CN104115823A - Preparation method of cyhalofop-butyl micro-emulsion - Google Patents

Preparation method of cyhalofop-butyl micro-emulsion Download PDF

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Publication number
CN104115823A
CN104115823A CN201310144806.3A CN201310144806A CN104115823A CN 104115823 A CN104115823 A CN 104115823A CN 201310144806 A CN201310144806 A CN 201310144806A CN 104115823 A CN104115823 A CN 104115823A
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China
Prior art keywords
cyhalofop
butyl
agitator
emulsion
micro
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CN201310144806.3A
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Chinese (zh)
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不公告发明人
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JIANGSU SANYI SINYI PHARMACEUTICAL Co Ltd
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JIANGSU SANYI SINYI PHARMACEUTICAL Co Ltd
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Priority to CN201310144806.3A priority Critical patent/CN104115823A/en
Publication of CN104115823A publication Critical patent/CN104115823A/en
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Abstract

The invention discloses a production method of a cyhalofop-butyl micro-emulsion, and belongs to the field of herbicides. The finished cyhalofop-butyl micro-emulsion is prepared by blending raw materials comprising cyhalofop-butyl, dimethyl formamide, glycol, lignosulfonate and water under specific conditions. The preparation method has the advantages of use of a general apparatus, simple process, mild reaction condition, no emission of pollutant wastes, and good product quality. The cyhalofop-butyl micro-emulsion is mainly used for killing weeds in rice seedling beds, direct seeding fields, transplanting fields and throwing seedling fields, is highly safe to rice, has a special efficacy on moleplant seed and barnyard grass, and can prevent above 30 grassy weeds, such as Paspalum distichum, crab grass, Setaria viridis, Eleusine indica, Alopecurus aequalis and other grassy weeds.

