CN103461328B - Isopropyl methoxalamine microcapsule suspending agent and its preparation method and application - Google Patents
Isopropyl methoxalamine microcapsule suspending agent and its preparation method and application Download PDFInfo
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- CN103461328B CN103461328B CN201310373632.8A CN201310373632A CN103461328B CN 103461328 B CN103461328 B CN 103461328B CN 201310373632 A CN201310373632 A CN 201310373632A CN 103461328 B CN103461328 B CN 103461328B
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- China
- Prior art keywords
- suspending agent
- active component
- microcapsule suspending
- weight
- isopropyl methoxalamine
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- 239000000375 suspending agent Substances 0.000 title claims abstract description 66
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- 238000004090 dissolution Methods 0.000 description 1
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- 230000000857 drug effect Effects 0.000 description 1
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- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 229940075507 glyceryl monostearate Drugs 0.000 description 1
- 229960002163 hydrogen peroxide Drugs 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000036244 malformation Effects 0.000 description 1
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 229940049964 oleate Drugs 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
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- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000004302 potassium sorbate Substances 0.000 description 1
- 235000010241 potassium sorbate Nutrition 0.000 description 1
- 229940069338 potassium sorbate Drugs 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
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- 229960003415 propylparaben Drugs 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000017454 sodium diacetate Nutrition 0.000 description 1
- 239000001540 sodium lactate Substances 0.000 description 1
- 235000011088 sodium lactate Nutrition 0.000 description 1
- 229940005581 sodium lactate Drugs 0.000 description 1
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Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to a kind of isopropyl methoxalamine microcapsule suspending agent, it is characterized in that, described microcapsule suspending agent contains active component and high molecular polymer, and described high molecular polymer is with active component described in the wrapped of cyst wall, wherein, described active component contains isopropyl methoxalamine.Additionally provide the preparation method of isopropyl methoxalamine microcapsule suspending agent and the isopropyl methoxalamine microcapsule suspending agent of preparation thereof, and the application of isopropyl methoxalamine microcapsule suspending agent in controlling weeds.Isopropyl methoxalamine microcapsule suspending agent activity of weeding of the present invention is high, the lasting period is long, greatly can improve preventive effect; Crop safety is good, and environmental pollution is little; Multiple weeds can be prevented and treated, there is broad spectrum activity; Be applicable to various crop; Raw material is easy to get, and preparation method is simple, has very high economic worth.
Description
Technical field
The present invention relates to a kind of microcapsule suspending agent and its preparation method and application, particularly, relate to a kind of isopropyl methoxalamine microcapsule suspending agent, the preparation method of isopropyl methoxalamine microcapsule suspending agent and an isopropyl methoxalamine microcapsule suspending agent for preparation thereof, and the application of isopropyl methoxalamine microcapsule suspending agent in controlling weeds.
Background technology
Weeds are plants that people unintentionally know cultivation, and it directly and crop strives fertilizer, strives water, the photograph that wins honour for, strive soil, has a strong impact on the yield and quality of crop.Some weeds or the vector of damage by disease and insect, be conducive to spreading and propagation of damage by disease and insect.According to statistics, when not using weed killer herbicide because of the average underproduction rate of Weed infestation, as paddy rice can reach 41%, corn can reach 17%, and soybean can reach 40%, and cotton can reach 64%, and peanut can reach 80%, and potato can reach 9%.People, in order to struggle with weeds, will pay huge human and material resources every year.Artificial weeding efficiency is low, and labour intensity is large; Weeding by machine not thoroughly and hinder seedling, and chemical weed control is efficient, thoroughly, saving of labor, volume increase, be increase substantially labor productivity to realize the modern important technique measure of agricultural machinery.
In agricultural production practice, weed killer herbicide closed soil treatment is one of main method of current land for growing field crops and Protectorate cultivation chemical weed control.Weed killer herbicide closed soil treatment mainly selects (position of namely stagger medicine layer and crop seed or Root Distribution) and time difference selection (time that the pesticide-clay mixture drug effect that namely staggers works and the time that crop sprout is emerged) to reach the object (Jiang Rongchang that weed eradication keeps a full stand of seedings by potential difference, weed killer herbicide closed soil treatment technology, " Jiangsu's agriculture science ", 03 phase in 1985,20-21 page).
