CN105410015B - A kind of chlopyrifos water dispersible granules and preparation method thereof - Google Patents

A kind of chlopyrifos water dispersible granules and preparation method thereof Download PDF

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Publication number
CN105410015B
CN105410015B CN201510991934.0A CN201510991934A CN105410015B CN 105410015 B CN105410015 B CN 105410015B CN 201510991934 A CN201510991934 A CN 201510991934A CN 105410015 B CN105410015 B CN 105410015B
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chlopyrifos
sodium
water dispersible
dispersible granules
present
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CN105410015A (en
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孙国庆
侯永生
张全
吴勇
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Shandong Weifang Rainbow Chemical Co Ltd
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Shandong Weifang Rainbow Chemical Co Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N57/00Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
    • A01N57/10Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
    • A01N57/16Biocides, 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
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/12Powders or granules
    • A01N25/14Powders or granules wettable

Abstract

The present invention provides a kind of chlopyrifos water dispersible granules, is prepared by the material including following mass fraction component:Chlopyrifos:10~75%, dispersant:1~10%, wetting agent:1~5%, chelating agent:1~5%, disintegrant:1~25%, adsorbent:1~10%, surplus is filler;The dispersant includes one or more of sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts, maleic acrylic copolymer salt, calcium lignosulfonate and polycarboxylate;The wetting agent includes one or more of lauryl sodium sulfate, sodium lignin sulfonate, Nekal BX and alkyl phenol polyethenoxy ether sodium sulfate;The chelating agent includes one or more of ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate and sodium tripolyphosphate.Chlopyrifos water dispersible granules active constituent content in the present invention is high and environmentally friendly, has good dispersibility and higher suspensibility.

Description

A kind of chlopyrifos water dispersible granules and preparation method thereof
Technical field
The invention belongs to technical field of pesticide preparations more particularly to a kind of chlopyrifos water dispersible granules and preparation method thereof.
Background technology
Chlopyrifos, English name chlorpyrifos, chemical name O, O- diethyl-O- (3,5,6- tri- Chloro-2-Pyridyles Base) phosphorothionate, it is crystallized for white granular.Chlopyrifos, which is one kind, having moderately toxic organophosphorus insecticide, has and touches It kills, stomach toxicity and fumigation action, can preferably prevent the pest above and below the ground of various crop, for rice, wheat, cotton, fruit Tree, vegetables, a variety of chewing types and sucking pest on tea tree, it can also be used to prevent sanitary insect pest.
The chlopyrifos preparation occurred currently on the market is mainly missible oil and wettable powder, the former is because use a large amount of emulsifications Agent, solvent cause waste of solvent and environmental pollution, and the latter is due in processing link, causing dust pollution using link and influence Environmental issue.
103238624 B of patent CN disclose a kind of chlopyrifos tablet and preparation method thereof, and machinery is used to mixed material Compressing dry granulation is carried out after crushing, although the tablet in the patent is more environmentally friendly to environment, in mechanical crushing or tabletting Cheng Zhong, temperature of charge easily heat up and material are caused to melt, to influence product quality.Currently, single chlopyrifos drug effectively at The water dispersible granules and preparation method thereof divided have not been reported.
Invention content
It is provided by the invention to poison with poison the purpose of the present invention is to provide a kind of chlopyrifos water dispersible granules and preparation method thereof Tick water dispersible granules are to environment environmental protection, and product active constituent content is high, and herbicidal effect is good.
The present invention provides a kind of chlopyrifos water dispersible granules, is prepared by the material including following mass fraction component:
Chlopyrifos:10~75%, dispersant:1~10%, wetting agent:1~5%, chelating agent:1~5%, disintegrant:1~ 25%, adsorbent:1~10%, surplus is filler;
The dispersant includes sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts, maleic acid-acrylic acid copolymer salt, lignin One or more of sulfoacid calcium and polycarboxylate;
The wetting agent includes lauryl sodium sulfate, sodium lignin sulfonate, Nekal BX and alkyl phenol polyoxyethylene ether One or more of sodium sulphate;
The chelating agent includes ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate and trimerization phosphorus One or more of sour sodium.
Preferably, the dispersant includes maleic acid-acrylic acid copolymer salt and calcium lignosulfonate;
The mass ratio of the maleic acid-acrylic acid copolymer salt and calcium lignosulfonate is (1~2):1.
Preferably, the mass fraction of the dispersant is 3~8%.
