CN111374125A - Pesticide composition in suspension emulsion and its preparation - Google Patents

Pesticide composition in suspension emulsion and its preparation Download PDF

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Publication number
CN111374125A
CN111374125A CN201811648924.7A CN201811648924A CN111374125A CN 111374125 A CN111374125 A CN 111374125A CN 201811648924 A CN201811648924 A CN 201811648924A CN 111374125 A CN111374125 A CN 111374125A
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thiram
polyoxyethylene ether
compound
percent
water
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CN111374125B (en
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顾玲玲
丑靖宇
莫迪
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Shenyang Sinochem Agrochemicals R&D Co Ltd
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Shenyang Sinochem Agrochemicals R&D Co Ltd
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
    • A01N33/18—Nitro compounds
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
    • A01N37/46—N-acyl derivatives
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
    • A01N37/50—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids the nitrogen atom being doubly bound to the carbon skeleton
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/50—1,3-Diazoles; Hydrogenated 1,3-diazoles
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/647—Triazoles; Hydrogenated triazoles
    • A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/26—Oxidation products of dithiocarbamic acid derivatives, e.g. thiuram sulfides
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N55/00—Biocides, pest repellants or attractants, or plant growth regulators, containing organic compounds containing elements other than carbon, hydrogen, halogen, oxygen, nitrogen and sulfur
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
    • A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
    • A01N57/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing heterocyclic radicals

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
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Abstract

The invention belongs to the technical field of pesticides, and relates to a suspended emulsion pesticide composition (containing a low-melting-point compound and thiram) and a preparation method thereof. The composition comprises an active component and a solvent; the active components are compound A and thiram; wherein the compound A is a bactericidal compound with a melting point of less than 90 ℃; the solvent is at least one aliphatic alcohol or alicyclic alcohol for dissolving the compound A. The solvent added into the composition provided by the invention further develops a wider idea of solvent selection in the suspension emulsion, and breaks through the bottleneck that the low-melting-point compound preparation cannot be produced on a large scale.

Description

Pesticide composition in suspension emulsion and its preparation
Technical Field
The invention belongs to the technical field of pesticides, and relates to a suspended emulsion pesticide composition (containing a low-melting-point compound and thiram) and a preparation method thereof.
Background
When a low-melting-point sterilization compound (such as propiconazole, prochloraz, pyrisoxazole, chlorpyrifos, trifloxystrobin, imazalil, pyraclostrobin, metalaxyl-M, tebufenpyrad, trifluralin, flusilazole, ipconazole and the like) is prepared into a preparation, a plurality of challenges are faced in auxiliary agent screening and production processes, and due to the inherent characteristic of low melting point, the product has the defects of easy crystallization, sudden drop of suspension rate after heat storage, poor stability with time and the like.
Thiram belongs to a dithiocarbamate fungicide, and is a protective fungicide. The bactericidal spectrum is wide, and the bactericidal composition has good control effects on various crops such as downy mildew, epidemic disease, anthracnose, cereal smut, seedling yellow blight and the like. The pesticide composition has good control effect on diseases of seed infection and seedling soil infection, is mainly used for seed treatment and soil treatment for a long time, and is widely used for foliage spraying at present.
The combination of low-melting-point compounds (propiconazole, prochloraz, pyrisoxazole, chlorpyrifos, trifloxystrobin, imazalil, pyraclostrobin) and thiram for sterilization is very common and popular in the market. For example, the combination of pyrisoxazole and thiram for sterilization has been disclosed in CN1608469A and CN 201511009335. CN1608469A discloses the use of a fungicidal composition of pyrisoxazole and thiocarbamate fungicides for controlling plant diseases caused by pathogenic fungi. Furthermore, CN201511009335 discloses bentonite stabilized pyrisoxazole and thiram suspoemulsion.
When the low-melting-point compound is developed into a liquid preparation, a stable preparation can also be obtained by a few means, for example, a method of making the low-melting-point compound propiconazole into a eutectic is described in WO2010034976, or the low-melting-point compound is wrapped in a microcapsule preparation, for example, WO2014018188, which describes that the low-melting-point compound clomazone is prepared into a microcapsule preparation, but at present, the most common method is to compound a high-melting-point active ingredient and a low-melting-point active substance into a suspension emulsion.
The suspoemulsion may comprise compound a (low-melting active ingredient) dissolved in a selected organic solvent and at the same time a second pesticidally active compound B (high-melting active ingredient) in the form of solid particles, wherein all components coexist in stable form.