Description

A kind of compound method of cyhalofop-butyl microemulsion
Technical field
The invention belongs to weed killer herbicide field, relate in particular to a kind of compound method of cyhalofop-butyl microemulsion.
Background technology
Cyhalofop-butyl belongs to aryloxy group phenoxy propionic acid class weed killer herbicide, have another name called a thousand pieces of gold, chemical name is (R)-2-[4 (4-cyano group-2-fluorophenoxy) phenoxy group]-butyl propionate, molecular formula is C20H20FNO4, molecular weight is 357.4, former medicine outward appearance is white crystalline solid, proportion is 1.2375,363 ℃ of boiling points, fusing point 48-49 ℃, dissolve in most organic solvents, water insoluble.Cyhalofop-butyl is interior suction conductivity weed killer herbicide, blade and leaf sheath by weeds absorb, phloem conduction, accumulate the meristem zone in weeds, resist acetyl-CoA carboxylase, fatty acid is synthesized and stop, the growth division of cell can not normally be carried out, film systems etc., containing fat structural deterioration, finally cause weeds dead.Controlling object, to paddy rice high safety, to moleplant seed, barnyard grass special efficacy, efficient to above the average age for marriage barnyard grass, hold concurrently and prevent multiple grassy weed simultaneously, as Paspalum distichum, lady's-grass, green foxtail, eleusine indica, amur foxtail etc. more than 30, plant grassy weed, can be used in rice seedling bed, live field, transplant field and seedling throwing field.Cyhalofop-butyl degraded in soil and in rice field rapidly, to succession crop and rice safety, but should not be used as soil treatment, i.e. pesticide-clay mixture or malicious fertile method.On market, for preventing and kill off the cyhalofop-butyl formulation of paddy field weed, be mainly missible oil at present, missible oil formulation is mainly the formulations of pesticide that obtained by mix and blends such as cyhalofop-butyl, emulsifier and organic solvents, because the organic solvent using in missible oil formulation is more, easily to environment, missible oil is in process simultaneously, because using a large amount of organic solvents, the as easy as rolling off a log harm producer.Product of the present invention is a kind of cyhalofop-butyl microemulsion, no matter microemulsion all can not used a large amount of organic solvents in process of manufacture and in use procedure, production cost is greatly reduced, can also reduce the harm to the producer and user, also reduced the pollution to environment simultaneously.The present invention be take cyhalofop-butyl, dimethyl formamide, ethylene glycol, lignosulfonates, water and is produced cyhalofop-butyl microemulsion as raw material, be characterized in that product organic solvent content is lower, handling safety when producing, surrounding environment is polluted few, product dispersity is high, strong to target body weeds permeability, adhesive force good, weeding ratio is high.
Summary of the invention
The problem that the present invention mainly solves is to provide a kind of production method of cyhalofop-butyl microemulsion, the method replaces with water section the microemulsion that most of solvent is produced cyhalofop-butyl, producing this product, to take cyhalofop-butyl, dimethyl formamide, ethylene glycol, lignosulfonates, water be raw material, blending by under given conditions makes finished product cyhalofop-butyl microemulsion, the advantage of this production method is: use common apparatus, technique is simple, reaction condition is gentle, pollution-free waste discharge, good product quality.The raw material weight proportioning of producing this product use is: cyhalofop-butyl 10-12%, dimethyl formamide 8-10%, ethylene glycol 25-27%, lignosulfonates 10-12%, surplus are water.
The present invention can be achieved through the following technical solutions:
A production method for cyhalofop-butyl microemulsion, is characterized in that consisting of following steps:
(1) in the first agitator tank, first the dimethyl formamide of formula ratio is added, start to stir under normal temperature, the rotating speed of agitator is 40 to turn-50 revs/min, adds successively while stirring ethylene glycol, the cyhalofop-butyl of formula ratio, stirring reaction 1.5-2 hour.
(2) in high-speed stirred tank, first the water of formula ratio is added, start to stir under normal temperature, the rotating speed of agitator is 60 to turn-70 revs/min, adds while stirring the lignosulfonates of formula ratio, is stirred to lignosulfonates and all dissolves; The rotating speed of heightening agitator in fast agitator tank is 210-220 rev/min, slowly the cyhalofop-butyl that is dissolved in dimethyl formamide and ethylene glycol is added to high-speed stirred tank, after stirring reaction 1.2-1.5 hour, obtains finished product.
Further technical scheme of the present invention is:
The purity of described cyhalofop-butyl is 97%.
The described stirring reaction time of step (1) is 1.8 hours; The described stirring reaction time of step (2) is 1.3 hours.
Step (1), the described normal temperature of step (2) are 5-35 ℃.
The invention has the beneficial effects as follows: a kind of production method of cyhalofop-butyl microemulsion is provided, and compared to the prior art, tool has the following advantages the method:
(1) technique is simple, and environmental pollution is little, and microemulsion is all used a small amount of organic solvent in process of manufacture and use procedure, and production cost is greatly reduced, and can also reduce the harm to the producer and user, has also reduced the pollution to environment simultaneously.
(2) reaction time short, reaction condition is gentle.
(3) improved drug effect, the oil droplet fineness of the sprinkling emulsion that microemulsion is prepared is 0.001-0.01 micron, has greatly improved the dispersing uniformity of cyhalofop-butyl active ingredient, has improved the availability of control efficiency and medicament.
Embodiment
By following examples, further describe the present invention.
Embodiment 1:
In the first agitator tank, by accounting for total amount, be first that 10% dimethyl formamide adds, under normal temperature, start to stir, the rotating speed of agitator is 40 to turn-50 revs/min, and to add successively while stirring accounting for total amount be 25% ethylene glycol, by accounting for total amount, be 10% cyhalofop-butyl, stirring reaction 1.5-2 hour.In high-speed stirred tank, first just account for total amount and be 43% water and add, start to stir under normal temperature, the rotating speed of agitator is 60 to turn-70 revs/min, and adding while stirring accounting for total amount is 12% lignosulfonates, is stirred to lignosulfonates and all dissolves; The rotating speed of heightening agitator in fast agitator tank is 210-220 rev/min, slowly the cyhalofop-butyl that is dissolved in dimethyl formamide and ethylene glycol is added to high-speed stirred tank, after stirring reaction 1.2-1.5 hour, obtains finished product.
Embodiment 2:
In the first agitator tank, by accounting for total amount, be first that 9% dimethyl formamide adds, under normal temperature, start to stir, the rotating speed of agitator is 40 to turn-50 revs/min, and to add successively while stirring accounting for total amount be 26% ethylene glycol, by accounting for total amount, be 11% cyhalofop-butyl, stirring reaction 1.5-2 hour.In high-speed stirred tank, first just account for total amount and be 43% water and add, start to stir under normal temperature, the rotating speed of agitator is 60 to turn-70 revs/min, and adding while stirring accounting for total amount is 11% lignosulfonates, is stirred to lignosulfonates and all dissolves; The rotating speed of heightening agitator in fast agitator tank is 210-220 rev/min, slowly the cyhalofop-butyl that is dissolved in dimethyl formamide and ethylene glycol is added to high-speed stirred tank, after stirring reaction 1.2-1.5 hour, obtains finished product.
Embodiment 3:
In the first agitator tank, by accounting for total amount, be first that 8% dimethyl formamide adds, under normal temperature, start to stir, the rotating speed of agitator is 40 to turn-50 revs/min, and to add successively while stirring accounting for total amount be 27% ethylene glycol, by accounting for total amount, be 12% cyhalofop-butyl, stirring reaction 1.5-2 hour.In high-speed stirred tank, first just account for total amount and be 43% water and add, start to stir under normal temperature, the rotating speed of agitator is 60 to turn-70 revs/min, and adding while stirring accounting for total amount is 10% lignosulfonates, is stirred to lignosulfonates and all dissolves; The rotating speed of heightening agitator in fast agitator tank is 210-220 rev/min, slowly the cyhalofop-butyl that is dissolved in dimethyl formamide and ethylene glycol is added to high-speed stirred tank, after stirring reaction 1.2-1.5 hour, obtains finished product.