Preferably, the wetting agent includes lauryl sodium sulfate and sodium lignin sulfonate;
The mass ratio of the lauryl sodium sulfate and sodium lignin sulfonate is 0.5:(0.5~2).
Preferably, the mass fraction of the wetting agent is 1.5~4%.
Preferably, the chelating agent include ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate and One or more of sodium tripolyphosphate;
The mass fraction of the chelating agent is 2~4%.
Preferably, the disintegrant includes one kind in calcium chloride, potassium sulfate, diammonium hydrogen phosphate, potassium nitrate and sodium chloride Or it is several;
The mass fraction of the disintegrant is 5~20%.
Preferably, the adsorbent includes one or more of sodium benzoate, white carbon and diatomite;
The mass fraction of the adsorbent is 4~8%.
Preferably, the filler includes one or more of calcined kaolin, cornstarch, bentonite and talcum powder.
The present invention provides a kind of preparation method of chlopyrifos water dispersible granules, includes the following steps:
A) based on mass fraction, by 10~75% chlopyrifos, 1~10% dispersant, 1~5% wetting agent, 1~ 5% chelating agent, 1~25% disintegrant, 1~10% adsorbent and the filler mixing of surplus, obtain mixed material;
The dispersant includes sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts, maleic acid-acrylic acid copolymer salt, lignin One or more of sulfoacid calcium and polycarboxylate;
The wetting agent includes lauryl sodium sulfate, sodium lignin sulfonate, Nekal BX and alkyl phenol polyoxyethylene ether One or more of sodium sulphate;
The chelating agent includes ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate and trimerization phosphorus One or more of sour sodium;
B) by the step A) in mixed material be granulated, obtain chlopyrifos water dispersible granules.
The present invention provides a kind of chlopyrifos water dispersible granules, is prepared by the material including following mass fraction component: Chlopyrifos:10~75%, dispersant:1~10%, wetting agent:1~5%, chelating agent:1~5%, disintegrant:1~25%, it inhales Attached dose:1~10%, surplus is filler;The dispersant includes sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts, maleic acid-propylene One or more of acid copolymer salt, calcium lignosulfonate and polycarboxylate;The wetting agent include lauryl sodium sulfate, One or more of sodium lignin sulfonate, Nekal BX and alkyl phenol polyethenoxy ether sodium sulfate.Using specific in the present invention Dispersant and specific wetting agent, be prepared chlopyrifos water dispersible granules, the chlopyrifos water dispersible granules in the present invention have Effective component content is high, does not use organic solvent, environmentally friendly, and has good dispersibility and higher suspensibility, The experimental results showed that the 3WHO aqueous suspension rates of the chlopyrifos water dispersible granules in the present invention are up to 97.4%, rice terrace rice is flown Preventive effect after lice medication 14 days is 96.6%.
Specific implementation mode
The present invention provides a kind of chlopyrifos water dispersible granules, are prepared by the material including following mass fraction component It arrives:
Chlopyrifos:10~75%, dispersant:1~10%, wetting agent:1~5%, chelating agent:1~5%, disintegrant:1~ 25%, adsorbent:1~10%, surplus is filler;
The dispersant includes sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts, maleic acid-acrylic acid copolymer salt, lignin One or more of sulfoacid calcium and polycarboxylate;
The wetting agent includes lauryl sodium sulfate, sodium lignin sulfonate, Nekal BX and alkyl phenol polyoxyethylene ether One or more of sodium sulphate;
The chelating agent includes ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate and trimerization phosphorus One or more of sour sodium.
Chlopyrifos water dispersible granules active constituent content provided by the invention is high, does not use organic solvent, to environment friend It is good, and with good dispersibility and higher suspensibility.
In the present invention, the mass fraction of the chlopyrifos be 10~75%, preferably 15~65%, more preferably 25~ 50%;Specifically, in an embodiment of the present invention, the mass fraction of chlopyrifos can be 10%, 75%, 25%, 18%, 35%, 32%, 50% and 47%.The present invention does not have the source of the chlopyrifos special limitation, and Lear chemistry stock can be used The 97% chlopyrifos product that part Co., Ltd provides.