In China, common annual weed has kind more than 170, and the serious weeds that harm the crops mainly contain: barnyard grass, lady's-grass, moleplant seed, green foxtail, eleusine indica, annual bluegrass, Siberian cocklebur, lamb's-quarters, knotweed, amaranth, acalypha copperleaf, piemarker, kitchen garden, cyperus iria and difformed galingale herb etc.Because weed species is various, vitality is indomitable; usually there is the problem of dissimilar weeds mixed growth; barnyard grass, moleplant seed, eleusine indica, green foxtail, amur foxtail, annual bluegrass, kitchen garden, acalypha copperleaf, amaranth, lamb's-quarters, Veronica, knotweed are the weeds often existing simultaneously or in succession exist, such as, in the fields, land for growing field crops such as paddy field, corn field, Soybean Field, Peanut Fields, potato fields, Cotton Fields, sugarcane field, watermelon field or in the Protectorate cultivation such as capsicum, tomato, wild cabbage.
In order to prevent and treat the weeds often existing or in succession exist simultaneously, develop the weed killer herbicide of some broad spectrum activities, such as isopropyl methoxalamine missible oil, acetochlor ec, pendimethalin missible oil, these weed killer herbicides can prevent and treat some or all in the above-mentioned weeds often simultaneously existed or in succession exist.
But the control efficiency of existing broad spectrum weeding agent is poor, and the lasting period is short, and containing a large amount of organic solvents in weed killer herbicide, have considerable influence to crop growth, safety is low.
Summary of the invention
The object of the invention is the defect that broad spectrum weeding agent control efficiency is poor, the lasting period is short and safety is low overcoming prior art, there is provided that activity of weeding is high, the lasting period is long, crop safety is good, broad spectrum activity acetamide-group herbicides isopropyl methoxalamine microcapsule suspending agent being applicable to various crop and its preparation method and application.
The present inventor surprisingly finds under study for action, when microcapsule suspending agent contains active component and high molecular polymer, described high molecular polymer is with active component described in the wrapped of cyst wall, wherein, when described active component contains isopropyl methoxalamine, the activity of weeding of microcapsule suspending agent is high, the lasting period is long, and crop safety is good, be applicable to various crop, and there is broad spectrum activity.
Therefore, to achieve these goals, on the one hand, the invention provides a kind of isopropyl methoxalamine microcapsule suspending agent, it is characterized in that, described microcapsule suspending agent contains active component and high molecular polymer, and described high molecular polymer is with active component described in the wrapped of cyst wall, wherein, described active component contains isopropyl methoxalamine.
The weight ratio of described active component and described high molecular polymer is preferably 1:0.01-100, is more preferably 1:0.05-30; Further be preferably 1:0.1-5, described active component contains the isopropyl methoxalamine of 0.1-80 % by weight.
Preferably, described high molecular polymer is selected from one or more in poly-hexylamine lactone, sodium carboxymethylcellulose, ethyl cellulose, hydroxyethylcellulose, poly-allyl acetate, polyvinyl alcohol and aldehyde resin.
On the other hand, the invention provides a kind of preparation method of isopropyl methoxalamine microcapsule suspending agent, the method comprises:
(1) active component and high molecular polymer are dissolved in solvent, form oil mixture;
(2) described oil mixture is contacted with the aqueous solution of emulsifier, form O/w emulsion;
(3) O/w emulsion is made to leave standstill 6-20 hour at 30 DEG C-80 DEG C;
Wherein, described active component contains isopropyl methoxalamine.
The weight ratio of described active component and described high molecular polymer is preferably 1:0.01-100, is more preferably 1:0.05-30; Further be preferably 1:0.1-5, described active component contains the isopropyl methoxalamine of 0.1-80 % by weight.
Preferably, described high molecular polymer is selected from one or more in poly-hexylamine lactone, sodium carboxymethylcellulose, ethyl cellulose, hydroxyethylcellulose, poly-allyl acetate, polyvinyl alcohol and aldehyde resin.
Preferably, the weight ratio of described active component, solvent and emulsifier is 1:0.01-10:0.01-5.
The third aspect, the invention provides isopropyl methoxalamine microcapsule suspending agent prepared by method as above.
Fourth aspect, the invention provides microcapsule suspending agent as above and is preventing and treating the application in one or more weeds in barnyard grass, moleplant seed, eleusine indica, green foxtail, amur foxtail, annual bluegrass, kitchen garden, acalypha copperleaf, amaranth, lamb's-quarters, Veronica and knotweed.
Isopropyl methoxalamine microcapsule suspending agent activity of weeding of the present invention is high, the lasting period is long, greatly can improve preventive effect; Crop safety is good, and environmental pollution is little; Multiple weeds can be prevented and treated, there is broad spectrum activity; Be applicable to various crop; Raw material is easy to get, and preparation method is simple, has very high economic worth.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of isopropyl methoxalamine microcapsule suspending agent, this microcapsule suspending agent contains active component and high molecular polymer, and high molecular polymer is with the wrapped active component of cyst wall, and active component contains isopropyl methoxalamine.