However, also low melting compounds, when prepared in emulsion form (e.g. aqueous and suspoemulsion), tend to crystallize and ostwald ripening over time and temperature, and more commonly when formulated with other solid compounds.
This makes the choice of solvent a critical aspect affecting the stability of the suspoemulsion, since it is subject to several requirements, on the one hand the solvent should have sufficient solubility to dissolve the low-melting active substance, and on the other hand it should not cause the austenitic ripening of the high-melting active substance itself and the formulation.
A more typical example, such as WO2011012493, can efficiently produce stable formulations containing low melting point compounds by adding lactate as a suspoemulsion solvent, but when thiram is the active ingredient of the suspended particles, the use of lactate does not inhibit its austenite ripening.
As another example, DE102016008444 prepares suspoemulsions by dissolving propiconazole in a conventional aromatic hydrocarbon solvent, but when the solid active ingredient is thiram, austenite ripening is very likely to occur using a conventional aromatic hydrocarbon solvent.
In summary, based on the prior art, the crystallization of propiconazole in a preparation can be effectively avoided by changing the crystal form, such as the above-mentioned method for forming a propiconazole eutectic crystal, but a lot of effort is required to search for a suitable compound for forming the eutectic crystal, and a special characterization means is used for assistance, so that the process is complicated, and the method is not easy to popularize in a factory. The stability is improved by wrapping the low-melting-point compound clomazone in a microcapsule preparation form, an isocyanate compound with strong toxicity is required to be used in the preparation process, the reaction condition is difficult to control, the requirements on experimental environment and factory qualification are high, and the large-scale production is difficult.
It is clear that it is easier to carry out mass production by preparing a low melting point compound and a high melting point compound as a suspoemulsion. However, when a suspension emulsion containing a low-melting compound is prepared, the use of a conventional solvent causes unstable phenomena such as crystallization, flocculation, austenite aging and the like of the preparation, and the quality of the preparation is not guaranteed. However, the use of a special solvent with a relatively high price, such as a lactate solvent, can solve the problem of stability of some low-melting-point compound suspoemulsions, but can greatly increase the cost of the suspoemulsions, severely restrict the large-scale production of the suspoemulsions, and the dual-component composition cannot have both sufficient solubility and the function of an austenite curing inhibitor when some high-cost solvents are selected, so that the bottleneck that a low-melting-point compound preparation cannot be produced on a large scale is urgently needed to be broken through at present.
Disclosure of Invention
The invention aims to provide a suspended emulsion pesticide composition (containing a low-melting-point compound and thiram) and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the composition comprises an active component and a solvent; the active components are compound A and thiram; wherein the compound A is a bactericidal compound with a melting point of less than 90 ℃; the solvent is at least one aliphatic alcohol or alicyclic alcohol for dissolving the compound A.
The effective content of active ingredients in the composition is 0.1-80%.
The weight ratio of the compound A to the thiram in the active ingredients is 1:100-100: 1.
Preferably, the weight ratio of the compound A to the thiram in the active ingredients is 1:50-50: 1.
Further preferably, the weight ratio of the compound A to the thiram in the active ingredients is 1:20-20: 1.
Still more preferably, the weight ratio of the compound A to the thiram in the active ingredients is 1:10-10: 1.
More preferably, the weight ratio of the compound A to the thiram in the active ingredients is 1:5-5: 1.
The weight ratio of the compound A to the solvent is 10:1 to 1: 10.
preferably, the weight ratio of the compound a to the solvent is 8: 1-1: 8.
further preferably, the weight ratio of the compound A to the solvent is 5:1 to 1: 5.
More preferably, the weight ratio of the compound A to the solvent is 3:1 to 1: 3.
The solvent is selected from C4-C12Saturated fatty alcohol, C4-C12Unsaturated fatty alcohol, C4-C12Saturated branched fatty alcohol, C4-C12Unsaturated branched fatty alcohol, C6-C12One or more alicyclic alcohols.
Preferably, the solvent is one or more of hexanol, n-octanol, isohexanol, isooctanol, cyclohexanol, alkyl-substituted cyclohexanol, hexenol, octenol, decenol, cyclohexenol, and alkyl-substituted cyclohexenol.
Further preferably, the solvent is one or more of n-hexanol, n-octanol, isohexanol, isooctanol and cyclohexanol.
More preferably, the solvent is n-hexanol, n-octanol, isohexanol, isooctanol, or cyclohexanol.
