CN1224318C - Amide-type herbiciding aqueous emulsion and its preparing process - Google Patents

Amide-type herbiciding aqueous emulsion and its preparing process Download PDF

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CN1224318C
CN1224318C CN 02138107 CN02138107A CN1224318C CN 1224318 C CN1224318 C CN 1224318C CN 02138107 CN02138107 CN 02138107 CN 02138107 A CN02138107 A CN 02138107A CN 1224318 C CN1224318 C CN 1224318C
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aqueous emulsion
water
emulsion
amide
oil phase
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CN1395831A (en
Inventor
徐年凤
朱学林
沈敏
马学明
韩顺宁
张瑶
熊建民
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JIANGSU LULILAI CO Ltd
JIANGSU PROV INST OF AGRICULTURAL CHEMICALS
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Abstract

The present invention relates to an aqueous emulsion prepared from an amide type weeding active substance of which the structural formula (1) is disclosed in the specification, an added emulsifying agent, an added dispersing agent, etc., and a preparing process of the aqueous emulsion. The aqueous emulsion is prepared from the raw amide type weeding active substance of which the structural formula (1) is disclosed in the specification, the emulsifying agent, an antifreeze agent and aquae through mixing and stir. The preparing process comprises: uniformly mixing the raw amide type weeding active substance with the emulsifying agent firstly to obtain an oil phase; then uniformly mixing the antifreeze agent and the aquae in the components to obtain an aqueous phase; adding the aqueous phase to the oil phase while stirring the mixture to obtain an emulsion; homogenizing the emulsion by a homogenizer to obtain the stable amide type weeding aqueous emulsion of the present invention.

