阅读说明：本技术 一种高药效草甘膦颗粒剂助剂的制备方法和应用 (Preparation method and application of glyphosate granule auxiliary agent with high drug effect ) 是由 刘畅 沈德方 崔炎 潘超 高正松 于 2019-11-07 设计创作，主要内容包括：本发明公开了一种高药效草甘膦颗粒剂助剂的制备方法和应用,制备方法包括：卤代烷烃、N,N-二甲基乙醇胺加入到第一溶剂中,在60-70℃反应4-8h,得到烷基二甲基乙醇基卤化铵；将烷基二甲基乙醇基卤化铵与烷基羧酸加入到第二溶剂中,加入催化剂,在95-110℃反应6-8h,得到所需助剂。应用过程包括：将草甘膦酸与碳酸氢铵在50～60℃反应4-8h得到草甘膦铵盐；向所述草甘膦铵盐中加入得到的草甘膦颗粒剂助剂,混合均匀后加入硫酸铵,搅拌均匀；将均匀物料加入到造粒机挤压,呈颗粒状出料；将颗粒状产物加入到沸腾流化床干燥机,烘干得高药效草甘膦颗粒剂制剂。本发明的助剂对草甘膦颗粒剂有着明显的增效作用,在稗草与百日草的除草速率上要优于市面在售助剂。(The invention discloses a preparation method and application of a glyphosate granule auxiliary agent with high drug effect, wherein the preparation method comprises the following steps: adding halogenated alkane and N, N-dimethylethanolamine into a first solvent, and reacting at 60-70 ℃ for 4-8h to obtain alkyl dimethylethanolamine-based ammonium halide; adding alkyl dimethyl ethanol-based ammonium halide and alkyl carboxylic acid into a second solvent, adding a catalyst, and reacting at 95-110 ℃ for 6-8h to obtain the required auxiliary agent. The application process comprises the following steps: reacting glyphosate acid with ammonium bicarbonate at 50-60 ℃ for 4-8h to obtain glyphosate ammonium salt; adding the obtained glyphosate granule auxiliary agent into the glyphosate ammonium salt, uniformly mixing, adding ammonium sulfate, and uniformly stirring; adding the uniform material into a granulator for extrusion, and discharging in a granular form; and adding the granular product into a fluidized bed dryer, and drying to obtain the glyphosate granular preparation with high drug effect. The adjuvant has obvious synergistic effect on glyphosate granules, and is superior to the market-sold adjuvant in weeding speed of barnyard grass and zinnia.)

1. A preparation method of a glyphosate granule auxiliary agent with high drug effect is characterized by comprising the following steps:

(1) adding halogenated alkane and N, N-dimethylethanolamine into a first solvent, and reacting at 60-70 ℃ for 4-8h to obtain alkyl dimethylethanolamine-based ammonium halide;

(2) adding alkyl dimethyl ethanol-based ammonium halide and alkyl carboxylic acid into a second solvent, adding a catalyst, and reacting at 95-110 ℃ for 6-8h to obtain the required auxiliary agent;

the reaction process is as follows:

2. the method for preparing glyphosate granule adjuvant with high drug effect as claimed in claim 1, wherein n is 12, 14, 16; wherein when n =12 or 14, m = 3; n =16, m = 2; and X is Cl or Br.

3. The preparation method of the glyphosate granule adjuvant with high drug effect as claimed in claim 1 or 2, wherein the molar ratio of the reaction of the halogenated alkane and the N, N-dimethylethanolamine is 1: 1-1: 1.2;

the first solvent is one of ethanol, isopropanol or butanol.

4. The method for preparing glyphosate granule adjuvant with high drug effect according to any one of claims 1 to 3, wherein the molar ratio of the alkyl carboxylic acid to the alkyl dimethylethanolammonium halide is 1:1 to 1: 1.2;

the second solvent is one of toluene, xylene or No. 150 solvent oil.

5. The method for preparing glyphosate granule adjuvant with high drug effect as claimed in claim 4, wherein the alkyl carboxylic acid is one of formic acid and glacial acetic acid.

6. The method for preparing glyphosate granule adjuvant with high drug effect according to any one of claims 1 to 5, wherein the catalyst is at least one of concentrated sulfuric acid, p-toluenesulfonic acid or sodium methoxide.

7. The application of the adjuvant prepared by the preparation method of the glyphosate granule adjuvant with high drug effect according to any one of claims 1 to 6 in the preparation of the glyphosate granule formulation with high drug effect is characterized in that the application process comprises the following steps:

(1) reacting glyphosate acid with ammonium bicarbonate at 50-60 ℃ for 4-8h to obtain glyphosate ammonium salt;

(2) adding the obtained glyphosate granule auxiliary agent into the glyphosate ammonium salt, uniformly mixing, adding ammonium sulfate, and uniformly stirring;

(3) adding the uniform material obtained in the step (2) into a granulator for extrusion, and discharging in a granular form;

(4) and (4) adding the granular product obtained in the step (3) into a fluidized bed dryer, and drying to obtain the glyphosate granular preparation with high drug effect.

Technical Field

The invention relates to a preparation method and application of a glyphosate granule auxiliary agent with high drug effect, belonging to the technical field of preparation and application of pesticide auxiliary agents.