According to the present invention, although microcapsule suspending agent contains active component and high molecular polymer, high molecular polymer is with the wrapped active component of cyst wall, and active component contains isopropyl methoxalamine, can realize object of the present invention, namely the activity of weeding of microcapsule suspending agent is high, the lasting period is long; Crop safety is good; Broad weed-killing spectrum; Be applicable to various crop.But under preferable case, the weight ratio of active component and high molecular polymer is 1:0.01-100, be preferably 1:0.05-30; Be more preferably 1:0.1-5, active component contains the isopropyl methoxalamine of 0.1-80 % by weight, can further improve the activity of weeding of microcapsule suspending agent, thus improves control efficiency further.
In the present invention, the chemical name of isopropyl methoxalamine is N-(2-ethyl-6 aminomethyl phenyl)-N-(1-methyl-2 methoxy ethyl)-chloroacetamide, and CAS accession number is [51218-45-2].
In the present invention, based on the gross weight of microcapsule suspending agent, the content of active component is 0.1-80 % by weight.
In the present invention, high molecular polymer be preferably selected from poly-hexylamine lactone, sodium carboxymethylcellulose, ethyl cellulose, hydroxyethylcellulose, poly-allyl acetate, polyvinyl alcohol and aldehyde resin one or more.The number-average molecular weight of poly-hexylamine lactone is preferably 3500-4000, the number-average molecular weight of sodium carboxymethylcellulose is preferably 10000-12000, the number-average molecular weight of ethyl cellulose is preferably 25000-30000, the number-average molecular weight of hydroxyethylcellulose is preferably 30000-40000, the number-average molecular weight of poly-allyl acetate is preferably 38000-43000, the number-average molecular weight of polyvinyl alcohol is preferably 75000-80000, and the number-average molecular weight of aldehyde resin is preferably 30000-40000.
In the present invention, microcapsule suspending agent is also containing solvent and emulsifier, and the weight ratio of active component, solvent and emulsifier is preferably 1:0.01-10:0.01-5.
For solvent and emulsifier all without particular/special requirement, the material that this area is conventional can be selected, such as:
Solvent can be selected from toluene, dimethylbenzene, ethyl acetate, aromatic solvent naphtha, mineral oil, methylated vegetable oil, cyclohexanone, benzinum and carrene one or more.
Emulsifier can be selected from calcium dodecyl benzene sulfonate, succinate sodium sulfonate, styryl phenol polyethenoxy ether phosphate, Ben-zylphenol Polyoxyethyl Ether phosphate, sorbitan trioleate, anhydrous sorbitol tristearate, polyoxyethylene ether alcohol six stearate, cithrol, polyoxyethylene sorbitol ether beeswax derivatives, polyethylene glycol mono stearate, sorbitan sesquioleate, glyceryl monostearate, sorbitan monooleate, sorbitan monostearate, dibenzyl phenol polyethenoxy ether, diethylene glycol fatty acid ester, diethylene glycol monolaurate, sorbitan mono-laurate, Brij30, polyoxyethylene monopalmitate, alkylphenol polyoxyethylene, Brij30, anhydrous sorbitol APEO, polyoxyethylene sorbitan ether monoleate, styryl phenol polyethenoxy ether, fatty alcohol-polyoxyethylene ether, one or more in aliphatic amine polyoxyethylene ether and castor oil polyoxyethylene ether.
In the present invention, microcapsule suspending agent can also contain the usual component such as dispersant and wetting agent, thickener, preservative, antifreezing agent, defoamer.
When containing mentioned component, the content of each composition is without particular/special requirement, the consumption of this area routine can be selected, such as, based on the gross weight of microcapsule suspending agent, the content of dispersant and wetting agent can be 0.1-10 % by weight, the content of thickener can be 0.1-20 % by weight, the content of preservative can be 0.1-0.5 % by weight, and the content of antifreezing agent can be 0.1-10 % by weight, and the content of defoamer can be 0.5-1.5 % by weight.
In the present invention, for the concrete material of mentioned component all without particular/special requirement, the material that this area is conventional can be adopted, such as:
Dispersant and wetting agent can be selected from polyvinylpyrrolidone, sodium methylene bis-naphthalene sulfonate, sodium lignin sulfonate, calcium lignosulfonate, calcium dodecyl benzene sulfonate, succinate sodium sulfonate, pull open in powder and sldium lauryl sulfate one or more.
Thickener can be selected from Magnesiumaluminumsilicate, xanthans, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose and phenolic resins one or more.
Preservative can be selected from Sodium Benzoate, benzoic acid, potassium sorbate, dehydro sodium acetate, calcium propionate, sodium Diacetate, sodium lactate, hydrogen peroxide, propylparaben one or more.
Antifreezing agent can be selected from ethylene glycol, glycerine, propane diols, sodium chloride, urea and polyethylene glycol one or more.