Description

Amide-type herbiciding aqueous emulsion and production method thereof
Technical field
The present invention relates to a kind of amide-type herbiciding active substance that contains structural formula for (1), add aqueous emulsion and production method thereof that emulsifier, dispersant etc. are formed.
Background technology
Along with the use of chemical pesticide, the worldwide environment and the ecological balance have all been suffered serious destruction.The toxicity of agricultural chemicals, residual and environmental pollution is very serious in China in order to address this problem, should be strengthened the development to the novel pesticide of high-efficiency low-toxicity, easily biological-degradable and environmentally compatible on the one hand, will study, develops and use the environment friendly agricultural preparation on the other hand.Along with China becomes a full member of the World Trade Organization, more should strengthen the research and development of environment-friendly type pesticides new formulation, to strengthen the international competitiveness of China's pesticide industry.
Summary of the invention
Purpose of the present invention is exactly in order to address the above problem, and proposes that a kind of technology is simple, equipment investment is few, is convenient to the amide-type herbiciding aqueous emulsion and the production method thereof of penetration and promotion.
The objective of the invention is to realize by following technical solution:
Amide-type herbiciding aqueous emulsion of the present invention contains (weight percent composition):
Structural formula is the former medicine 10-60% of the acetamide-group herbicides of (1)
Emulsifier 2-10%
Antifreeze 2-10%
Water surplus
Production method of the present invention is, former medicine of acetamide-group herbicides in the said components and emulsifier are evenly made oil phase, antifreeze in the component and water mixed make water, while stirring water is added oil phase and make emulsion, after homogenizer homogenizes, promptly get the stable aqueous emulsion product of the present invention again.
Product of the present invention greatly reduces preparation and changes into this with water to replace organic solvent, and the stronger market competitiveness is arranged; On the other hand,, reduced pollution,, belonged to environmental type agricultural chemicals novel formulation, after applying, will produce important social benefit and economic benefit operator safety to environment because product does not contain organic solvent.
Embodiment
Amide-type herbiciding aqueous emulsion of the present invention by structural formula is
The former medicine of acetamide-group herbicides, emulsifier, antifreeze and water make through mix stirring, the percentage by weight of its each composition consists of:
Structural formula is the former medicine 10-60% of the acetamide-group herbicides of (1)
Emulsifier 2-10%
Antifreeze 2-10%
Water is supplied surplus
Production method of the present invention is, former medicine of acetamide-group herbicides in the said components and emulsifier are evenly made oil phase, make water and the antifreeze in the component and water mixed, while stirring water is added oil phase and make emulsion, after homogenizer homogenizes, promptly get stable amide-type herbiciding aqueous emulsion product of the present invention again.
In described each the composition combination of the above-mentioned technical solution of the present invention:
Structural formula is the R in the former medicine of the acetamide-group herbicides of (1) 1, R 2Desirable CH 3, C 2H 5, R 3Desirable CH 2OCH 3, CH 2OC 2H 5, CH 2OC 3H 7, (CH 3) CHCH 2OCH 3, CH 2OC 4H 9Deng the alkyl ether group;
Emulsifier is: alkyl phenol ethylene oxide condensate, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene, fatty acid and ethylene oxide condensate, sodium alkyl benzene sulfonate, phenethyl phenol polyethenoxy ether, they may be used alone, can also be used in combination.
Sometimes need in oil phase, optionally to add following dispersant: sorbitan monooleate APEO, polyoxyethylene sorbitol liver monostearate APEO, polyoxyethylene sorbitol liver monostearate, phenethyl phenol polyethenoxy ether phenylsulfate, polyvinyl alcohol, fatty alcohol-polyoxyethylene ether etc., consumption is 1-8%, they may be used alone, can also be used in combination; Sometimes need to select to add following thickener at aqueous phase: polyacrylate, Magnesiumaluminumsilicate, carboxymethyl cellulose, xanthans, PAA etc., consumption is 0.2-3%, they may be used alone, can also be used in combination.
Antifreeze is: ethylene glycol, propane diols, urea, glycerine, isopropyl alcohol etc.They may be used alone, can also be used in combination.
The present invention also can add amount of colorant.
The invention will be further described below in conjunction with embodiment:
Example 1
Get third careless amine weed killer herbicide 53 grams, alkyl phenol ethylene oxide condensate 6 grams, fatty alcohol-polyoxyethylene ether 4 gram mixing, heated and stirred makes it to form uniform oil phase I slightly, getting xanthans 0.1 gram, propane diols 6 grams and water 24.74 grams mixes, stir into homogeneous water II, stir on the limit, and the limit adds uniform water II among the above-mentioned oil phase I that is made into, and constantly stirs and make it to become emulsion, emulsion is added to high pressure homogenizer homogenizes, promptly get 50% the third careless amine aqueous emulsion.
Embodiment 2
Get Acetochlor weed killer herbicide 53 grams, alkylphenol polyoxyethylene 5 grams, the 3 gram mixing of alkylphenol-polyethenoxy phosphate, heated and stirred makes it to form uniform oil phase III slightly.Get PAA 1 gram, glycerine 4 grams and water 35.0 grams and mix, stir into a water IV, water IV is added to makes it to become uniform emulsion among the oil phase III while stirring, emulsion is homogenized through high pressure homogenizer, promptly get 50% Acetochlor aqueous emulsion.
Embodiment 3