The compound A is propiconazole, prochloraz, pyrisoxazole, chlorpyrifos, trifloxystrobin, imazalil, pyraclostrobin, metalaxyl-M, tebufenpyrad, trifluralin, flusilazole or ipconazole. Preferably pyrisoxazole, propiconazole or pyraclostrobin.
The suspended emulsion pesticide composition comprises, by weight, 1-50% of a low-melting-point compound A, 1-60% of thiram, 2-20% of a solvent, 7-10% of an auxiliary agent and the balance of a carrier or a dispersion medium.
The auxiliary agent is one or more of wetting dispersant, emulsifier, thickener, antifreezing agent and stabilizer.
A preparation method of a suspended emulsion pesticide composition comprises the following steps:
(a) dispersing an oil phase: dissolving the compound A in at least one solvent of aliphatic alcohol or alicyclic alcohol;
(b) continuous aqueous phase: dissolving thiram in water to obtain thiram suspension;
(c) and uniformly mixing the dispersed oil and the water phase, and adding an auxiliary agent to obtain the suspended emulsion pesticide composition.
The wetting dispersant is selected from lignosulfonate, macromolecular carboxylate, naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and polysubstituted aryl polyoxyethylene ether phosphate; wherein the lignosulfonate may for example be selected from, but not limited to, Ultrazine NA or Borresperse NA; the polymeric carboxylate may be selected from, for example, but not limited to, Tersperse 2700, Geropon T36; naphthalenesulfonates, for example, may be selected from, but not limited to, NNO, Morwet D425, or Morwet EFW; the polysubstituted aryl polyoxyethylene ether phosphate may for example be selected from, but not limited to, Soprophor SC.
The emulsifier is selected from one or more of anionic surfactant, nonionic surfactant and anionic and nonionic compound surfactant; wherein the anionic surfactant mainly comprises calcium dodecylbenzene sulfonate and sodium polyacrylate; the nonionic surfactant is mainly castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether, phenethyl phenol polyoxyethylene ether, alkylphenol polyoxyethylene formaldehyde condensate, fatty alcohol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, styrene maleic anhydride copolymer, phenethyl phenol polyoxyethylene polyoxypropylene ether and formaldehyde condensate. Wherein the castor oil polyoxyethylene ethers may be selected from the Alkamuls OR series, such as but not limited to Alkamuls OR 36; the alkylphenol polyoxyethylene ethers may be selected from the TX series such as but not limited to TX-10; the alkylphenol ethoxylates may also be selected from the OP series such as, but not limited to, OP-7, OP-10; the alkylphenol polyoxyethylene ethers may also be selected from the NP series such as, but not limited to, NP-10; the phenethylphenol polyoxyethylene ethers may be selected from, for example, but not limited to, farm milk 600 #; the alkylphenol polyoxyethylene ether formaldehyde condensate may be selected from, for example, but not limited to, agricultural milk 700 #; the fatty alcohol polyoxyethylene ethers may be selected from the AEO series such as, but not limited to, AEO-3, AEO-9; the fatty alcohol polyoxyethylene ethers may also be selected from the peregal series such as, but not limited to, SA-20; the sorbitan fatty acid ester may be selected from the Span series such as, but not limited to, Span-80; the sorbitan fatty acid ester polyoxyethylene ether may be selected from the Tween series such as, but not limited to, Tween-80; the phenylethylphenol polyoxyethylene polyoxypropylene ether and formaldehyde condensate may be selected from, for example, but not limited to, agro-milk 1601#, agro-milk 1602 #; the anionic nonionic built surfactant may be selected from, for example, but not limited to, Nongru 0201B.
The thickening agent is selected from one or more of xanthan gum and magnesium aluminum silicate.
If the suspension emulsion is used or stored in tropical regions with higher temperature, a proper amount of stabilizing agent such as one or more of epoxidized soybean oil, sodium benzoate, sodium sorbate, epichlorohydrin and hydroquinone can be added; if the product is used or stored in cold area with low temperature, one or more of ethylene glycol, propylene glycol, glycerol and urea can be added. This is familiar to those skilled in the art of pesticide processing.
The suspoemulsions of the present invention employ sodium hydroxide and/or hydrochloric acid to adjust the pH of the system according to techniques familiar to those of ordinary skill in the pesticide processing art.
The low-melting-point compound and the thiram-containing composition are added with at least one of aliphatic alcohol and alicyclic alcohol as a solvent of the emulsion, so that the crystallization of the composition at low temperature, the crystallization of the composition when the composition is diluted into an aqueous solution and the aging of austenite can be solved.