Defoamer can be selected from dimethicone, isooctanol, soybean oil, rapeseed oil, glycerine trihydroxy polyethers, benzyl carbinol oleate and benzyl carbinol laurate one or more.
On the other hand, the invention provides a kind of preparation method of isopropyl methoxalamine microcapsule suspending agent, the method comprises:
(1) active component and high molecular polymer are dissolved in solvent, form oil mixture;
(2) described oil mixture is contacted with the aqueous solution of emulsifier, form O/w emulsion;
(3) O/w emulsion is made to leave standstill 6-20 hour at 30 DEG C-80 DEG C;
Wherein, described active component contains isopropyl methoxalamine.
In step of the present invention (1), for concrete grammar active component and high molecular polymer are dissolved in solvent without particular/special requirement, the various methods that this area is conventional can be adopted.Such as, first by solubilize active ingredients in a solvent, and then high molecular polymer can be added, can by being stirred to dissolve evenly fast in course of dissolution.
In the present invention, the weight ratio of active component and high molecular polymer is preferably 1:0.01-100, is more preferably 1:0.05-30; Further be preferably 1:0.1-5, active component contains the isopropyl methoxalamine of 0.1-80 % by weight, can further improve the activity of weeding of microcapsule suspending agent, thus improves control efficiency further.
In the present invention, the mode contacted with the aqueous solution of emulsifier for oil mixture is without particular/special requirement, as long as can O/w emulsion be formed, contact more fully to form O/w emulsion with the aqueous solution of emulsifier to enable oil mixture, oil mixture slowly can be added in the aqueous solution of emulsifier, such as dropwise add, stir while adding, add rear continuation completely and stir 25-35 minute.
In the present invention, the weight ratio of active component, solvent and emulsifier is preferably 1:0.01-10:0.01-5.
In the present invention, O/w emulsion leaves standstill 6-20 hour at 30 DEG C-80 DEG C, and namely cyst material solidifies encystation.After leaving standstill, can also add in dispersant and wetting agent, thickener, preservative, antifreezing agent, defoamer one or more, stir.
In the present invention, water is preferably deionized water or distilled water.
In the present invention, for the addition sequence of dispersant and wetting agent, thickener, preservative, antifreezing agent and defoamer without particular/special requirement, adopt any order, on the character of microcapsule suspending agent of the present invention all without impact.
In the present invention, for the concrete material used such as high molecular polymer, solvent, emulsifier, dispersant and wetting agent, thickener, preservative, antifreezing agent, defoamer, each material consumption as previously mentioned, do not repeat them here.
The third aspect, the invention provides isopropyl methoxalamine microcapsule suspending agent prepared by method as above.
Fourth aspect, the invention provides microcapsule suspending agent as above and is preventing and treating the application in one or more weeds in barnyard grass, moleplant seed, eleusine indica, green foxtail, amur foxtail, annual bluegrass, kitchen garden, acalypha copperleaf, amaranth, lamb's-quarters, Veronica and knotweed.
Namely microcapsule suspending agent of the present invention may be used in field, land for growing field crops; such as; paddy field, corn field, Soybean Field, Peanut Fields, potato fields, Cotton Fields, sugarcane field, watermelon field etc., also may be used in Protectorate cultivation, such as, in the Protectorate cultivation of capsicum, tomato, wild cabbage etc.
It will be understood by those skilled in the art that microcapsule suspending agent of the present invention can dilute use according to actual needs when reality uses.
Embodiment
Embodiment 1
(1) 48 grams of former medicines of isopropyl methoxalamine (calculating with pure isopropyl methoxalamine) are dissolved in 5 grams of ethyl acetate, then add 4.8 grams of polyvinyl alcohol (number-average molecular weight 80000) and stir, form oil mixture;
(2) oil mixture of step (1) is dropped to 31.4 grams containing 6gAEO-9(fatty alcohol-polyoxyethylene ether, be purchased from Nanning City and gallop Chemical Co., Ltd.) the aqueous solution in, dropping limit, limit is stirred, and drips completely, continue stirring 30 minutes, form O/w emulsion;
(3) by O/w emulsion at 70 DEG C, leave standstill 6 hours;
(4) add sodium lignin sulfonate 5 grams, xanthans 0.2 gram, Sodium Benzoate 0.1 gram, ethylene glycol 5 grams, dimethicone 0.5 gram, stirs, i.e. the isopropyl methoxalamine microcapsule suspending agent of obtained 48 % by weight.
In microcapsule suspending agent, each component content is: isopropyl methoxalamine 48 % by weight, ethyl acetate 5 % by weight, polyvinyl alcohol is 4.8 % by weight, fatty alcohol-polyoxyethylene ether 6 % by weight, sodium lignin sulfonate 5 % by weight, xanthans 0.2 % by weight, Sodium Benzoate 0.1 % by weight, ethylene glycol 5 % by weight, dimethicone 0.5 % by weight, deionized water 25.4 % by weight.