Get alachlor weed killer herbicide 31 grams, phenethyl phenol polyethenoxy ether 5 grams, the 3 gram mixing of alkylphenol-polyethenoxy phosphate, heated and stirred makes it to form uniform oil phase V slightly.Get PAA 1 gram, glycerine 4 grams and water 55.42 grams and mix, stir into a water VI, water VI is added to makes it to become uniform emulsion among the oil phase V while stirring, emulsion is homogenized through high pressure homogenizer, promptly get 30% alachlor aqueous emulsion.
Embodiment 4
Get Acetochlor weed killer herbicide 10.5 gram, castor oil polyoxyethylene ether 7 grams, polyvinyl alcohol 2 grams and mix, heating slightly, stir and make it to form uniform oil phase g.Get carboxymethyl cellulose 1.5 grams, ethylene glycol 5 grams and water 73.97 grams and mix, stir into a water h, stir on the limit, the limit adds water h among the above-mentioned oil phase g that is made into, constantly stir and make it to become uniform emulsion, emulsion is homogenized through high pressure homogenizer, promptly get 10% aqueous emulsion finished product.
Embodiment 5
Get herbicide butachlor 53 grams, triphen ethyl phenol APEO 5 grams, the 3 gram mixing of alkylphenol-polyethenoxy phosphate, heated and stirred makes it to form uniform oil phase i slightly.Get PAA 1 gram, glycerine 4 grams and water 35.4 grams and mix, stir into a water j, water j is added to makes it to become uniform emulsion among the oil phase i while stirring, emulsion is homogenized through high pressure homogenizer, promptly get 50% butachlor aqueous emulsion.
Embodiment 6
Get isopropyl methoxalamine weed killer herbicide 45 gram, castor oil polyoxyethylene ether 3 grams, alkylphenol-polyethenoxy phosphate 3 grams, heating slightly, stir and make it to form uniform oil phase k.Get carboxymethyl cellulose 1.0 grams, ethylene glycol 5 grams and water 43.0 grams and mix, stir into a water l, stir on the limit, the limit adds water l among the above-mentioned oil phase k that is made into, constantly stir and make it to become uniform emulsion, emulsion is homogenized through high pressure homogenizer, promptly get 40% aqueous emulsion finished product.
Embodiment 7
Get Acetochlor weed killer herbicide 53 grams, alkyl phenol ethylene oxide condensate 6 grams, fatty alcohol-polyoxyethylene ether 4 gram mixing, heated and stirred makes it to form uniform oil phase m slightly, getting xanthans 0.1 gram, propane diols 6 grams and excess water mixes, stir into homogeneous water n, stir on the limit, and the limit adds uniform water n among the above-mentioned oil phase m that is made into, and constantly stirs and make it to become emulsion, emulsion is added to high pressure homogenizer homogenizes, promptly get 50% Acetochlor aqueous emulsion.
Wherein embodiment 7 is carried out the rape field and the soybean field weeding test of pesticide effectiveness, the results are shown in Table 1, table 2, table 3.
Drug effect result shows: use rape Tanaka, the Acetochlor aqueous emulsion has special efficacy to grassy weed, and each strain, fresh weight preventive effect of handling reaches 97.8-100% and 99-100% respectively; The Acetochlor aqueous emulsion has preventive effect preferably to broad leaved weed, and integrated control effect is more than 74%, and the fresh weight preventive effect is more than 92%; Rape there is certain synergistic effect.Use soybean Tanaka, the Acetochlor aqueous emulsion is active high, kills careless wide spectrum, and preventive effect is good.The monocotyledon weed preventive effect is higher than broadleaf weed, and mother uses 50ML, and after 45 days, preventive effect is still more than 90%.
Test preventive effect application form is eliminated in table 1 rape field
Handle numbering Handle (ml/ mu) Grass family Broad leaved weeds
Strain/chi 2 Preventive effect (%) Fresh weight gram/chi 2 Preventive effect (%) Herba Galii Teneri Chickweed Shepherd's purse Comprehensive strain preventive effect Comprehensive fresh weight preventive effect
Strain/chi 2 Preventive effect (%) Strain/chi 2 Preventive effect (%) Strain/chi 2 Preventive effect (%) Strain/chi 2 Preventive effect (%) Fresh weight gram/chi 2 Preventive effect (%)
1 50% Acetochlor EW50ml 1.0 97.8 0.1 99 4.0 63.6 5 52.4 0 100 9.0 74 0.57 92.5
2 50% Acetochlor EW750ml 0 100 0 100 3.0 72.7 5 52.4 0 100 8.0 77 0.28 96.3
3 Artificial weeding ck1 9 80 0.1 90.1 3 72.7 3 71.43 1 85.71 18 48 2.33 69.4
4 Not weeding ck2 45 1.0 11 10.5 7 84.5 7.6
Table 2 yield of rape structure investigation table
Handle (ml (g)/mu) Density (ten thousand strain/mu) Plant height (cm) Plant height increases (S) Every strain pod number Seeds per pod Thousand kernel weight (gram) Folding mu per unit area yield (jin/mu) Rate of growth (%)
50 Acetochlor EW50ml 1.4 147 0 180 22.4 3.2 361 7.2
50% acetochlor ec 50ml 1.4 147 0 178 22.5 3.2 359 6.5
Artificial weeding ck1 1.4 148 0.68 175 22.6 3.2 354 5.2
Not weeding ck2 1.4 147 168 22.4 3.2 337
Annotate: spacing in the rows 0.55 chi, line-spacing 0.7 chi, the investigation date is: May 15 2001
The different dosages of table 3 are to the soybean weeds preventive effect
7 days strain preventive effects behind the medicine 15 days strain preventive effects behind the medicine 45 days fresh weight preventive effects behind the medicine
Unifacial leaf Dicotyledonous Total preventive effect (%) Unifacial leaf Dicotyledonous Total preventive effect (%)
(the strain/rice of strain number 2 Preventive effect (%) (the strain/rice of strain number 2 Preventive effect (%) (the strain/rice of strain number 2) Preventive effect (%) (the strain/rice of strain number 2 Preventive effect (%) Fresh weight (gram/rice 2 Preventive effect (%)
50% Acetochlor EW50ml 7.9 95.0 1.7 92.7 94.1 9.2 98.0 16.11 96.0 98.0 163.3 95.9
50% Acetochlor EW100ml 3.5 97.8 3.7 84.1 95.7 4.1 99.1 7.0 97.8 93.6 71.7 98.2
50% Acetochlor EW150ml 2.7 98.3 2.3 90.1 92.1 4.1 99.1 4.1 98.8 98.8 47.8 93.8
50% Acetochlor EW200ml 1.4 99.1 1.9 91.8 98.1 3.8 99.2 4.0 98.7 98.4 36.2 99.0
50% Acetochlor EW250ml 0.8 94.4 0.7 96.9 99.1 3.1 99.3 3.1 99.0 98.8 19.3 99.2
Artificial weeding 132.0 20.1 430.2 296 190.4
ck 157.0 23.3 460.3 319 3983.3