Stable compositions within the scope of the invention include those that can be easily resuspended or redispersed by only a small amount of agitation in which case the formulation exhibits delamination or precipitation as described by t.f. tadros [ Surfactants in adhesives, Marcel Dekker, New York (1995) ].
The invention has the advantages that:
aiming at the stability problem of the suspension emulsion with compounded active ingredients of high-melting point substances and low-melting point substances, the invention provides that aliphatic alcohol or alicyclic alcohol is used as a crystallization inhibitor and an austenite curing inhibitor in a low-melting point compound and thiram suspension emulsion, so that the solubility of the low-melting point compound in the composition can be ensured, the low-temperature crystallization can be effectively prevented, the crystallization of a diluted aqueous solution can be effectively prevented, and the austenite curing phenomenon can be effectively inhibited.
Meanwhile, in the composition added with the solvent, the low-melting-point compound is mixed with the solvent at first and then is mixed with the thiram, so that the crystallization and austenite curing phenomena of the active component are obviously inhibited, the stability of the suspended emulsion composition is ensured, and the preparation cost is obviously reduced by adding the fatty alcohol or the alicyclic alcohol.
The solvent added into the composition provided by the invention further develops a wider idea of solvent selection in the suspension emulsion, and breaks through the bottleneck that the low-melting-point compound preparation cannot be produced on a large scale.
Detailed Description
The following specific examples are intended to illustrate the invention in detail, but the invention is not limited to these examples. All formulations were given in weight percent. The active component in the formula is metered after being reduced by hundred, and the pyrisoxazole is purchased from Shenyang Kechuang chemical company Limited; other auxiliary agents and raw materials are conventional varieties sold in the market.
Formulation examples of compositions containing Low melting Compound and thiram
According to the formula requirement, the preparation process is divided into three steps:
step 1: preparation of an emulsifiable concentrate of the Low-melting Compound phase (a)
Mixing the compound with melting point less than 90 deg.C with fatty alcohol or alicyclic alcohol at room temperature. After standing for 30 minutes, the emulsifier (fatty alcohol-polyoxyethylene ether) was added and stirred until a homogeneous solution was formed.
Step 2: preparation of dispersed particles of thiram active ingredient in a continuous aqueous phase (b)
Mixing the active ingredient thiram, the dispersant, other additives (such as an antifreezing agent and an antifoaming agent) and required water uniformly, finely grinding the mixture by using a horizontal stirring bead mill to maintain process parameters, such as the average particle size d50 not more than 3 microns and almost all particles d90 not more than 6 microns, detecting control indexes at any time, discharging after the particles are qualified, and subpackaging to obtain the suspension emulsion.
And step 3: preparation of the suspoemulsion
Oil phase (a) was added to aqueous phase (b) with stirring at room temperature for an optimal amount of time. Then, an appropriate amount of thickener was added to the above mixture and stirring was continued until the mixture became a uniform suspoemulsion at room temperature.
Preparation examples of the formulations
Example 1:
the composition comprises, by weight, 1% of propiconazole, 2% of n-octanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 2:
the composition comprises, by weight, 1% of propiconazole, 2% of isooctanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 3:
the composition comprises, by weight, 1% of propiconazole, 2% of cyclohexanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 4:
the composition comprises, by weight, 15% of propiconazole, 15% of n-octanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 5:
the composition comprises, by weight, 15% of propiconazole, 15% of isooctanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 6:
according to the weight percentage, propiconazole is 15%, cyclohexanol is 15%, fatty alcohol-polyoxyethylene ether is 5%, thiram is 15%, naphthalenesulfonic acid formaldehyde condensation compound is 1%, triphenylethylene phenol polyoxyethylene ether phosphate is 2%, polyoxyethylene polyoxypropylene block copolymer is 2%, xanthan gum is 0.05%, and water is added to 100%.
Example 7:
according to the weight percentage, the propiconazole is 50 percent, the n-octanol is 20 percent, the fatty alcohol-polyoxyethylene ether is 5 percent, the thiram is 1 percent, the triphenyl ethylene phenol polyoxyethylene ether phosphate is 2 percent, the xanthan gum is 0.2 percent, and the water is complemented to 100 percent.
Example 8:
according to the weight percentage, the propiconazole is 50 percent, the isooctyl alcohol is 20 percent, the fatty alcohol-polyoxyethylene ether is 5 percent, the thiram is 1 percent, the triphenyl vinyl phenol polyoxyethylene ether phosphate is 2 percent, the xanthan gum is 0.2 percent, and the water is complemented to 100 percent.