In the present invention, the dispersant includes sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts, maleic-acrylic acid copolymerization One or more of object salt, calcium lignosulfonate and polycarboxylate;Preferably include maleic acid-acrylic acid copolymer salt and wooden The mass ratio of plain sulfoacid calcium, the maleic acid-acrylic acid copolymer salt and calcium lignosulfonate is preferably (1~2):1, more preferably It is 1.5:1;The mass fraction of the dispersant is 1~10%, preferably 3~8%, more preferably 4~6%;Specifically, at this Can be 5%, 7%, 10% or 6% in the embodiment of invention, e.g., by maleic acid-acrylic acid copolymer salt 3% and lignin Sulfoacid calcium 2% is used cooperatively, and maleic acid-acrylic acid copolymer salt 3% and sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts 4% coordinate It uses, calcium lignosulfonate 4% and polycarboxylate 6% are used cooperatively, maleic acid-acrylic acid copolymer salt 1%, polycarboxylate 3% and 2% three of calcium lignosulfonate be used cooperatively, sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts 3%, calcium lignosulfonate 2% and polycarboxylate 2% be used cooperatively.The present invention does not have the source of the dispersant special limitation, specifically, in this hair In bright embodiment, the calcium lignosulfonate of Meadwestvaco companies offer can be used.
In the present invention, the wetting agent includes lauryl sodium sulfate, sodium lignin sulfonate, Nekal BX and alkyl phenol One or more of polyethenoxy ether sodium sulfate;Preferably include lauryl sodium sulfate and sodium lignin sulfonate, described 12 The mass ratio of sodium alkyl sulfate and sodium lignin sulfonate is preferably 0.5:(0.5~2), more preferably 0.5:1;The wetting agent Mass fraction is 1~5%, preferably 1.5~4%, specifically, in an embodiment of the present invention, the quality point of the wetting agent Number may be used 1.5%, 3%, 2% or 4.5%.A variety of wetting agents are preferably used cooperatively by the present invention, e.g., dodecyl sulphate Sodium 0.5% and sodium lignin sulfonate 1% are used cooperatively;Lauryl sodium sulfate 1% and sodium lignin sulfonate 2% are used cooperatively; Sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts 4% and Nekal BX 2% are used cooperatively;It lauryl sodium sulfate 1.5% and pulls open Powder BX 3% is used cooperatively;Alkyl phenol polyethenoxy ether sodium sulfate 0.5%, Nekal BX 0.5% and sodium lignin sulfonate 1% Three is used cooperatively;Sodium lignin sulfonate 1% and alkyl phenol polyethenoxy ether sodium sulfate 1% are used cooperatively.The present invention is to described The source of wetting agent does not have special limitation, specifically, in an embodiment of the present invention, the huge victory in Hubei can be used in the wetting agent The lauryl sodium sulfate that Science and Technology Ltd. provides.
In the present invention, the chelating agent includes ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, ethylenediamine tetra-acetic acid four One or more of sodium and sodium tripolyphosphate;The mass fraction of the chelating agent is 1~5%, preferably 2~4%, specifically , it can be 1.5%, 1%, 2%, 3%, 5%, 2.5% in an embodiment of the present invention, a variety of chelating agents can also be taken It is used cooperatively with use, such as sodium tripolyphosphate 1% and tetrasodium ethylenediamine tetraacetate 1.5%.The present invention carrys out the chelating agent Source does not have special limitation, specifically, in an embodiment of the present invention, the chelating agent can be used Jinan and praise the limited public affairs of abundant chemical industry The tetrasodium ethylenediamine tetraacetate provided is provided.In the present invention, the chelating agent can improve the chlopyrifos water dispersible granules Hard water resistance performance.
In the present invention, the disintegrant preferably includes calcium chloride, potassium sulfate, diammonium hydrogen phosphate, potassium nitrate and sodium chloride One or more of;The mass fraction of the disintegrant is 1~25%, more preferably 5~20%, specifically, in the present invention Embodiment in, can be 6%, 10%, 4%, 25% or 16%.
In the present invention, the adsorbent preferably includes one or more of sodium benzoate, white carbon and diatomite;Institute The mass fraction for stating adsorbent is 1~10%, preferably 4~8%, more preferably 7%, 10%, 5%, 3% or 4%.The present invention There is no special limitation to the source of the adsorbent, specifically, in an embodiment of the present invention, Yixing City monarch can be used and join object Provide the diatomite that Co., Ltd provides.
In the present invention, the filler includes one kind or several in calcined kaolin, cornstarch, bentonite and talcum powder Kind;The sum of the filler and the mass percent of other raw materials are 100%.
