CN104222101A - A preparing method of a carfentrazone-ethyl/2-methyl-4-chlorophenoxy acetic acid microemulsion - Google Patents

A preparing method of a carfentrazone-ethyl/2-methyl-4-chlorophenoxy acetic acid microemulsion Download PDF

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Publication number
CN104222101A
CN104222101A CN201310230962.1A CN201310230962A CN104222101A CN 104222101 A CN104222101 A CN 104222101A CN 201310230962 A CN201310230962 A CN 201310230962A CN 104222101 A CN104222101 A CN 104222101A
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agitator
azoles humulone
methoxone
hour
product
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CN201310230962.1A
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不公告发明人
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XINYI HANLING BIO-ENGINEERING Co Ltd
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XINYI HANLING BIO-ENGINEERING Co Ltd
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Publication of CN104222101A publication Critical patent/CN104222101A/en
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Abstract

The invention discloses a preparing method of a carfentrazone-ethyl/2-methyl-4-chlorophenoxy acetic acid microemulsion. A product of the method belongs to the field of herbicides. Carfentrazone-ethyl is adopted as the main raw material, 2-methyl-4-chlorophenoxy acetic acid, toluene, diethyl ether, sodium alkyl alcohol polyoxyethylene ether sulfate and water are adopted as auxiliary materials. A finished product is obtained by a series of blending processes under specific conditions. The preparing method has advantages of using of universal equipment, simple process, mild reaction conditions, no discharge of pollutants or waste and high product quality; the product is mainly used for control of broad-leaf weeds and red couch grass; the product has excellent control effects especially for catchweed, piemarker, chenopodium album, shepherd's purse, sun euphorbia herb, lithospermum arvense, fistular morning glory, and other weeds; and the product has high activity for weeds generating resistance to sulfonylurea type herbicides.

