CN104115828A - Preparation method of cyhalofop butyl and pretilachlor mixed microemulsion - Google Patents

Preparation method of cyhalofop butyl and pretilachlor mixed microemulsion Download PDF

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Publication number
CN104115828A
CN104115828A CN201310149944.0A CN201310149944A CN104115828A CN 104115828 A CN104115828 A CN 104115828A CN 201310149944 A CN201310149944 A CN 201310149944A CN 104115828 A CN104115828 A CN 104115828A
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China
Prior art keywords
cyhalofop
butyl
pretilachlor
careless amine
adds
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CN201310149944.0A
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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 CN201310149944.0A priority Critical patent/CN104115828A/en
Publication of CN104115828A publication Critical patent/CN104115828A/en
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Abstract

The invention discloses a preparation method of cyhalofop butyl and pretilachlor mixed microemulsion; the cyhalofop butyl and pretilachlor mixed microemulsion product belongs to the field of herbicides; the finished cyhalofop butyl and pretilachlor mixed microemulsion product is prepared from cyhalofop butyl, pretilachlor, toluene cyclohexanone, styrene, polyoxyethylene lauryl ether sodium sulfonate and water as raw materials by mixing under specific conditions, and the production method has the advantages of use of general equipment, simple process, mild reaction condition, no pollution waste emissions and good product quality. The finished cyhalofop butyl and pretilachlor mixed microemulsion product is high in security to rice, has significant effects on moleplant seed, sheathed monochoria herb, difformed galingale herb, eleocharis yokoscensis, eclipta prostrate, rotala indica, lindernia procumbens, false loosestrife, scirpus juncoides roxb, cyperus iria and the like, and has treatment and inhibition effects on digitaria haller, water purslane, marsilea quadrifolia L and the like, and the effect lasting period is 30-50 day.