Example 9:
according to the weight percentage, the propiconazole is 50 percent, the cyclohexanol is 20 percent, the fatty alcohol-polyoxyethylene ether is 5 percent, the thiram is 1 percent, the triphenylethylene phenol polyoxyethylene ether phosphate is 2 percent, the xanthan gum is 0.2 percent, and the water is complemented to 100 percent.
Example 10:
the composition comprises, by weight, 1% of prochloraz, 2% of n-octyl alcohol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of a naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of a polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water which are complemented to 100%.
Example 11: the composition comprises, by weight, 1% of prochloraz, 2% of isooctanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water in balance to 100%.
Example 12: the composition comprises, by weight, 1% of prochloraz, 2% of cyclohexanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water which are complemented to 100%.
Example 13: the composition comprises, by weight, 15% of prochloraz, 15% of n-octanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 14: the composition comprises, by weight, 15% of prochloraz, 15% of isooctanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 15: the composition comprises, by weight, 15% of prochloraz, 15% of cyclohexanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water, wherein the water is added to 100%.
Example 16: according to the weight percentage, the prochloraz is 50 percent, the n-octanol is 20 percent, the fatty alcohol-polyoxyethylene ether is 5 percent, the thiram is 1 percent, the triphenylethylene phenol polyoxyethylene ether phosphate is 2 percent, the xanthan gum is 0.2 percent, and the water is complemented to 100 percent.
Example 17: according to the weight percentage, the prochloraz is 50 percent, the isooctanol is 20 percent, the fatty alcohol-polyoxyethylene ether is 5 percent, the thiram is 1 percent, the triphenyl vinyl phenol polyoxyethylene ether phosphate is 2 percent, the xanthan gum is 0.2 percent, and the water is complemented to 100 percent.
Example 18: according to the weight percentage, the prochloraz is 50 percent, the cyclohexanol is 20 percent, the fatty alcohol-polyoxyethylene ether is 5 percent, the thiram is 1 percent, the triphenylethylene phenol polyoxyethylene ether phosphate is 2 percent, the xanthan gum is 0.2 percent, and the water is complemented to 100 percent.
Example 19: the composition comprises, by weight, 1% of pyrisoxazole, 2% of n-octyl alcohol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water in balance to 100%.
Example 20: the composition comprises, by weight, 1% of pyrisoxazole, 2% of isooctanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water in balance to 100%.
Example 21: the composition comprises, by weight, 1% of pyrisoxazole, 2% of cyclohexanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 22: the composition comprises, by weight, 15% of pyrisoxazole, 15% of n-octyl alcohol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 23: the composition comprises, by weight, 15% of pyrisoxazole, 15% of isooctanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 24: the composition comprises, by weight, 15% of pyrisoxazole, 15% of cyclohexanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water, wherein the water is supplemented to 100%.
Example 25: the composition comprises, by weight, 50% of pyrisoxazole, 20% of n-octanol, 5% of fatty alcohol-polyoxyethylene ether, 1% of thiram, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2% of xanthan gum and water in balance to 100%.
Example 26: the composition comprises, by weight, 50% of pyrisoxazole, 20% of isooctanol, 5% of fatty alcohol-polyoxyethylene ether, 1% of thiram, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2% of xanthan gum and water in balance to 100%.
Example 27: according to the weight percentage, the pyridine bacteria oxazole is 50 percent, the cyclohexanol is 20 percent, the fatty alcohol polyoxyethylene ether is 5 percent, the thiram is 1 percent, the triphenylethylene phenol polyoxyethylene ether phosphate is 2 percent, the xanthan gum is 0.2 percent, and the water is complemented to 100 percent.
Example 28: the composition comprises, by weight, 1% of chlorpyrifos, 2% of n-octanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 29: the composition comprises, by weight, 1% of chlorpyrifos, 2% of isooctanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 30: according to the weight percentage, 1% of chlorpyrifos, 2% of cyclohexanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water are supplemented to 100%.
Example 31: according to the weight percentage, 15 percent of chlorpyrifos, 15 percent of n-octanol, 5 percent of fatty alcohol-polyoxyethylene ether, 15 percent of thiram, 1 percent of naphthalenesulfonic acid formaldehyde condensate, 2 percent of triphenylethylene phenol polyoxyethylene ether phosphate, 2 percent of polyoxyethylene polyoxypropylene block copolymer, 0.05 percent of xanthan gum and water which are complemented to 100 percent.