Specifically, based on mass fraction, following proportioning may be used in the chlopyrifos water dispersible granules in the present invention:
Chlopyrifos 10%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 0.5%, sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1.5%, sodium chloride 6%, white carbon 4%, calcined kaolin are mended Foot 100%;
Chlopyrifos 75%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 0.5%, sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1.5%, sodium chloride 6%, white carbon 4%, calcined kaolin are mended Foot 100%;
Chlopyrifos 25%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 0.5%, sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1%, sodium chloride 6%, white carbon 5%, calcined kaolin are supplied 100%;
Chlopyrifos 18%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 1%, sodium lignin sulfonate 2%, tetrasodium ethylenediamine tetraacetate 2%, sodium chloride 10%, white carbon 3%, calcined kaolin are supplied 100%;
Chlopyrifos 35%, sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts 4%, is drawn maleic acid-acrylic acid copolymer salt 3% It opens powder BX 2%, disodium ethylene diamine tetraacetate 1.5%, potassium sulfate 4%, diatomite 3%, bentonite and supplies 100%;
Chlopyrifos 32%, calcium lignosulfonate 4%, polycarboxylate 6%, lauryl sodium sulfate 1.5%, Nekal BX 3%, sodium tripolyphosphate 3%, potassium nitrate 25%, sodium benzoate 5%, talcum powder supply 100%;
Chlopyrifos 50%, maleic acid-acrylic acid copolymer salt 1%, polycarboxylate 3%, calcium lignosulfonate 2%, alkyl Phenol polyethenoxy ether sodium sulfate 0.5%, Nekal BX 0.5%, sodium lignin sulfonate 1%, ethylenediamine tetra-acetic acid 5%, phosphoric acid hydrogen Diammonium 10%, white carbon 10%, talcum powder supply 100%;
Chlopyrifos 47%, sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts 3%, calcium lignosulfonate 2%, polycarboxylate 2%, Sodium lignin sulfonate 1%, alkyl phenol polyethenoxy ether sodium sulfate 1%, sodium tripolyphosphate 1%, tetrasodium ethylenediamine tetraacetate 1.5%, calcium chloride 16%, diatomite 7%, cornstarch supply 100%.
The present invention also provides a kind of preparation methods of chlopyrifos water dispersible granules, include the following steps:
A) based on mass fraction, by 10~75% chlopyrifos, 1~10% dispersant, 1~5% wetting agent, 1~ 5% chelating agent, 1~25% disintegrant, 1~10% adsorbent and the filler mixing of surplus, obtain mixed material;
The dispersant includes sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts, maleic acid-acrylic acid copolymer salt, lignin One or more of sulfoacid calcium and polycarboxylate;
The wetting agent includes lauryl sodium sulfate, sodium lignin sulfonate, Nekal BX and alkyl phenol polyoxyethylene ether One or more of sodium sulphate;
The chelating agent includes ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate and trimerization phosphorus One or more of sour sodium;
B) by the step A) in mixed material be granulated, obtain chlopyrifos water dispersible granules.
The present invention is preferably by 10~75% chlopyrifos, 1~10% dispersant, 1~5% wetting agent, 1~5% The filler addition mixing machine of chelating agent, 1~25% disintegrant, 1~10% adsorbent and surplus, after mixing, progress It crushes, then the material after crushing is mixed, obtain mixed material.In the present invention, the chlopyrifos, dispersant, wetting Agent, chelating agent.Disintegrant, the type of adsorbent and filler, dosage and source and above-mentioned technical proposal Chlorpyrifos, dispersant, Wetting agent, chelating agent.Disintegrant, adsorbent and the type of filler, dosage are consistent with source, and details are not described herein.
In the present invention, the grain size of the crushing is preferably 20~40 μm, more preferably 25~35 μm;The present invention preferably adopts The crushing of above-mentioned material is carried out with airslide disintegrating mill.
After obtaining mixed material, present invention preferably employs the method being granulated is mediated, the mixed material is pelletized, institute It is preferably the 20~30% of mixed material quality, more preferably 25~28% to state and mediate amount of water;It is described to mediate the process being granulated For method of granulating well known to those skilled in the art.
After completing granulation, the present invention preferably dries the obtained water dispersible granules of pelletizing, and obtains methoxy miaow grass Cigarette water dispersible granules.In the present invention, the temperature of the drying is preferably 30~50 DEG C, more preferably 35~45 DEG C;The baking The dry time is preferably 30~50min.