Embodiment 2
(1) 24 grams of former medicines of isopropyl methoxalamine (calculating with pure isopropyl methoxalamine) are dissolved in 10 grams of dimethylbenzene, then add 15 grams of poly-allyl acetates (number-average molecular weight 40000) and stir, form oil mixture;
(2) oil mixture of step (1) is dropped to 41.2 grams containing in the aqueous solution of 9g sorbitan monooleate, dropping limit, limit is stirred, and drips completely, continues stirring 35 minutes, form O/w emulsion;
(3) by O/w emulsion at 50 DEG C, static 12 hours;
(4) add sodium methylene bis-naphthalene sulfonate 4 grams, xanthans 0.2 gram, Sodium Benzoate 0.1 gram, propane diols 5 grams, dimethicone 0.5 gram, stirs, i.e. the isopropyl methoxalamine microcapsule suspending agent of obtained 24 % by weight.
In microcapsule suspending agent, each component content is: isopropyl methoxalamine 24 % by weight; Dimethylbenzene 10 % by weight; Poly-allyl acetate is 15 % by weight; Sorbitan monooleate 9 % by weight; Sodium methylene bis-naphthalene sulfonate 4 % by weight; Xanthans 0.2 % by weight; Sodium Benzoate 0.1 % by weight; Propane diols 5 % by weight; Dimethicone 0.5 % by weight; Deionized water 32.2 % by weight.
Embodiment 3
(1) 5 grams of former medicines of isopropyl methoxalamine (calculating with pure isopropyl methoxalamine) are dissolved in 4 grams of cyclohexanone, then add 25 grams of poly-hexylamine lactones (number-average molecular weight 3800) and stir, form oil mixture;
(2) dropped to by the oil mixture of step (1) in the aqueous solution of the styryl phenol polyethenoxy ether phosphate (number-average molecular weight 60000) containing 20g of 858 grams, dropping limit, limit is stirred, and drips completely, continues stirring 25 minutes, form O/w emulsion;
(3) by O/w emulsion at 30 DEG C, react 20 hours;
(4) add sldium lauryl sulfate 50 grams, Magnesiumaluminumsilicate 2 grams, Sodium Benzoate 1 gram, glycerine 50 grams, dimethicone 5 grams, stirs, i.e. the isopropyl methoxalamine microcapsule suspending agent of obtained 0.5 % by weight.
In microcapsule suspending agent, each component content is: isopropyl methoxalamine 0.5 % by weight, cyclohexanone 0.4 % by weight, poly-hexylamine lactone is 2.5 % by weight, styryl phenol polyethenoxy ether phosphate 2 % by weight, sldium lauryl sulfate 5 % by weight, Magnesiumaluminumsilicate 0.2 % by weight, Sodium Benzoate 0.1 % by weight, glycerine 5 % by weight, dimethicone 0.5 % by weight, deionized water 83.8 % by weight.
Embodiment 4
(1) 5 grams of former medicines of isopropyl methoxalamine (calculating with pure isopropyl methoxalamine) are dissolved in 4 grams of cyclohexanone, then add 0.25 gram of poly-hexylamine lactone (number-average molecular weight 3800) and stir, form oil mixture;
(2) oil mixture of step (1) is dropped to 882.75 grams containing 20g styryl phenol polyethenoxy ether phosphate (number-average molecular weight 60000) the aqueous solution in, dropping limit, limit is stirred, drip completely, continue stirring 25 minutes, form O/w emulsion;
(3) by O/w emulsion at 30 DEG C, react 20 hours;
(4) add sldium lauryl sulfate 50 grams, Magnesiumaluminumsilicate 2 grams, Sodium Benzoate 1 gram, glycerine 50 grams, dimethicone 5 grams, stirs, i.e. the isopropyl methoxalamine microcapsule suspending agent of obtained 0.5 % by weight.
In microcapsule suspending agent, each component content is: isopropyl methoxalamine 0.5 % by weight, cyclohexanone 0.4 % by weight, poly-hexylamine lactone is 0.025 % by weight, styryl phenol polyethenoxy ether phosphate 2 % by weight, sldium lauryl sulfate 5 % by weight, Magnesiumaluminumsilicate 0.2 % by weight, Sodium Benzoate 0.1 % by weight, glycerine 5 % by weight, dimethicone 0.5 % by weight, deionized water 86.275 % by weight.