Background

Glyphosate is used as a biocidal herbicide in the global range for many years, and currently, aqueous glyphosate products are mainly used in the market at home, but more and more enterprises select products for preparing glyphosate granule series due to higher cost of the aqueous glyphosate in packaging and transportation. The weeding rate of the glyphosate granules on the market is slower than that of a glyphosate aqueous solution in the actual use process, and the weeding rate is greatly related to the types of the additives used in the glyphosate granules.

Chinese patent document CN1433690A proposes the use of polyoxyethylene block copolymer, polyoxyethylene ether alkyl sorbitol ester, tallow amine polyoxyethylene ether, etc. as adjuvants to prepare glyphosate granules; in the preparation of glyphosate granules in chinese patent document CN103109801A, isomeric mixed alcohol polyoxyethylene ether, complex fatty group ethoxylate, and cocamidopropyl oxide are used as adjuvants. Most of the adjuvants used in the glyphosate granules on the market are compounded by the monomers, but the early weeding speed is slow in practical use, so that the preparation method of the glyphosate granule preparation needs to be improved, and the high weeding efficiency of the glyphosate granules is achieved.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a preparation method and application of a glyphosate granule auxiliary agent with high drug effect.

The technical purpose of the invention is realized by the following technical scheme:

the invention provides a preparation method of a glyphosate granule auxiliary agent with high drug effect, which comprises the following steps:

(1) adding halogenated alkane and N, N-dimethylethanolamine into a first solvent, and reacting at 60-70 ℃ for 4-8h to obtain alkyl dimethylethanolamine-based ammonium halide;

(2) adding alkyl dimethyl ethanol-based ammonium halide and alkyl carboxylic acid into a second solvent, adding a catalyst, and reacting at 95-110 ℃ for 6-8h to obtain the required auxiliary agent;

the reaction process is as follows:

by adopting the technical scheme, the high-drug-effect glyphosate granule auxiliary agent is prepared through simple two-step reaction, the reaction process is mild, excessive temperature and reaction conditions are not needed, and the auxiliary agent obtained through the reaction is low in cost.

Preferably, n is 12, 14, 16; wherein when n is 12 or 14, m is 3; when n is 16, m is 2; and X is Cl or Br.

By adopting the technical scheme and the substituent groups, the reaction process is easy to control, the reaction yield is high, and the alkyl chain is easy to control.

Preferably, the molar ratio of the halogenated alkane to the N, N-dimethylethanolamine is 1: 1-1: 1.2; the first solvent is one of ethanol, isopropanol or butanol.

By adopting the technical scheme, under the condition of proper molar ratio, the obtained product has high purity and easy purification, and simultaneously, the pollution caused by adding excessive raw materials is avoided.

Preferably, the molar ratio of the alkyl carboxylic acid to the alkyl dimethylethanol-based ammonium halide is 1:1 to 1: 1.2; the second solvent is one of toluene, xylene or No. 150 solvent oil.

By adopting the technical scheme, under the condition of proper molar ratio, the obtained product has high purity and easy purification, and simultaneously, the pollution caused by adding excessive raw materials is avoided.

Preferably, the alkyl carboxylic acid is one of formic acid or glacial acetic acid.

By adopting the technical scheme, the obtained product has good treatment effect, and poor reaction effect caused by overlong alkyl chains is avoided.

Preferably, the catalyst is at least one of concentrated sulfuric acid, p-toluenesulfonic acid or sodium methoxide.

By adopting the technical scheme, the reaction rate is high, and the increase of byproducts caused by overlong reaction time is avoided.

Meanwhile, the invention also provides application of the high-drug-effect glyphosate granule auxiliary agent in preparation of a high-drug-effect glyphosate granule preparation, and the application process comprises the following steps:

(1) reacting glyphosate acid with ammonium bicarbonate at 50-60 ℃ for 4-8h to obtain glyphosate ammonium salt;

(2) adding the obtained glyphosate granule auxiliary agent into the glyphosate ammonium salt, uniformly mixing, adding ammonium sulfate, and uniformly stirring;

(3) adding the uniform material obtained in the step (2) into a granulator for extrusion, and discharging in a granular form;

(4) and (4) adding the granular product obtained in the step (3) into a fluidized bed dryer, and drying to obtain the glyphosate granular preparation with high drug effect.

By adopting the technical scheme, the glyphosate granule preparation with high drug effect is prepared, the application method of the auxiliary agent is simple, and the application process is easy to control.

In conclusion, the invention has the following beneficial effects:

(1) the preparation method of the high-drug-effect glyphosate granule auxiliary agent provided by the invention can be used for preparing the high-drug-effect glyphosate granule auxiliary agent through simple two-step reaction, the reaction process is mild, excessive temperature and reaction conditions are not needed, and the auxiliary agent obtained through the reaction is low in cost.

(2) The application of the high-drug-effect glyphosate granular agent in the preparation of the high-drug-effect glyphosate granular preparation is simple in application method and easy to control in application process, and compared with the glyphosate granular preparation obtained by adopting other commercially available agents, the obtained high-drug-effect glyphosate granular preparation has the advantages that the weeding speed of barnyard grass and zinnia elegans is obviously increased, the control efficiency of the barnyard grass after 5 days can reach 95.6%, and the control efficiency of the zinnia elegans after 5 days is 90.4%.

Detailed Description

The invention is further described below. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.