The present invention tests Chlorpyrifos water dispersible granules of the present invention according to the assay method of 184 suspensibilities of CIPAC MT Suspensibility, the results showed that, the present invention in chlopyrifos water dispersible granules aqueous suspension rate be 97.4%.
The present invention stores chlopyrifos water dispersible granules 14 days at 54 DEG C, then tests Chlorpyrifos moisture of the present invention The stability of shot agent, the results showed that, the present invention in chlopyrifos water dispersible granules stability it is preferable, heat storage after disintegration and The variation of aqueous suspension rate is little.
The present invention is into the 100mL tool plug graduated cylinders (interior high 22.5cm, internal diameter 28mm) containing 90mL distilled water, at 25 DEG C The chlopyrifos water dispersible granules 0.5g in the present invention is added, clamps the middle part of graduated cylinder later, clogs nozzle, with the speed of 8r/min It is rotated around center, until sample is disintegrated completely in water, the results showed that, the chlopyrifos water dispersible granules in the present invention are in 60s Disintegration completely.
Method during the present invention is tested according to CIPAC MT185 wet screenings tests Chlorpyrifos water dispersible granules of the present invention Wet screening tests percent of pass, the results showed that, the wet screening experiment percent of pass of Chlorpyrifos water dispersible granules of the present invention is 99.9%.
The present invention tests Chlorpyrifos water dispersible granules of the present invention to the control effect of rice terrace planthopper, as a result table Bright, Chlorpyrifos water dispersible granules of the present invention are up to 96.6% to the preventive effect after rice terrace planthopper medication 14 days.
The present invention provides a kind of chlopyrifos water dispersible granules, is prepared by the material including following mass fraction component: Chlopyrifos:10~75%, dispersant:1~10%, wetting agent:1~5%, chelating agent:1~5%, disintegrant:1~25%, it inhales Attached dose:1~10%, surplus is filler;The dispersant includes sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts, maleic acid-propylene One or more of acid copolymer salt, calcium lignosulfonate and polycarboxylate;The wetting agent include lauryl sodium sulfate, One or more of sodium lignin sulfonate, Nekal BX and alkyl phenol polyethenoxy ether sodium sulfate.Chlopyrifos in the present invention Water dispersible granules have the following advantages:(1) use and the dust pollution of a large amount of organic solvents, safety and environmental protection, convenient for storage are avoided Deposit transport;(2) processing method is simple, is conducive to serialization industrial production;(3) active constituent content is high, reduce packaging, transport at This;(4) chelating agent is added, there is stronger hard water resistance effect, it is without geographical restrictions, more adaptable.
In order to further illustrate the present invention, with reference to embodiments to a kind of chlopyrifos water dispersible granules provided by the invention And preparation method thereof be described in detail, but limiting the scope of the present invention cannot be understood as.
In the examples below, chlopyrifos is purchased from Lier Chemical Co., Ltd;Polycarboxylate, maleic acid-propylene Acid copolymer salt is purchased from HUNTSMAN;Calcium lignosulfonate, sodium lignin sulfonate are purchased from Meadwestvaco;White carbon is purchased From in Weifang Jin Haiwang Chemical Co., Ltd.s;Calcined kaolin is purchased from Jinan Man Hong Chemical Co., Ltd.s;Alkyl phenol polyoxy second Alkene ether sodium sulfate, sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts are purchased from the promise of Zhengzhou nation purchased from Clariant, Nekal BX Chemical product Co., Ltd;Diatomite is purchased from Yixing City Jun Lian goods and materials Co., Ltd;Bentonite is purchased from Weifang letter Xiang bentonite Co., Ltd;Talcum powder is purchased from Weifang Xin Fa talcum powder Co., Ltd;Cornstarch is purchased from the sub- limited public affairs of Anhua work in Jinan Department.
1 10% chlopyrifos water dispersible granules of embodiment
Formula is:Chlopyrifos 10%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, dodecyl sulphur Sour sodium 0.5%, sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1.5%, sodium chloride 6%, white carbon 4%, calcining kaolinite Soil supplies 100%.
Preparation method is:By the chlopyrifos of above-mentioned formula dosage, dispersant, wetting agent, chelating agent, disintegrant, adsorbent, Filler is added in mixing machine and is uniformly mixed, and after airslide disintegrating mill is crushed to 25-35 μm of grain size, remixes uniformly, mediates and add water Amount 30%, is granulated, 40 DEG C of drying, you can 10% chlopyrifos water dispersible granules product is made.