Example 32: according to the weight percentage, 15 percent of chlorpyrifos, 15 percent of isooctanol, 5 percent of fatty alcohol-polyoxyethylene ether, 15 percent of thiram, 1 percent of naphthalenesulfonic acid formaldehyde condensation compound, 2 percent of triphenylethylene phenol polyoxyethylene ether phosphate, 2 percent of polyoxyethylene polyoxypropylene block copolymer, 0.05 percent of xanthan gum and water which are complemented to 100 percent.
Example 33: according to the weight percentage, 15 percent of chlorpyrifos, 15 percent of cyclohexanol, 5 percent of fatty alcohol-polyoxyethylene ether, 15 percent of thiram, 1 percent of naphthalenesulfonic acid formaldehyde condensate, 2 percent of triphenylethylene phenol polyoxyethylene ether phosphate, 2 percent of polyoxyethylene polyoxypropylene block copolymer, 0.05 percent of xanthan gum and water which are complemented to 100 percent.
Example 34: according to the weight percentage, 50 percent of chlorpyrifos, 20 percent of n-octanol, 5 percent of fatty alcohol-polyoxyethylene ether, 1 percent of thiram, 2 percent of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2 percent of xanthan gum and water are complemented to 100 percent.
Example 35: according to the weight percentage, 50 percent of chlorpyrifos, 20 percent of isooctanol, 5 percent of fatty alcohol-polyoxyethylene ether, 1 percent of thiram, 2 percent of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2 percent of xanthan gum and water are complemented to 100 percent.
Example 36: according to the weight percentage, 50 percent of chlorpyrifos, 20 percent of cyclohexanol, 5 percent of fatty alcohol-polyoxyethylene ether, 1 percent of thiram, 2 percent of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2 percent of xanthan gum and water are complemented to 100 percent.
Example 37: the composition comprises, by weight, 1% of trifloxystrobin, 2% of n-octanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of a naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of a polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate, and the balance of water to 100%.
Example 38: the composition comprises, by weight, 1% of trifloxystrobin, 2% of isooctanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of a naphthalenesulfonic acid-formaldehyde condensate, 2% of a triphenylethylene phenol polyoxyethylene ether phosphate, 2% of a polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 39: the composition comprises, by weight, 1% of trifloxystrobin, 2% of cyclohexanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of a naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of a polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate, and water in a balance of 100%.
Example 40: the composition comprises, by weight, 15% of trifloxystrobin, 15% of n-octanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 41: the composition comprises, by weight, 15% of trifloxystrobin, 15% of isooctanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of a naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of a polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 42: the composition comprises, by weight, 15% of trifloxystrobin, 15% of cyclohexanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of a naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of a polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water, wherein the water is supplemented to 100%.
Example 43: according to the weight percentage, the trifloxystrobin is 50%, the n-octanol is 20%, the fatty alcohol-polyoxyethylene ether is 5%, the thiram is 1%, the triphenylethylene phenol polyoxyethylene ether phosphate is 2%, the xanthan gum is 0.2%, and the water is supplemented to 100%.
Example 44: according to the weight percentage, the trifloxystrobin is 50%, the isooctyl alcohol is 20%, the fatty alcohol-polyoxyethylene ether is 5%, the thiram is 1%, the triphenylethylene phenol polyoxyethylene ether phosphate is 2%, the xanthan gum is 0.2%, and the water is supplemented to 100%.
Example 45: the composition comprises, by weight, 50% of trifloxystrobin, 20% of cyclohexanol, 5% of fatty alcohol-polyoxyethylene ether, 1% of thiram, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2% of xanthan gum and water in a balance of 100%.
Example 46: the composition comprises, by weight, 1% of imazalil, 2% of n-octanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 47: the composition comprises, by weight, 1% of imazalil, 2% of isooctanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 48: the composition comprises, by weight, 1% of imazalil, 2% of cyclohexanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of a naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of a polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 49: the composition comprises, by weight, 15% of imazalil, 15% of n-octanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 50: the composition comprises, by weight, 15% of imazalil, 15% of isooctyl alcohol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 51: the composition comprises, by weight, 15% of imazalil, 15% of cyclohexanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water, wherein the water is supplemented to 100%.
