CN107751228A - A kind of chlorimuronethyl herbicide of silica absorption and preparation method thereof - Google Patents
A kind of chlorimuronethyl herbicide of silica absorption and preparation method thereof Download PDFInfo
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- CN107751228A CN107751228A CN201710906786.7A CN201710906786A CN107751228A CN 107751228 A CN107751228 A CN 107751228A CN 201710906786 A CN201710906786 A CN 201710906786A CN 107751228 A CN107751228 A CN 107751228A
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- China
- Prior art keywords
- chlorimuronethyl
- herbicide
- silica
- preparation
- sodium hydroxide
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses chlorimuronethyl herbicide of a kind of silica absorption and preparation method thereof, it is characterised in that is made up of the raw material of following parts by weight：Silica 38, soybean oil 30 40, sodium hydroxide 15 20, methanol 100 200, DTAB 23, appropriate calcium chloride, polyoxyethylene nonylphenol ether 10 48, Tween 80 48, chlorimuronethyl 10 20, hydroxypropyl beta cyclodextrin 40 50, distilled water 200 500, appropriate warm water.The present invention carries out assistance synergy with esterification soybean oil to herbicide, the surface tension of spray solution, plays an important role in links such as droplet dispersion, adhesion, spread, deposition, infiltration, conduction and promotes herbicide to play higher activity when can significantly reduce later stage application；The silica and cationic surfactant for coordinating addition can adsorb chlorimuronethyl, strengthen its stability.
Description
Technical field
The present invention relates to a kind of herbicide, more particularly to a kind of chlorimuronethyl herbicide of esterification soybean oil synergy and its
Preparation method.
Background technology
At present, agricultural chemicals is following 4 points in subject matter present on use：（1）Dissolubility is poor.The agricultural chemicals of chemical synthesis is former
Medicine is all organic compound, and only part active compound can be dissolved in water and directly use, and most active compounds are all to be insoluble in dredging for water
It aqueous compounds, can not effectively be dissolved in water, active compound addition auxiliary agent or organic solvent etc. are often processed into missible oil, pulvis etc.
Pesticidal preparations are used；（2）Stability is poor.Because organic agricultural chemicals molecular characterization shows as easily waving under natural environment
Hair, photodissociation, hydrolysis etc., reduce active ingredient, are commonly incorporated into the auxiliary agents such as stabilizer；（3）Adsorption by soil, effective rate of utilization is low, production
Raw residues of pesticides.Hydrophobic pesticidal causes it to be lost in soil or leaching loss, not only reduced easily by soil colloid granular absorption
The effective rate of utilization of agricultural chemicals, and make degraded transmission of the agricultural chemicals in soil difficult, easily cause accumulation and the residual of agricultural chemicals；（4）
Environmental pollution is serious.It is often excessive in actual production operation in order to ensure the drug effect of agricultural chemicals because the effective rate of utilization of agricultural chemicals is low
Use, cause environment pollution.
Hydroxypropyl-β-cyclodextrin is to be distinguished by hydroxypropyl in Chagerdβcyclodextrins 6 and 2,3-OH on glucose molecule
On H atom and the derivative of beta-schardinger dextrin that is formed.Compared with parent P-cyclodextrin, hydroxypropyl-β-cyclodextrin both maintained
The inclusion characteristic of the hydrophobic cavity of parent, and due to adding hydroxypropyl outside the cavity of parent, substantially increase its water
Dissolubility, expand its application.The water solubility of hydroxypropyl-β-cyclodextrin is very high, and the solubility in water is up to 750 at room temperature
G/L, the solubilization to medicine are far longer than beta-schardinger dextrin, the solubility that can solve some insoluble drugs.
Zhang Jinyan is in its Ph.D. Dissertation《Cyclodextrin is to the including of herbicide, the research of solubilising and activity of weeding》In,
Herbicide is included with cyclodextrin, and have studied its performance, but the phase is also low, viscous there is droplet dispersion degree after application
The problems such as property is small.
The content of the invention
Think deeply based on more than, the present invention is intended to provide the herbicide that a kind of droplet dispersion is uniform, adherence is good, and its prepare
Method.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of chlorimuronethyl herbicide of silica absorption, it is characterised in that be made up of the raw material of following parts by weight：
Silica 3-8, soybean oil 30-40, sodium hydroxide 15-20, methanol 100-200, DTAB 2-
3, appropriate calcium chloride, emulsifier op-10 4-8, Tween 80 4-8, chlorimuronethyl 10-20, hydroxypropyl-β-cyclodextrin 40-50, steam
Distilled water 200-500, appropriate warm water.