2 75% chlopyrifos water dispersible granules of embodiment
Formula is:Chlopyrifos 75%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, dodecyl sulphur Sour sodium 0.5%, sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1.5%, sodium chloride 6%, white carbon 4%, calcining kaolinite Soil supplies 100%.The preparation method is the same as that of Example 1.
3 25% chlopyrifos water dispersible granules of embodiment
Formula is:Chlopyrifos 25%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, dodecyl sulphur Sour sodium 0.5%, sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1%, sodium chloride 6%, white carbon 5%, calcined kaolin Supply 100%.The preparation method is the same as that of Example 1.
4 18% chlopyrifos water dispersible granules of embodiment
Formula is:Chlopyrifos 18%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, dodecyl sulphur Sour sodium 1%, sodium lignin sulfonate 2%, tetrasodium ethylenediamine tetraacetate 2%, sodium chloride 10%, white carbon 3%, calcined kaolin are mended Foot 100%.The preparation method is the same as that of Example 1.
5 35% chlopyrifos water dispersible granules of embodiment
Formula is:Chlopyrifos 35%, maleic acid-acrylic acid copolymer salt 3%, sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts 4%, Nekal BX 2%, disodium ethylene diamine tetraacetate 1.5%, potassium sulfate 4%, diatomite 3%, bentonite supply 100%.System Preparation Method is the same as embodiment 1.
6 32% chlopyrifos water dispersible granules of embodiment
Formula is:Chlopyrifos 32%, polycarboxylate 6%, lauryl sodium sulfate 1.5%, is drawn calcium lignosulfonate 4% It opens powder BX 3%, sodium tripolyphosphate 3%, potassium nitrate 25%, sodium benzoate 5%, talcum powder and supplies 100%.Preparation method is the same as real Apply example 1.
7 50% chlopyrifos water dispersible granules of embodiment
Formula is:Chlopyrifos 50%, maleic acid-acrylic acid copolymer salt 1%, polycarboxylate 3%, calcium lignosulfonate 2%, alkyl phenol polyethenoxy ether sodium sulfate 0.5%, Nekal BX 0.5%, sodium lignin sulfonate 1%, ethylenediamine tetra-acetic acid 5%, diammonium hydrogen phosphate 10%, white carbon 10%, talcum powder supply 100%.The preparation method is the same as that of Example 1.
8 47% chlopyrifos water dispersible granules of embodiment
Formula is:Chlopyrifos 47%, sub- double naphthalenesulfonate formaldehyde condensation compound sodium salts 3%, calcium lignosulfonate 2%, poly- carboxylic Hydrochlorate 2%, sodium lignin sulfonate 1%, alkyl phenol polyethenoxy ether sodium sulfate 1%, sodium tripolyphosphate 1%, ethylenediamine tetra-acetic acid Four sodium 1.5%, calcium chloride 16%, diatomite 7%, cornstarch supply 100%.The preparation method is the same as that of Example 1.
1 10% chlopyrifos water dispersible granules of comparative example
Formula is:Chlopyrifos 10%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, dodecyl sulphur Sour sodium 0.5%, sodium lignin sulfonate 1%, sodium chloride 6%, white carbon 4%, calcined kaolin supply 100%.Preparation method is same Embodiment 1.
2 75% chlopyrifos water dispersible granules of comparative example
Formula is:Chlopyrifos 75%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, dodecyl sulphur Sour sodium 0.5%, sodium lignin sulfonate 1%, sodium chloride 6%, white carbon 4%, calcined kaolin supply 100%.Preparation method is same Embodiment 1.
3 14% chlopyrifos water dispersible granules of comparative example
Chlopyrifos 14%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 0.5%, sodium lignin sulfonate 1%, laminated crystal of sodium disilicate 1.5%, sodium chloride 6%, white carbon 4%, calcined kaolin are mended Foot 100%.
The present invention surveys the stability for the chlopyrifos water dispersible granules that Examples 1 to 8 and comparative example 1~3 obtain Examination, the results are shown in Table 1, and table 1 is the steady of the chlopyrifos water dispersible granules that the embodiment of the present invention 1~8 and comparative example 1~3 obtain Qualitative test result.