Description

The compound method of a kind of cyhalofop-butyl and the third careless amine complex microemulsion
Technical field
The invention belongs to weed killer herbicide field, relate in particular to the compound method of a kind of cyhalofop-butyl and the third careless amine complex microemulsion.
Background technology
Cyhalofop-butyl belongs to aryloxy group phenoxy propionic acid class weed killer herbicide, has another name called a thousand pieces of gold, and molecular formula is C20H20FNO4, and molecular weight is 357.4, former medicine outward appearance is white crystalline solid, and proportion is 1.2375,363 ℃ of boiling points, fusing point 48-49 ℃, dissolves 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 is rapid, to succession crop and rice safety.The third careless amine, claim again ten safeners, processing formulation is 30% missible oil, and effective ingredient is every 1 liter and contains 300 grams of the third careless amine, the third careless amine is selective herbicide before the bud of amide-type rice field, can to a leaf, wholeheartedly with interior barnyard grass preventive effect, can reach more than 95% safely for live field and rice seedling bed safe due to it, user can reduce seeding quantity, the spending of saving seed has reduced the sandwich barnyard grass to paddy rice underproduction maximum, for increasing production of rice has been laid reliable basis simultaneously; The third careless amine is except weeds gramineous are had good preventive effect, can also prevent and kill off multiple annual nutgrass flatsedge and broadleaf weed, as Monochoria vaginalis, difformed galingale herb, needle spikesedge herb, Eclipta prostrata, mexicana, Procumbent Falsepimpernel, false loosestrife, firefly Lin, cyperus iria etc., knotgrass, water purslane, four Ye Ping etc. are also had to double controlling and inhibitory action, remarkable to difficult anti-weeds preventive effects such as moleplant seeds, lasting period 30-50 days, substantially can control nursery period overall process weeds, and easy to use, after can directly diluting, with sprayer, be sprayed on seedling bed, also can mix fine earth, be spread on seedling face.Cyhalofop-butyl and the third careless amine is composite a synergistic effect, by above-mentioned two kinds of weed killer herbicides and auxiliary material composite after, the effect of preventing and kill off paddy field weed is significantly higher than alone cyanogen fluorine grass or the third careless amine, herbicidal effect strengthens greatly.
Summary of the invention
The problem that the present invention mainly solves is to provide the production method of a kind of cyhalofop-butyl and the third careless amine complex microemulsion, producing this product, to take cyhalofop-butyl, the third careless amine, toluene cyclohexanone, styrene, ethoxylated dodecyl alcohol sodium sulfonate, water be raw material, blending by under given conditions makes finished product, 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 8-9%, the third careless amine 5-6%, toluene cyclohexanone 5-6%, styrene 12-13%, ethoxylated dodecyl alcohol sodium sulfonate 5-6%, surplus are water.
The present invention can be achieved through the following technical solutions:
A compound method for cyhalofop-butyl and the third careless amine complex microemulsion, is characterized in that consisting of following steps:
(1) in the first agitator tank, first the toluene cyclohexanone of formula ratio is added, start to stir under normal temperature, the rotating speed of agitator is 35 to turn-40 revs/min, adds successively while stirring styrene, cyhalofop-butyl, the third careless amine of formula ratio, stirring reaction 1.0-1.2 hour.
(2) in high-speed stirred tank, first the water of formula ratio is added, under normal temperature, start to stir, the rotating speed of agitator is 50 to turn-60 revs/min, adds while stirring the ethoxylated dodecyl alcohol sodium sulfonate of formula ratio, is stirred to ethoxylated dodecyl alcohol sodium sulfonate and all dissolves; Heightening the rotating speed of agitator in fast agitator tank is 210-220 rev/min, will be dissolved in slowly toluene cyclohexanone and cinnamic cyhalofop-butyl, the third careless amine adds high-speed stirred tank, after stirring reaction 0.9-1.0 hour, obtains finished product.
Further technical scheme of the present invention is:
Described cyhalofop-butyl purity is 97%, the purity of benthiocarb is 30%.
The described stirring reaction time of step (1) is 1.1 hours; The described high-speed stirred reaction time of step (2) is 0.95 hour.
Step (1), the described normal temperature of step (2) are 5-35 ℃.
The invention has the beneficial effects as follows: the compound method that a kind of cyhalofop-butyl and the third careless amine complex microemulsion are provided, the advantage of the method is: technique is simple, environmental pollution is little, the reaction time is short, reaction condition is gentle, by above-mentioned two kinds of weed killer herbicides and auxiliary material composite after, product is mainly used in paddy field, the effect of anti-weeding significantly strengthens, and the kind of anti-weeding further increases.
Embodiment
By following examples, further describe the present invention.
Embodiment 1:
In the first agitator tank, by accounting for total amount, be first that 5% toluene cyclohexanone adds, under normal temperature, start to stir, the rotating speed of agitator is 35 to turn-40 revs/min, to add successively while stirring that to account for total amount be 13% styrene, account for total amount be 8% cyhalofop-butyl, account for total amount is the third careless amine of 6%, stirring reaction 1.0-1.2 hour.In high-speed stirred tank, by accounting for total amount, be first that 63% water adds, under normal temperature, start to stir, the rotating speed of agitator is 50 to turn-60 revs/min, adds while stirring that to account for total amount be 5% ethoxylated dodecyl alcohol sodium sulfonate, is stirred to ethoxylated dodecyl alcohol sodium sulfonate and all dissolves; Heightening the rotating speed of agitator in fast agitator tank is 210-220 rev/min, will be dissolved in slowly toluene cyclohexanone and cinnamic cyhalofop-butyl, the third careless amine adds high-speed stirred tank, after stirring reaction 0.9-1.0 hour, obtains finished product.
Embodiment 2:
In the first agitator tank, by accounting for total amount, be first that 5.5% toluene cyclohexanone adds, under normal temperature, start to stir, the rotating speed of agitator is 35 to turn-40 revs/min, to add successively while stirring that to account for total amount be 12.5% styrene, account for total amount be 8.5% cyhalofop-butyl, account for total amount is the third careless amine of 5.5%, stirring reaction 1.0-1.2 hour.In high-speed stirred tank, by accounting for total amount, be first that 62.5% water adds, under normal temperature, start to stir, the rotating speed of agitator is 50 to turn-60 revs/min, adds while stirring that to account for total amount be 5.5% ethoxylated dodecyl alcohol sodium sulfonate, is stirred to ethoxylated dodecyl alcohol sodium sulfonate and all dissolves; Heightening the rotating speed of agitator in fast agitator tank is 210-220 rev/min, will be dissolved in slowly toluene cyclohexanone and cinnamic cyhalofop-butyl, the third careless amine adds high-speed stirred tank, after stirring reaction 0.9-1.0 hour, obtains finished product.
Embodiment 3:
In the first agitator tank, by accounting for total amount, be first that 6% toluene cyclohexanone adds, under normal temperature, start to stir, the rotating speed of agitator is 35 to turn-40 revs/min, to add successively while stirring that to account for total amount be 12% styrene, account for total amount be 9% cyhalofop-butyl, account for total amount is the third careless amine of 5%, stirring reaction 1.0-1.2 hour.In high-speed stirred tank, by accounting for total amount, be first that 62% water adds, under normal temperature, start to stir, the rotating speed of agitator is 50 to turn-60 revs/min, adds while stirring that to account for total amount be 6% ethoxylated dodecyl alcohol sodium sulfonate, is stirred to ethoxylated dodecyl alcohol sodium sulfonate and all dissolves; Heightening the rotating speed of agitator in fast agitator tank is 210-220 rev/min, will be dissolved in slowly toluene cyclohexanone and cinnamic cyhalofop-butyl, the third careless amine adds high-speed stirred tank, after stirring reaction 0.9-1.0 hour, obtains finished product.