Embodiment 5
(1) 5 grams of former medicines of isopropyl methoxalamine (calculating with pure isopropyl methoxalamine) are dissolved in 4 grams of cyclohexanone, then add 150 grams of poly-hexylamine lactones (number-average molecular weight 3800) and stir, form oil mixture;
(2) oil mixture of step (1) is dropped to 733 grams containing in the aqueous solution of 20g styryl phenol polyethenoxy ether phosphate (number-average molecular weight 60000), dropping limit, limit is stirred, and drips completely, continues stirring 25 minutes, form O/w emulsion;
(3) by O/w emulsion at 30 DEG C, react 20 hours;
(4) add sldium lauryl sulfate 50 grams, Magnesiumaluminumsilicate 2 grams, Sodium Benzoate 1 gram, glycerine 50 grams, dimethicone 5 grams, stirs, i.e. the isopropyl methoxalamine microcapsule suspending agent of obtained 0.5 % by weight.
In microcapsule suspending agent, each component content is: isopropyl methoxalamine 0.5 % by weight, cyclohexanone 0.4 % by weight, poly-hexylamine lactone is 15 % by weight, styryl phenol polyethenoxy ether phosphate 2 % by weight, sldium lauryl sulfate 5 % by weight, Magnesiumaluminumsilicate 0.2 % by weight, Sodium Benzoate 0.1 % by weight, glycerine 5 % by weight, dimethicone 0.5 % by weight, deionized water 71.3 % by weight.
Embodiment 6
(1) 5 grams of former medicines of isopropyl methoxalamine (calculating with pure isopropyl methoxalamine) are dissolved in 4 grams of cyclohexanone, then add 0.05 gram of poly-hexylamine lactone (number-average molecular weight 3800) and stir, form oil mixture;
(2) oil mixture of step (1) is dropped to 882.95 grams containing 20g styryl phenol polyethenoxy ether phosphate (number-average molecular weight 60000) the aqueous solution in, dropping limit, limit is stirred, drip completely, continue stirring 25 minutes, form O/w emulsion;
(3) by O/w emulsion at 30 DEG C, react 20 hours;
(4) add sldium lauryl sulfate 50 grams, Magnesiumaluminumsilicate 2 grams, Sodium Benzoate 1 gram, glycerine 50 grams, dimethicone 5 grams, stirs, i.e. the isopropyl methoxalamine microcapsule suspending agent of obtained 0.5 % by weight.
In microcapsule suspending agent, each component content is: isopropyl methoxalamine 0.5 % by weight, cyclohexanone 0.4 % by weight, poly-hexylamine lactone is 0.005 % by weight, styryl phenol polyethenoxy ether phosphate 2 % by weight, sldium lauryl sulfate 5 % by weight, Magnesiumaluminumsilicate 0.2 % by weight, Sodium Benzoate 0.1 % by weight, glycerine 5 % by weight, dimethicone 0.5 % by weight, deionized water 86.295 % by weight.
Embodiment 7
(1) 5 grams of former medicines of isopropyl methoxalamine (calculating with pure isopropyl methoxalamine) are dissolved in 4 grams of cyclohexanone, then add 500 grams of poly-hexylamine lactones (number-average molecular weight 3800) and stir, form oil mixture;
(2) oil mixture of step (1) is dropped to 383 grams containing in the aqueous solution of 20 grams of styryl phenol polyethenoxy ether phosphates (number-average molecular weight 60000), dropping limit, limit is stirred, and drips completely, continues stirring 25 minutes, form O/w emulsion;
(3) by O/w emulsion at 30 DEG C, react 20 hours;
(4) add sldium lauryl sulfate 50 grams, Magnesiumaluminumsilicate 2 grams, Sodium Benzoate 1 gram, glycerine 50 grams, dimethicone 5 grams, stirs, i.e. the isopropyl methoxalamine microcapsule suspending agent of obtained 0.5 % by weight.
In microcapsule suspending agent, each component content is: isopropyl methoxalamine 0.5 % by weight, cyclohexanone 0.4 % by weight, poly-hexylamine lactone is 50 % by weight, styryl phenol polyethenoxy ether phosphate 2 % by weight, sldium lauryl sulfate 5 % by weight, Magnesiumaluminumsilicate 0.2 % by weight, Sodium Benzoate 0.1 % by weight, glycerine 5 % by weight, dimethicone 0.5 % by weight, deionized water 36.3 % by weight.
Comparative example 1
720g/L isopropyl methoxalamine missible oil (being purchased from Syngenta Co., Ltd)
Comparative example 2
900g/L acetochlor ec (being purchased from Monsanto Company)
Comparative example 3
330g/L pendimethalin missible oil (being purchased from BASF AG)
Test example 1:
Experimental field be located in From Shijiazhuang City of Hebei Province Zhengding County one peasant household farmland covered by contract, area 0.8hm
2, soil is loam, slightly biased alkali, and the content of organic matter is medium, and preceding crop is wheat, does not use weed killer herbicide.Main weeds has green foxtail, lamb's-quarters, amaranth, acalypha copperleaf, amur foxtail.Experimental field managerial skills are consistent.