The stability test result for the chlopyrifos water dispersible granules that 1 embodiment of the present invention 1~8 of table and comparative example 1~3 obtain
Known by table 1, the product stability in the embodiment of the present invention is preferable, and the disintegration and the variation of aqueous suspension rate after heat storage are not Greatly, after specific preferred auxiliary agent has especially been selected in Examples 1 to 4, property indices are better, and aqueous suspension rate exists 94% or more, reach as high as 97.4%.
Rice terrace planthopper prevents field control effectiveness test
Test medicine:
Chlopyrifos water dispersible granules made from the embodiment of the present invention 1~8 and comparative example 1~3;
Comparison medicament is:480g/L chlopyrifos EC (is purchased from Shandong Dongtai Agrochemical Co., Ltd).
Experimental condition and application method:
This experiment is arranged in the progress of the Feixi County towns San He, and prevention planthopper carries out in late rice, and preceding stubble is early rice. Experimental field fertility uniformity, topography are flat.The inclined sand mold of soil, middle fertility.Rice is in milk stage when experiment, in planthopper Deng generation.Medical instruments use -16 type knapsack sprayer of workers and peasants, spouting liquid 50kg/667m2, artificial even spraying.Field when dispenser Between keep 3~5cm of water layer, 7d is retained after medicine, so that drug effect plays.Investigate insect population before dispenser, 7,14d is adjusted respectively after medicine Residual borer population living is looked into, Revision insect recluced rate and Rectifying efficacies are calculated.Its control effect see the table below 2, and table 2 is the embodiment of the present invention 1~8 With the chlopyrifos water dispersible granules in comparative example 1~2 to the preventive effect of rice terrace planthopper.
The check plot is clear water check plot, does not spray medicament.
Chlopyrifos water dispersible granules in 2 embodiment of the present invention 1~8 of table and comparative example 1~3 prevent rice terrace planthopper Effect
As can be seen from Table 2, the present invention in chlopyrifos water dispersible granules preventive effect be maintained at 85% or more, by match with And the optimizely select of different type auxiliary agent is matched, the water dispersible granules drug effect as obtained by Examples 1 to 44 is more preferably.Without containing chela of the present invention The water dispersible granules and comparative example 3 of the comparative example 1~2 of mixture use the water dispersible granules of other kind of quasi-chelate compound since it is anti- Hard water effect is poor, therefore preventive effect is relatively poor.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (2)

1. a kind of chlopyrifos water dispersible granules are prepared by the material including following mass fraction component:
Chlopyrifos 10%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 0.5%, Sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1.5%, sodium chloride 6%, white carbon 4%, calcined kaolin are supplied 100%;
Or
Chlopyrifos 75%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 0.5%, Sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1.5%, sodium chloride 6%, white carbon 4%, calcined kaolin are supplied 100%;
Or
Chlopyrifos 25%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 0.5%, Sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1%, sodium chloride 6%, white carbon 5%, calcined kaolin supply 100%;
Or
Chlopyrifos 18%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 1%, wood Quality sodium sulfonate 2%, tetrasodium ethylenediamine tetraacetate 2%, sodium chloride 10%, white carbon 3%, calcined kaolin supply 100%.
2. a kind of preparation method of chlopyrifos water dispersible granules, includes the following steps:
A) material is mixed, obtains mixed material;
The material includes the component of following mass fraction:Chlopyrifos 10%, maleic acid-acrylic acid copolymer salt 3%, lignin Sulfoacid calcium 2%, lauryl sodium sulfate 0.5%, sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1.5%, sodium chloride 6%, white carbon 4%, calcined kaolin supply 100%;
Or
Chlopyrifos 75%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 0.5%, Sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1.5%, sodium chloride 6%, white carbon 4%, calcined kaolin are supplied 100%;
Or
Chlopyrifos 25%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 0.5%, Sodium lignin sulfonate 1%, tetrasodium ethylenediamine tetraacetate 1%, sodium chloride 6%, white carbon 5%, calcined kaolin supply 100%;
Or
Chlopyrifos 18%, maleic acid-acrylic acid copolymer salt 3%, calcium lignosulfonate 2%, lauryl sodium sulfate 1%, wood Quality sodium sulfonate 2%, tetrasodium ethylenediamine tetraacetate 2%, sodium chloride 10%, white carbon 3%, calcined kaolin supply 100%;
B) by the step A) in mixed material be granulated, obtain chlopyrifos water dispersible granules.
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