The preparation method of the chlorimuronethyl herbicide of described a kind of silica absorption, it is characterised in that be by following
Step is made：
A. after soybean oil being warming up into 60-70 DEG C, the methanol solution of sodium hydroxide is added, reacts 40-80min under stirring condition,
Excessive methanol is distilled off after end, cools down, stands reactant mixture, removes oil reservoir, washs methyl esters layer with warm water, then use chlorine
Change calcium to dry；
B. 50-70 parts distilled water, emulsifier op-10, Tween 80 and the phonetic sulphur of chlorine are added into esterification soybean oil obtained by step a
It is grand, 20-30min is stirred, forms homogeneous missible oil solution；
C. silica, DTAB are added in step b resulting solutions, 10-30min are stirred by ultrasonic,
Place 5-10h；
D. hydroxypropyl-β-cyclodextrin is dissolved in 80-150 part distilled water, magnetic agitation 10-30min, at room temperature by step c institutes
Obtain solution to be added slowly thereto, continue magnetic agitation 10-15h after dripping, reaction solution rotary evaporation concentrates, filtering, vacuum
4h is dried, obtains white powder.
A kind of preparation method of the chlorimuronethyl herbicide of described silica absorption, it is characterised in that sodium hydroxide
The preparation method of methanol solution be：Sodium hydroxide is dissolved in methanol solution under agitation.
The beneficial effects of the invention are as follows：Assistance synergy is carried out to herbicide with esterification soybean oil, the later stage can be significantly reduced
Using when spray solution surface tension, played an important role in links such as droplet dispersion, adhesion, spread, deposition, infiltration, conduction
And herbicide is promoted to play higher activity；The herbicide after synergy is included with hydroxypropyl-β-cyclodextrin, due to hydroxypropyl
The hydrophily of hydroxypropyl existing for group-beta-cyclodextrin surface, the water solubility and bioavilability of hydrophobic molecule are substantially increased,
Its big application；Emulsifier op-10 and Tween 80 are used in mixed way with one to one ratio, overcome single emulsifier breast
Change the problem of ineffective, contribute to the fusion of esterification soybean oil and chlorimuronethyl, form homogeneous missible oil；Coordinate addition
Silica and cationic surfactant can adsorb chlorimuronethyl, strengthen its stability.
Embodiment
The embodiment of the present invention is further described with reference to embodiment.
Embodiment
A kind of chlorimuronethyl herbicide of silica absorption, it is characterised in that be made up of the raw material of following parts by weight：
Silica 8, soybean oil 40, sodium hydroxide 20, methanol 200, DTAB 3, appropriate calcium chloride, breast
Agent OP-10 8, Tween 80 8, chlorimuronethyl 20, hydroxypropyl-β-cyclodextrin 50, distilled water 500, appropriate warm water.
The preparation method of the chlorimuronethyl herbicide of described a kind of silica absorption, it is characterised in that be by following
Step is made：
A. after soybean oil being warming up into 60-70 DEG C, the methanol solution of sodium hydroxide is added, reacts 40-80min under stirring condition,
Excessive methanol is distilled off after end, cools down, stands reactant mixture, removes oil reservoir, washs methyl esters layer with warm water, then use chlorine
Change calcium to dry；
B. 50-70 parts distilled water, emulsifier op-10, Tween 80 and the phonetic sulphur of chlorine are added into esterification soybean oil obtained by step a
It is grand, 20-30min is stirred, forms homogeneous missible oil solution；
C. silica, DTAB are added in step b resulting solutions, 10-30min are stirred by ultrasonic,
Place 5-10h；
D. hydroxypropyl-β-cyclodextrin is dissolved in 80-150 part distilled water, magnetic agitation 10-30min, at room temperature by step c institutes
Obtain solution to be added slowly thereto, continue magnetic agitation 10-15h after dripping, reaction solution rotary evaporation concentrates, filtering, vacuum
4h is dried, obtains white powder.
A kind of preparation method of the chlorimuronethyl herbicide of described silica absorption, it is characterised in that sodium hydroxide
The preparation method of methanol solution be：Sodium hydroxide is dissolved in methanol solution under agitation.