Example 52: according to the weight percentage, 50 percent of imazalil, 20 percent of n-octanol, 5 percent of fatty alcohol-polyoxyethylene ether, 1 percent of thiram, 2 percent of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2 percent of xanthan gum and water are complemented to 100 percent.
Example 53: according to the weight percentage, 50 percent of imazalil, 20 percent of isooctanol, 5 percent of fatty alcohol-polyoxyethylene ether, 1 percent of thiram, 2 percent of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2 percent of xanthan gum and water are complemented to 100 percent.
Example 54: according to the weight percentage, 50 percent of imazalil, 20 percent of cyclohexanol, 5 percent of fatty alcohol-polyoxyethylene ether, 1 percent of thiram, 2 percent of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2 percent of xanthan gum and water are complemented to 100 percent.
Example 55: the composition comprises, by weight, 1% of pyraclostrobin, 2% of n-octanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 56: the composition comprises, by weight, 1% of pyraclostrobin, 2% of isooctanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water which are complemented to 100%.
Example 57: the composition comprises, by weight, 1% of pyraclostrobin, 2% of cyclohexanol, 2% of fatty alcohol-polyoxyethylene ether, 60% of thiram, 2% of a naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of a polyoxyethylene polyoxypropylene block copolymer, 0.02% of xanthan gum, 0.08% of magnesium aluminum silicate and water, wherein the water is supplemented to 100%.
Example 58: the composition comprises, by weight, 15% of pyraclostrobin, 15% of n-octanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water, wherein the water is supplemented to 100%.
Example 59: the composition comprises, by weight, 15% of pyraclostrobin, 15% of isooctanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Example 60: the composition comprises, by weight, 15% of pyraclostrobin, 15% of cyclohexanol, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water, wherein the water is supplemented to 100%.
Example 61: the composition comprises, by weight, 50% of pyraclostrobin, 20% of n-octanol, 5% of fatty alcohol-polyoxyethylene ether, 1% of thiram, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2% of xanthan gum and water in balance to 100%.
Example 62: the pesticide composition comprises, by weight, 50% of pyraclostrobin, 20% of isooctanol, 5% of fatty alcohol-polyoxyethylene ether, 1% of thiram, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2% of xanthan gum and water, wherein the water is supplemented to 100%.
Example 63: the composition comprises, by weight, 50% of pyraclostrobin, 20% of cyclohexanol, 5% of fatty alcohol-polyoxyethylene ether, 1% of thiram, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 0.2% of xanthan gum and water, wherein the water is supplemented to 100%.
Comparative example 1: 15% of propiconazole, 15% of 150# aromatic hydrocarbon solvent, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol-polyoxyethylene ether phosphate, 2% of polyoxyethylene-polyoxypropylene block copolymer, 0.05% of xanthan gum and water, wherein the water is supplemented to 100%.
Comparative example 2: 15% of propiconazole, 15% of methyl oleate, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and the balance of water to 100%.
Comparative example 3: 15% of prochloraz, 15% of 150# aromatic solvent, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water which are complemented to 100%.
Comparative example 4: 15% of prochloraz, 15% of methyl oleate, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and the balance of water to 100%.
Comparative example 5: 15% of pyrisoxazole, 15% of 150# aromatic solvent, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water for supplementing to 100%.
Comparative example 6: 15% of pyrisoxazole, 15% of methyl oleate, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and the balance of water to 100%.
Comparative example 7: 15% of chlorpyrifos, 15% of 150# aromatic solvent, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol-polyoxyethylene ether phosphate, 2% of polyoxyethylene-polyoxypropylene block copolymer, 0.05% of xanthan gum and water, wherein the water is supplemented to 100%.
Comparative example 8: 15% of chlorpyrifos, 15% of methyl oleate, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and the balance of water to 100%.
Comparative example 9: 15% of trifloxystrobin, 15% of 150# aromatic solvent, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and the balance of water to 100%.
Comparative example 10: 15% of trifloxystrobin, 15% of methyl oleate, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water in balance to 100%.
Comparative example 11: 15% of imazalil, 15% of 150# aromatic solvent, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and water, wherein the water is supplemented to 100%.
Comparative example 12: 15% of imazalil, 15% of methyl oleate, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and the balance of water to 100%.
Comparative example 13: 15% of pyraclostrobin, 15% of 150# aromatic solvent, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid-formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and the balance of water to 100%.
Comparative example 14: 15% of pyraclostrobin, 15% of methyl oleate, 5% of fatty alcohol-polyoxyethylene ether, 15% of thiram, 1% of naphthalenesulfonic acid formaldehyde condensate, 2% of triphenylethylene phenol polyoxyethylene ether phosphate, 2% of polyoxyethylene polyoxypropylene block copolymer, 0.05% of xanthan gum and the balance of water to 100%.