Claims (4)

1. a compound method for cyhalofop-butyl and the third careless amine complex microemulsion, is used the weight proportion of raw material to be: to comprise that cyhalofop-butyl 8-9%, the third careless amine 5-6%, toluene cyclohexanone 5-6%, styrene 12-13%, ethoxylated dodecyl alcohol sodium sulfonate 5-6%, surplus are water; It is characterized in that: step (1) first adds the toluene cyclohexanone of formula ratio in the first agitator tank, under normal temperature, start to stir, the rotating speed of agitator is 35 to turn-40 revs/min, adds successively while stirring styrene, cyhalofop-butyl, the third careless amine of formula ratio, stirring reaction 1.0-1.2 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 50 to turn-60 revs/min, adds while stirring the ethoxylated dodecyl alcohol sodium sulfonate of formula ratio, is stirred to ethoxylated dodecyl alcohol sodium sulfonate and all dissolves; Heightening the rotating speed of agitator in fast agitator tank is 210-220 rev/min, will be dissolved in slowly toluene cyclohexanone and cinnamic cyhalofop-butyl, the third careless amine adds high-speed stirred tank, after stirring reaction 0.9-1.0 hour, obtains finished product.
2. the compound method of a kind of cyhalofop-butyl as claimed in claim 1 and the third careless amine complex microemulsion, is characterized in that: described cyhalofop-butyl purity is 97%, the purity of benthiocarb is 30%.
3. the compound method of a kind of cyhalofop-butyl as claimed in claim 1 and the third careless amine complex microemulsion, is characterized in that: the described stirring reaction time of step (1) is 1.1 hours; The described high-speed stirred reaction time of step (2) is 0.95 hour.
4. the compound method of a kind of cyhalofop-butyl as claimed in claim 1 and the third careless amine complex microemulsion, is characterized in that: step (1), the described normal temperature of step (2) are 5-35 ℃.
CN201310149944.0A 2013-04-27 2013-04-27 Preparation method of cyhalofop butyl and pretilachlor mixed microemulsion Pending CN104115828A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105746548A (en) * 2015-07-31 2016-07-13 南通惠然生物科技有限公司 Rice herbicide
CN106719683A (en) * 2016-12-14 2017-05-31 安徽扬子化工有限公司 A kind of efficient farmland weeding agent prescription

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105746548A (en) * 2015-07-31 2016-07-13 南通惠然生物科技有限公司 Rice herbicide
CN106719683A (en) * 2016-12-14 2017-05-31 安徽扬子化工有限公司 A kind of efficient farmland weeding agent prescription

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Application publication date: 20141029