Claims (3)
1. a kind of chlorimuronethyl herbicide of silica absorption, it is characterised in that be made up of the raw material of following parts by weight：
Silica 3-8, soybean oil 30-40, sodium hydroxide 15-20, methanol 100-200, DTAB 2-
3, appropriate calcium chloride, emulsifier op-10 4-8, Tween 80 4-8, chlorimuronethyl 10-20, hydroxypropyl-β-cyclodextrin 40-50, steam
Distilled water 200-500, appropriate warm water.
2. a kind of preparation method of the chlorimuronethyl herbicide of silica absorption according to claim 1, its feature exist
In being made up of following steps：
A. after soybean oil being warming up into 60-70 DEG C, the methanol solution of sodium hydroxide is added, reacts 40-80min under stirring condition,
Excessive methanol is distilled off after end, cools down, stands reactant mixture, removes oil reservoir, washs methyl esters layer with warm water, then use chlorine
Change calcium to dry；
B. 50-70 parts distilled water, emulsifier op-10, Tween 80 and the phonetic sulphur of chlorine are added into esterification soybean oil obtained by step a
It is grand, 20-30min is stirred, forms homogeneous missible oil solution；
C. silica, DTAB are added in step b resulting solutions, 10-30min are stirred by ultrasonic,
Place 5-10h；
D. hydroxypropyl-β-cyclodextrin is dissolved in 80-150 part distilled water, magnetic agitation 10-30min, at room temperature by step c institutes
Obtain solution to be added slowly thereto, continue magnetic agitation 10-15h after dripping, reaction solution rotary evaporation concentrates, filtering, vacuum
4h is dried, obtains white powder.
3. a kind of preparation method of the chlorimuronethyl herbicide of silica absorption according to claim 2, its feature exist
In the preparation method of the methanol solution of sodium hydroxide is：Sodium hydroxide is dissolved in methanol solution under agitation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710906786.7A CN107751228A (en) | 2017-09-29 | 2017-09-29 | A kind of chlorimuronethyl herbicide of silica absorption and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710906786.7A CN107751228A (en) | 2017-09-29 | 2017-09-29 | A kind of chlorimuronethyl herbicide of silica absorption and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107751228A true CN107751228A (en) | 2018-03-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710906786.7A Pending CN107751228A (en) | 2017-09-29 | 2017-09-29 | A kind of chlorimuronethyl herbicide of silica absorption and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101449675A (en) * | 2008-11-19 | 2009-06-10 | 东北农业大学 | Preparation method of herbicide methylated vegetable oil adjuvants |
| CN103535345A (en) * | 2013-09-30 | 2014-01-29 | 江苏省农业科学院 | Mixed pesticide spray auxiliary prepared from waste soybean oil-sunflower oil mixture, and preparation method and application method thereof |
| CN103535346A (en) * | 2013-10-11 | 2014-01-29 | 江苏省农业科学院 | Mixed pesticide spray assistant prepared from waste animal-plant oil mixture and its preparation method and use method |
-
2017
- 2017-09-29 CN CN201710906786.7A patent/CN107751228A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101449675A (en) * | 2008-11-19 | 2009-06-10 | 东北农业大学 | Preparation method of herbicide methylated vegetable oil adjuvants |
| CN103535345A (en) * | 2013-09-30 | 2014-01-29 | 江苏省农业科学院 | Mixed pesticide spray auxiliary prepared from waste soybean oil-sunflower oil mixture, and preparation method and application method thereof |
| CN103535346A (en) * | 2013-10-11 | 2014-01-29 | 江苏省农业科学院 | Mixed pesticide spray assistant prepared from waste animal-plant oil mixture and its preparation method and use method |
Non-Patent Citations (4)
| Title |
|---|
| 中国农业百科全书编辑部: "《中国农业百科全书 农药卷》", 31 October 1993, 农业出版社 * |
| 张金艳: "环糊精对除草剂的包合、增溶与除草活性的研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
| 毕只初等: "十六烷基三甲基溴化铵在二氧化硅表面吸附的研究", 《化学试剂》 * |
| 王秋霞: "甲酯化大豆油助剂的制备及其对除草剂增效作用的研究", 《中国优秀博硕士学位论文全文数据库（硕士） 工程科技I辑》 * |
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Application publication date: 20180306 |
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