Respectively the medicament of embodiment 1-7 and comparative example 1-3 is carried out for 3 days after peanut seeding closed soil treatment namely broadcast after soil spraying before seedling, the mu consumption of often kind of medicament is as follows respectively:
Embodiment 1:150g/ mu
Embodiment 2:300g/ mu
Embodiment 3:14400g/ mu
Embodiment 4:14400g/ mu
Embodiment 5:14400g/ mu
Embodiment 6:14400g/ mu
Embodiment 7:14400g/ mu
Comparative example 1:100ml/ mu
Comparative example 2:80ml/ mu
Comparative example 3:150ml/ mu
Often kind of medicament uses after being all watered dilution, and with active ingredient, being diluted to active component content is 0.0002 % by weight, and establishes blank (blank spray equivalent clear water).Each process repetition 4 times, every plot area 20m
2, completely random district group arranges.Use bodyguard's board WS-16 knapsack hand sprayer, shower nozzle adopts 2 cone nozzles.Pressure 0.3MPa, flow 0.7-0.9L/min.
Weedy rices requires to carry out according to " agricultural field control effectiveness test criterion (two) weed killer herbicide control Weed in peanut field " (GB/T17980.126-2004).Random 3 samplings in every community, often some 0.25m
2, after medicine, the 7th, 15,35,45,60 day investigation weeds strain number, calculates control efficiency.Preventive effect computational methods:
Observe medicament to peanut with or without poisoning, record poisoning grade.Poisoning classification is as shown in table 1 below:
Table 1
| Poisoning classification | Plant state | Blade state |
| 0 | Plant height is normal | Blade is normal |
| Ⅰ | Plant height downgrades for normal plant height more than 3/4 | Blade 1/4 is withered and yellow |
| Ⅱ | Plant height downgrades the 2/3-3/4 for normal plant height | Blade mild malformation, 1/2 is withered and yellow |
| Ⅲ | Plant height downgrades the 1/2-2/3 for normal plant height | Blade severe deformities, 3/4 is withered and yellow |
| Ⅳ | Complete stool is dead | Blade more than 3/4 is withered and yellow to dead |
To peanut weedy rices time and preventive effect result of calculation in table 2.
Table 2
To the poisoning investigation result of peanut in table 3.
Table 3
| Poisoning grade | |
| Embodiment 1 | 0 |
| Embodiment 2 | 0 |
| Embodiment 3 | 0 |
| Embodiment 4 | 0 |
| Embodiment 5 | 0 |
| Embodiment 6 | 0 |
| Embodiment 7 | 0 |
| Comparative example 1 | Ⅰ |
| Comparative example 2 | 0 |
| Comparative example 3 | Ⅰ |
Test example 2:
Experimental field be selected in Qing County, Cangzhou, Hebei Province one peasant household farmland covered by contract and carry out, front stubble is Xiaoqinling Nature Reserve, does not use weed killer herbicide, sandy loam, in fertility.Main weeds is Veronica, kitchen garden, eleusine indica, barnyard grass.Experimental field managerial skills are consistent.
Closed soil treatment is carried out according to the method for test example 1, unlike, crop is corn.Preventive effect is calculated, statistics poisoning according to the method for test example 1.Preventive effect the results are shown in Table 4, and chemical injury of crops is in table 5.
Table 4
Table 5
| Poisoning grade | |
| Embodiment 1 | 0 |
| Embodiment 2 | 0 |
| Embodiment 3 | 0 |
| Embodiment 4 | 0 |
| Embodiment 5 | 0 |
| Embodiment 6 | 0 |
| Embodiment 7 | 0 |
| Comparative example 1 | Ⅰ |
| Comparative example 2 | Ⅰ |
| Comparative example 3 | 0 |
Test example 3:
Experimental field be selected in Jiaxiang County, Jining of Shandong Province city soybean Breeding base, soil types is sandy loam, middle fertility, and preceding crop is corn, does not use weed killer herbicide.Main weeds is moleplant seed, annual bluegrass, knotweed, green foxtail.
Closed soil treatment is carried out according to the method for test example 1, unlike, crop is soybean.Preventive effect is calculated, statistics poisoning according to the method for test example 1.Preventive effect the results are shown in Table 6, and chemical injury of crops is in table 7.