Description

The compound method of a kind of azoles humulone and methoxone microemulsion
Technical field
The invention belongs to weed killer herbicide field, particularly relate to the compound method of a kind of azoles humulone and methoxone microemulsion.
Background technology
Azoles humulone have another name called good fortune agriculture, soon go out spirit, triazolone grass ester, carfentrazone, molecular formula is C15H14Cl2F3N3O3,
Former medicine outward appearance is sticky yellow liquid, be slightly soluble in water, very easily be dissolved in toluene, azoles humulone is a kind of contact killing type selective herbicide, under the condition having light, in chlcrophyll biosynthesis process, by the accumulation suppressing proporphyrinogen oxidase to cause poisonous intermediate, thus destroy the cell membrane of weeds, blade is dried up rapidly, dead, namely azoles humulone is absorbed by plant leaf blade in 15 minutes after spray medicine, it is not drenched with rain affects, after 3-4 hours just there is poisoning symptom in weeds, 2-4 days dead, its action character is that herbicide speed is fast, fool proof to succession crop, it is the fine herbicide that wheatland is eliminated spring, be mainly used in preventing and kill off broad leaved weed and nutgrass flatsedge, especially to clearvers, piemarker, red heart lamb's-quarters, shepherd's purse, wartwort, corn gromwell, the blank pipe weeds such as to lead a cow have excellent preventive effect, the weeds etc. sulfonylurea herbicide being produced to resistance have good activity.Methoxone is colourless crystallization, belong to lower toxicity weed killer herbicide, be slightly soluble in water, be soluble in the organic solvent such as ethanol, ether, 2 first 4 chlorine belong to phenoxy carboxylic acid selective herbicide, there is stronger Uptake and translocation, be mainly used in cauline leaf process after seedling, medicament, through cuticula and cytoplasma membrane, is finally transmitted to each several part, produces Different Effects at different parts to nucleic acid and protein synthesis, the synthesis of metabolism of nucleic acid and protein is suppressed at plant tip, photosynthesis growing point stopped growing, young leaflet tablet not tensible, until can not normally carry out; Be transmitted to the medicament of plant bottom, the synthesis of the nucleic acid that plant stem is organized and protein increases, and promote abnormal cell division, the tip of a root expands, lose the ability absorbing nutrient, cause cane distortion, deformity, screen casing blocks, and phloem destroys, organic matter transport is obstructed, thus destroy the normal viability of plant, finally cause Plant death, can be used for preventing and kill off most of annual broadleaf weed.Product of the present invention with azoles humulone for major ingredient, made by a series of blending technique for auxiliary material with methoxone, toluene, ether, alkylol polyoxyethylene groups ether sodium sulfate, water, this production method has series of advantages such as use common apparatus, technique is simple, reaction condition is gentle, pollution-free waste discharge, good product quality etc., product is good dispersion in water, active high, strong to target body weeds permeability, adhesive force is good, kills power powerful.
Summary of the invention
The problem that the present invention mainly solves is to provide the compound method of a kind of azoles humulone and methoxone microemulsion, produce this product with azoles humulone for major ingredient, with methoxone, toluene, ether, alkylol polyoxyethylene groups ether sodium sulfate, water for auxiliary material, obtained finished product is carried out by blending under given conditions, 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 the use of this product is: azoles humulone 10-12%, toluene 14-16%, methoxone 4-6%, ether 8-10%, alkylol polyoxyethylene groups ether sodium sulfate 3-5%, surplus are water.
The present invention can be achieved through the following technical solutions:
A compound method for azoles humulone and methoxone microemulsion, is characterized in that being made up of following steps:
(1) first added by the ether of formula ratio in the first agitator tank, start under normal temperature to stir, the rotating speed of agitator is 30-35 rev/min, adds the methoxone of formula ratio while stirring, stirring reaction 0.5-0.7 hour.
(2) first added by the toluene of formula ratio in the second agitator tank, start under normal temperature to stir, the rotating speed of agitator is 30-35 rev/min, adds the azoles humulone of formula ratio while stirring, stirring reaction 0.3-0.5 hour.
(3) first added by the water of formula ratio in high-speed stirred tank, start under normal temperature to stir, the rotating speed of agitator is 30-40 rev/min, adds the alkylol polyoxyethylene groups ether sodium sulfate of formula ratio while stirring, is stirred to and mixes; The rotating speed heightening agitator in fast agitator tank is 210-220 rev/min, slowly the methoxone being dissolved in ether is added after high-speed stirred tank stirs 0.3 hour and again the azoles humulone being dissolved in toluene is added high-speed stirred tank, after stirring reaction 1.0-1.2 hour, obtain finished product.
Further technical scheme of the present invention is:
The purity of described azoles humulone is 90%.
The stirring reaction time described in step (1) is 0.6 hour; The stirring reaction time described in step (2) is 0.4 hour; The high-speed stirred reaction time described in step (3) is 1.1 hours.
Step (1), step (2), normal temperature described in step (3) are 5-35 DEG C.
The invention has the beneficial effects as follows: the compound method providing a kind of azoles humulone and methoxone microemulsion, the method tool has the following advantages: production technology is simple, environmental pollution is little, reaction time is short, and reaction condition is gentle, and product is good dispersion in water, active high, strong to target body broad leaved weed and nutgrass flatsedge permeability, adhesive force is good, kills power powerful.
Embodiment
The present invention is further described by following examples.
Embodiment 1:
In the first agitator tank first by account for total amount be 10% ether add, start under normal temperature stir, the rotating speed of agitator is 30-35 rev/min, adds while stirring and accounts for the methoxone that total amount is 4%, stirring reaction 0.5-0.7 hour.In the second agitator tank first by account for total amount be 16% toluene add, start under normal temperature stir, the rotating speed of agitator is 30-35 rev/min, adds while stirring and accounts for the azoles humulone that total amount is 10%, stirring reaction 0.3-0.5 hour.In high-speed stirred tank first by account for total amount be 57% water add, start under normal temperature stir, the rotating speed of agitator is 30-40 rev/min, adds while stirring and accounts for the alkylol polyoxyethylene groups ether sodium sulfate that total amount is 3%, be stirred to and mix; The rotating speed heightening agitator in fast agitator tank is 210-220 rev/min, slowly the methoxone being dissolved in ether is added after high-speed stirred tank stirs 0.3 hour and again the azoles humulone being dissolved in toluene is added high-speed stirred tank, after stirring reaction 1.0-1.2 hour, obtain finished product.
Embodiment 2:
In the first agitator tank first by account for total amount be 9% ether add, start under normal temperature stir, the rotating speed of agitator is 30-35 rev/min, adds while stirring and accounts for the methoxone that total amount is 5%, stirring reaction 0.5-0.7 hour.In the second agitator tank first by account for total amount be 15% toluene add, start under normal temperature stir, the rotating speed of agitator is 30-35 rev/min, adds while stirring and accounts for the azoles humulone that total amount is 11%, stirring reaction 0.3-0.5 hour.In high-speed stirred tank first by account for total amount be 56% water add, start under normal temperature stir, the rotating speed of agitator is 30-40 rev/min, adds while stirring and accounts for the alkylol polyoxyethylene groups ether sodium sulfate that total amount is 4%, be stirred to and mix; The rotating speed heightening agitator in fast agitator tank is 210-220 rev/min, slowly the methoxone being dissolved in ether is added after high-speed stirred tank stirs 0.3 hour and again the azoles humulone being dissolved in toluene is added high-speed stirred tank, after stirring reaction 1.0-1.2 hour, obtain finished product.
Embodiment 3:
In the first agitator tank first by account for total amount be 8% ether add, start under normal temperature stir, the rotating speed of agitator is 30-35 rev/min, adds while stirring and accounts for the methoxone that total amount is 6%, stirring reaction 0.5-0.7 hour.In the second agitator tank first by account for total amount be 14% toluene add, start under normal temperature stir, the rotating speed of agitator is 30-35 rev/min, adds while stirring and accounts for the azoles humulone that total amount is 12%, stirring reaction 0.3-0.5 hour.In high-speed stirred tank first by account for total amount be 55% water add, start under normal temperature stir, the rotating speed of agitator is 30-40 rev/min, adds while stirring and accounts for the alkylol polyoxyethylene groups ether sodium sulfate that total amount is 5%, be stirred to and mix; The rotating speed heightening agitator in fast agitator tank is 210-220 rev/min, slowly the methoxone being dissolved in ether is added after high-speed stirred tank stirs 0.3 hour and again the azoles humulone being dissolved in toluene is added high-speed stirred tank, after stirring reaction 1.0-1.2 hour, obtain finished product.