Claims (4)

1. a compound method for cyhalofop-butyl microemulsion, is used the weight proportion of raw material to be: to comprise that cyhalofop-butyl 10-12%, dimethyl formamide 8-10%, ethylene glycol 25-27%, lignosulfonates 10-12%, surplus are water; It is characterized in that: step (1) first adds the dimethyl formamide of formula ratio in the first agitator tank, under normal temperature, start to stir, the rotating speed of agitator is 40 to turn-50 revs/min, adds successively while stirring ethylene glycol, the cyhalofop-butyl of formula ratio, stirring reaction 1.5-2 hour; Step (2) first adds the water of formula ratio in high-speed stirred tank, under normal temperature, start to stir, the rotating speed of agitator is 60 to turn-70 revs/min, the lignosulfonates that add while stirring formula ratio, being stirred to lignosulfonates all dissolves, the rotating speed of heightening agitator in fast agitator tank is 210-220 rev/min, slowly the cyhalofop-butyl that is dissolved in dimethyl formamide and ethylene glycol is added to high-speed stirred tank, after stirring reaction 1.2-1.5 hour, obtains finished product.
2. the compound method of a kind of cyhalofop-butyl microemulsion as claimed in claim 1, is characterized in that: the purity of described cyhalofop-butyl is 97%.
3. the compound method of a kind of cyhalofop-butyl microemulsion as claimed in claim 1, is characterized in that: the described stirring reaction time of step (1) is 1.8 hours; The described stirring reaction time of step (2) is 1.3 hours.
4. the compound method of a kind of cyhalofop-butyl microemulsion as claimed in claim 1, is characterized in that: step (1), the described normal temperature of step (2) are 5-35 ℃.
CN201310144806.3A 2013-04-25 2013-04-25 Preparation method of cyhalofop-butyl micro-emulsion Pending CN104115823A (en)

Priority Applications (1)

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CN201310144806.3A CN104115823A (en) 2013-04-25 2013-04-25 Preparation method of cyhalofop-butyl micro-emulsion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310144806.3A CN104115823A (en) 2013-04-25 2013-04-25 Preparation method of cyhalofop-butyl micro-emulsion

Publications (1)

Publication Number Publication Date
CN104115823A true CN104115823A (en) 2014-10-29

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Application publication date: 20141029