Table 6
Table 7
| Poisoning grade | |
| Embodiment 1 | 0 |
| Embodiment 2 | 0 |
| Embodiment 3 | 0 |
| Embodiment 4 | 0 |
| Embodiment 5 | 0 |
| Embodiment 6 | 0 |
| Embodiment 7 | 0 |
| Comparative example 1 | Ⅰ |
| Comparative example 2 | 0 |
| Comparative example 3 | Ⅰ |
As can be seen from table 2,4,6, the control efficiency of isopropyl methoxalamine microcapsule suspending agent of the present invention is obviously better than market medicament, and within 45 days and 60 days, still keeps higher preventive effect after spray medicine, and visible isopropyl methoxalamine microcapsule suspending agent lasting effect of the present invention is good; As can be seen from table 3,5,7, isopropyl methoxalamine microcapsule suspending agent of the present invention is light to the degree of injury of crop, substantially without poisoning.
Embodiment 1 is compared can be found out with embodiment 4 and 5, embodiment 6 and 7 respectively, and the weight ratio of isopropyl methoxalamine and high molecular polymer is 1:0.05-30, can further improve control efficiency; The weight ratio of isopropyl methoxalamine and high molecular polymer is 1:0.1-5, further can improve control efficiency.
Isopropyl methoxalamine microcapsule suspending agent activity of weeding of the present invention is high, the lasting period is long, greatly can improve preventive effect; Crop safety is good, and environmental pollution is little; Multiple weeds can be prevented and treated, there is broad spectrum activity; Be applicable to various crop; Raw material is easy to get, and preparation method is simple, has very high economic worth.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible combination.
In addition, also can be combined between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (8)
1. an isopropyl methoxalamine microcapsule suspending agent, is characterized in that, described microcapsule suspending agent contains active component and high molecular polymer, and described high molecular polymer is with active component described in the wrapped of cyst wall, and wherein, described active component is isopropyl methoxalamine;
Wherein, the weight ratio of described active component and described high molecular polymer is 1:0.01-100, and based on the gross weight of microcapsule suspending agent, the content of described active component is 0.1-80 % by weight;
Wherein, described high molecular polymer is selected from one or more in poly-hexylamine lactone, sodium carboxymethylcellulose, ethyl cellulose, hydroxyethylcellulose, poly-allyl acetate, polyvinyl alcohol and aldehyde resin;
Wherein, described microcapsule suspending agent is also containing solvent and emulsifier, and the weight ratio of described active component, solvent and emulsifier is 1:0.01-10:0.01-5.
2. microcapsule suspending agent according to claim 1, wherein, the weight ratio of described active component and described high molecular polymer is 1:0.05-30.
3. microcapsule suspending agent according to claim 2, wherein, the weight ratio of described active component and described high molecular polymer is 1:0.1-5.
4. a preparation method for isopropyl methoxalamine microcapsule suspending agent, the method comprises:
(1) active component and high molecular polymer are dissolved in solvent, form oil mixture;
(2) described oil mixture is contacted with the aqueous solution of emulsifier, form O/w emulsion;
(3) O/w emulsion is made to leave standstill 6-20 hour at 30 DEG C-80 DEG C;
Wherein, described active component is isopropyl methoxalamine;
Wherein, the weight ratio of described active component and described high molecular polymer is 1:0.01-100, and based on the gross weight of microcapsule suspending agent, the content of described active component is 0.1-80 % by weight;
Wherein, described high molecular polymer is selected from one or more in poly-hexylamine lactone, sodium carboxymethylcellulose, ethyl cellulose, hydroxyethylcellulose, poly-allyl acetate, polyvinyl alcohol and aldehyde resin;
Wherein, the weight ratio of described active component, solvent and emulsifier is 1:0.01-10:0.01-5.
5. method according to claim 4, wherein, the weight ratio of described active component and described high molecular polymer is 1:0.05-30.
6. method according to claim 5, wherein, the weight ratio of described active component and described high molecular polymer is 1:0.1-5.
7. isopropyl methoxalamine microcapsule suspending agent prepared by the method in claim 4-6 described in any one.
8. the isopropyl methoxalamine microcapsule suspending agent in claim 1-3 and 7 described in any one is preventing and treating the application in one or more weeds in barnyard grass, moleplant seed, eleusine indica, green foxtail, amur foxtail, annual bluegrass, kitchen garden, acalypha copperleaf, amaranth, lamb's-quarters, Veronica and knotweed.
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| CN105557748B (en) * | 2015-12-30 | 2018-06-05 | 北京明德立达农业科技有限公司 | A kind of herbicidal composition and application thereof |
| CN105557747A (en) * | 2016-02-02 | 2016-05-11 | 南京高正农用化工有限公司 | Stable pesticide microcapsule suspending agent |
| CN106538551A (en) * | 2016-10-25 | 2017-03-29 | 北京明德立达农业科技有限公司 | A kind of microcapsule suspension suspending agent of S-metolachlor and oxadiargyl and preparation method thereof |
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