Claims (4)

1. a compound method for azoles humulone and methoxone microemulsion, uses the weight proportion of raw material to be: comprise azoles humulone 10-12%, toluene 14-16%, methoxone 4-6%, ether 8-10%, alkylol polyoxyethylene groups ether sodium sulfate 3-5%, surplus be water; It is characterized in that: the ether of formula ratio first adds by step (1) in the first agitator tank, start under normal temperature to stir, the rotating speed of agitator is 30-35 rev/min, adds the methoxone of formula ratio while stirring, stirring reaction 0.5-0.7 hour; The toluene of formula ratio first adds by step (2) in the second agitator tank, starts to stir under normal temperature, and the rotating speed of agitator is 30-35 rev/min, adds the azoles humulone of formula ratio while stirring, stirring reaction 0.3-0.5 hour; The water of formula ratio first adds by step (3) in high-speed stirred tank, starts to stir under normal temperature, and the rotating speed of agitator is 30-40 rev/min, adds the alkylol polyoxyethylene groups ether sodium sulfate of formula ratio while stirring, is stirred to and mixes; The rotating speed heightening agitator in fast agitator tank is 210-220 rev/min, slowly the methoxone being dissolved in ether is added after high-speed stirred tank stirs 0.3 hour and again the azoles humulone being dissolved in toluene is added high-speed stirred tank, after stirring reaction 1.0-1.2 hour, obtain finished product.
2. the compound method of a kind of azoles humulone as claimed in claim 1 and methoxone microemulsion, is characterized in that: the purity of described azoles humulone is 90%.
3. the compound method of a kind of azoles humulone as claimed in claim 1 and methoxone microemulsion, is characterized in that: the stirring reaction time described in step (1) is 0.6 hour; The stirring reaction time described in step (2) is 0.4 hour; The high-speed stirred reaction time described in step (3) is 1.1 hours.
4. the compound method of a kind of azoles humulone as claimed in claim 1 and methoxone microemulsion, is characterized in that: step (1), step (2), normal temperature described in step (3) are 5-35 DEG C.
CN201310230962.1A 2013-06-10 2013-06-10 A preparing method of a carfentrazone-ethyl/2-methyl-4-chlorophenoxy acetic acid microemulsion Pending CN104222101A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108064868A (en) * 2016-11-15 2018-05-25 江苏龙灯化学有限公司 A kind of Herbicidal combinations
WO2021148304A1 (en) * 2020-01-23 2021-07-29 Basf Se Ppo formulations containing ether sulfates

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108064868A (en) * 2016-11-15 2018-05-25 江苏龙灯化学有限公司 A kind of Herbicidal combinations
WO2021148304A1 (en) * 2020-01-23 2021-07-29 Basf Se Ppo formulations containing ether sulfates

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Application publication date: 20141224