Claims (4)

1, a kind of amide-type herbiciding aqueous emulsion is characterized in that it by structural formula is
Figure C021381070002C1
The former medicine of acetamide-group herbicides, emulsifier, antifreeze and water make through mix stirring, the percentage by weight of its each composition consists of:
Structural formula is the former medicine 10-60% of the acetamide-group herbicides of (1)
Emulsifier 2-10%
Antifreeze 2-10%
Water is supplied surplus;
Wherein, structural formula is the R in the former medicine of acetamide-group herbicides of (1) 1, R 2Choose CH 3, C 2H 5, R 3Choose CH 2OCH 3, CH 2OC 2H 5, CH 2OC 3H 7, (CH 3) CHCH 2OCH 3, CH 2OC 4H 9The alkyl ether group; Emulsifier is selected alkyl phenol ethylene oxide condensate, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene, fatty acid and ethylene oxide condensate, sodium alkyl benzene sulfonate, phenethyl phenol polyethenoxy ether for use, they or use separately, or mix and use; Antifreeze is selected ethylene glycol, propane diols, urea, glycerine, isopropyl alcohol for use, they or use separately, or mix and use.
2, a kind of production method of amide-type herbiciding aqueous emulsion, it is characterized in that earlier former medicine of the acetamide-group herbicides in claim 1 component and emulsifier evenly being made oil phase, again the antifreeze in the component and water are mixed and make water, while stirring water is added oil phase and make emulsion, after homogenizer homogenizes, promptly get stable amide-type herbiciding aqueous emulsion product of the present invention again.
3, press the production method of the described amide-type herbiciding aqueous emulsion of claim 2, it is characterized in that in oil phase, optionally adding following dispersant: sorbitan monooleate APEO, polyoxyethylene sorbitol liver monostearate APEO, polyoxyethylene sorbitol liver monostearate, phenethyl phenol polyethenoxy ether phenylsulfate, polyvinyl alcohol, fatty alcohol-polyoxyethylene ether, consumption is 1-8%, they or use separately, or mix and use.
4, press the production method of the described amide-type herbiciding aqueous emulsion of claim 2, it is characterized in that selecting to add following thickener: polyacrylate, Magnesiumaluminumsilicate, carboxymethyl cellulose, xanthans, PAA at aqueous phase, consumption is 0.2-3%, they or use separately, or mix and use.
CN 02138107 2002-08-14 2002-08-14 Amide-type herbiciding aqueous emulsion and its preparing process Expired - Fee Related CN1224318C (en)

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CN102187864A (en) * 2010-11-19 2011-09-21 南通联农农药制剂研究开发有限公司 Pretilachlor aqueous emulsion and preparation method thereof
CN112889824B (en) * 2021-01-22 2022-05-24 济南天邦化工有限公司 Self-emulsifying aqueous emulsion containing acetochlor

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Address after: 210036 screw Bridge No. 80, Jiangsu, Nanjing

Co-patentee after: Jiangsu Lulilai Co., Ltd.

Patentee after: Jiangsu Prov. Inst. of Agricultural Chemicals

Address before: 210036 screw Bridge No. 80, Jiangsu, Nanjing

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Granted publication date: 20051026

Termination date: 20190814