The stability test was carried out on the suspoemulsion obtained above:
the method specifically comprises the following steps: the samples of each of the above examples and comparative examples were tested for low temperature stability and thermal storage stability. The low temperature stability was tested in a low temperature apparatus at-5 ℃ for 7 days. The thermal storage stability was tested in an oven at 54 ℃ for 14 days. After completion of the test, the formulation was filtered through a 342 mesh screen, and the flowability of the formulation and the formation of crystals were observed.
The suspoemulsions were tested for low temperature storage stability (-5 ℃), high temperature storage stability (54 ℃) and stability on dilution at 30 ℃.
The determination results show that the preparation prepared in the embodiment of the invention has no crystal during cold and hot storage, no crystallization phenomenon occurs when the preparation is diluted by water, the particle size and the suspension rate are stable after hot storage, and table 1 is the determination effect data of the preparation obtained in some embodiments.
TABLE 1
Figure BDA0001932579080000131
As can be seen from the above tests, the compositions obtained in the examples of the present invention have no crystal during cold and hot storage, no crystallization occurs when the compositions are diluted with water, and the particle size and the suspension percentage are stable after hot storage. When the comparative example composition is placed at normal temperature after cold storage or hot storage, crystals are generated, the crystals crystallize after being diluted by water for two hours, the particle size sharply increases after the hot storage, and the suspension percentage sharply decreases after the hot storage; therefore, the composition suspension emulsion has high stability, inhibits the crystallization and austenite curing phenomena of the preparation, and obviously reduces the preparation cost.

Claims (10)

1. A suspended emulsion pesticide composition comprises an active component and an auxiliary agent, and is characterized in that: the composition comprises an active component and a solvent; the active components are compound A and thiram; wherein the compound A is a bactericidal compound with a melting point of less than 90 ℃; the solvent is at least one aliphatic alcohol or alicyclic alcohol for dissolving the compound A.
2. A suspoemulsion pesticidal composition according to claim 1 wherein: the effective content of active ingredients in the composition is 0.1-80%; wherein the weight ratio of the compound A to the thiram is 1:100-100: 1.
3. A suspoemulsion pesticidal composition according to claim 1 wherein: the weight ratio of the compound A to the solvent is 10:1 to 1: 10.
4. a suspoemulsion pesticidal composition according to claim 3 wherein: the weight ratio of the compound A to the solvent is 8: 1-1: 8.
5. a suspoemulsion pesticidal composition according to claim 1, 3 or 4 wherein: the solvent is selected from C4-C12Saturated fatty alcohol, C4-C12Unsaturated fatty alcohol, C4-C12Saturated branched fatty alcohol, C4-C12Unsaturated branched fatty alcohol, C6-C12One or more alicyclic alcohols.
6. A suspoemulsion pesticidal composition according to claim 5, wherein: the solvent is one or more of hexanol, n-octanol, isohexanol, isooctanol, cyclohexanol, alkyl substituted cyclohexanol, hexenol, octenol, decenol, cyclohexenol, and alkyl substituted cyclohexenol.
7. A suspoemulsion pesticidal composition according to claim 1 or 2 wherein: the compound A is propiconazole, prochloraz, pyrisoxazole, chlorpyrifos, trifloxystrobin, imazalil, pyraclostrobin, metalaxyl-M, tebufenpyrad, trifluralin, flusilazole or ipconazole.
8. A suspoemulsion pesticidal composition according to claim 1 wherein: the composition comprises, by weight, 1-50% of a low-melting-point compound A, 1-60% of thiram, 2-20% of a solvent, 7-10% of an auxiliary agent, and the balance of a carrier or a dispersion medium.
9. A suspoemulsion pesticidal composition according to claim 8 wherein: the auxiliary agent is one or more of wetting dispersant, emulsifier, thickener, antifreezing agent and stabilizer.
10. A method of preparing a suspoemulsion pesticidal composition of claim 1, characterized by:
(a) dispersing an oil phase: dissolving the compound A in at least one solvent of aliphatic alcohol or alicyclic alcohol;
(b) continuous aqueous phase: dissolving thiram in water to obtain thiram suspension;
(c) and uniformly mixing the dispersed oil and the water phase, and adding an auxiliary agent to obtain the suspended emulsion pesticide composition.
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