.
The results of the regression equation, the related coefficient and the co-toxicity coefficient for killing the broad bean aphids are shown in table 1.
TABLE 1
From examples 1 to 8, when 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine and sulfoxaflor are compounded according to the different proportions, the proportion of the co-toxicity coefficient of more than 120 is A: B = 1. When the ratio of the 2-chloro-5- ((4-phenoxyphenoxy) methyl) pyridine to the sulfoxaflor is 1, the cotoxicity coefficient reaches 126.4, which is the highest value of the cotoxicity coefficients of all formulas, and the synergistic effect is most obvious.
From the data in examples 9-15, it can be seen that when 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole and sulfoxaflor are compounded in the different proportions, the proportion of co-toxicity coefficient greater than 120 is A: B = 1. When the ratio of the 2-chloro-5- ((4-phenoxyphenoxy) methyl) thiazole to the sulfoxaflor is 2.
2. And (3) testing the stability: high-temperature stability: the suspensions prepared in examples 16 to 19 were placed in an incubator at 54 ℃ and stored for 14 days, and then taken out, and viscosity was measured using a viscometer, average particle size was measured using a particle size analyzer, and appearance was visually observed.
Stability at normal temperature: the suspensions prepared in examples 16 to 19 were placed in a thermostat at 25 ℃ and stored for 24 months and then taken out, the viscosity was measured using a viscometer, the average particle size was measured using a particle size analyzer, and the appearance was visually observed.
The test results are shown in Table 2.
TABLE 2
Claims (10)
1. The high-stability sulfoxaflor suspending agent is characterized in that the preparation raw materials at least comprise a first component and a second component, wherein the first component is a halogen-containing compound with a 4-p-phenoxy phenoxymethyl structure, and the second component is sulfoxaflor.
2. The high-stability sulfoxaflor suspending agent according to claim 1, wherein the halogen in the compound containing a halogen 4-p-phenoxy phenoxymethyl structure is selected from one or two of chlorine, fluorine and bromine, and the compound is selected from one of pyridine and thiazole.
3. The high-stability sulfoxaflor suspending agent as claimed in claim 1, wherein the weight ratio of the first component to the second component is (80-1): (1-80).
4. The high-stability sulfoxaflor suspending agent according to claim 1, wherein the preparation raw materials further comprise an auxiliary agent, and the auxiliary agent is one or a combination of several selected from a dispersing agent, an antifreezing agent, an antifoaming agent, a thickening agent, a stabilizing agent, a wetting agent, a filler, a pH regulator and water.
5. The high-stability sulfoxaflor suspending agent according to claim 4, wherein the preparation raw materials comprise, in weight percent: 10-20% of a first component, 10-20% of a second component, 5-10% of a dispersant, 3-8% of an antifreeze, 1-5% of a defoamer, 1-5% of a pH regulator, 1-3 parts of a thickener and the balance of water.
6. The high-stability sulfoxaflor suspending agent according to claim 5, wherein the dispersing agent is selected from one or more of polycarboxylate, lignosulfonate, fatty alcohol-polyoxyethylene ether, alkylphenol ethoxylate, aryl phenol ethoxylate sulfonate, alkylphenol ethoxylate phosphate and polyether dispersing agent.
7. The high-stability sulfoxaflor suspending agent as claimed in claim 6, wherein the polyether dispersant is propylene glycol block polyether having a molecular weight of 1000-2000Da, an HLB value of 3-10, and a viscosity of 200-400cps at 25 ℃.
8. The high-stability sulfoxaflor suspension according to claim 6, wherein the aryl phenol polyoxyethylene ether sulfonate is triphenylethyl phenol polyoxyethylene ether sulfate, and the acid value is less than or equal to 10mg KOH/g.
9. The high-stability sulfoxaflor suspending agent as claimed in claim 5, wherein the thickener is selected from xanthan gum, hydroxymethyl cellulose, hydroxyethyl cellulose, magnesium aluminum silicate, methyl cellulose, and acrylate.
10. A method for preparing the high-stability sulfoxaflor suspending agent according to claim 1, which comprises the following steps:
(1) Putting the first component, the second component, the dispersing agent, the antifreezing agent, the pH regulator, the defoaming agent, the thickening agent and water into a shearing kettle, and shearing for 20-50min;
(2) And then the suspension enters a sand mill, and the high-stability sulfoxaflor is prepared after sand milling.
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