CN102939991A - Preparation technology of isopropylamine salt of n-glycine with mass percentage of 41% - Google Patents

Abstract

The invention provides a preparation technology of isopropylamine salt of n-glycine with mass percentage of 41%, comprising the following steps: carrying out alkaline hydrolysis, acidification, condensation, and crystallization on raw material iminodiacetonitrile, filtering to obtain intermediate pmida, carrying out air oxidation on pmida in the presence of catalyst to obtain glyphosate, then conducting cooling crystallization to separate solids out, carrying out amination, circulation, filtration, and mixing on the solids to finally obtain isopropylamine salt of n-glycine with mass percentage of 41%. According to the invention, the steps of amination, acidification, crystallization, centrifugation and drying related in using raw powder to produce isopropylamine salt of n-glycine with mass percentage of 41% in the prior art are omitted, the production technology of glyphosate isopropylamine is greatly simplified; the preparation technology disclosed herein can raise the product yield by 8%, reduces the production cost of isopropylamine salt of n-glycine with mass percentage of 41%, reduces raw material and energy consumption, and reduces environmental pollution.

Description

A kind of mass percent is the manufacturing process of 41% glyphosate isopropylamine salt water solution

Technical field

The present invention relates to the manufacturing process of weed killer herbicide, concrete finger is that a kind of mass percent is the manufacturing process of 41% glyphosate isopropylamine salt water solution.

Background technology

Glyphosate is a kind of good organic phosphine class nonselective herbicide, is the natural disposition highy potent herbicide that goes out behind the bud of a kind of efficient, low toxicity, low-residual, broad weed-killing spectrum, has good interior suction, conductive performance.At present, to mainly contain mass percent be 10% gyphosate solution, 30% glyphosate amine salt aqua, 41% glyphosate isopropylamine salt water solution, 62% glyphosate isopropyl amine salt, 68% glyphosate amine salt soluble granule and 50% glyphosate amine salt soluble powder etc. to the production formulation of glyphosate.In order further to enrich glyphosate products series, the in addition 10% gyphosate solution production that will be under an embargo, its market vacancy will be by 30% glyphosate amine salt aqua, 41% glyphosate isopropylamine salt water solution, 62% glyphosate isopropyl amine salt, 68% glyphosate amine salt soluble granule and 50% glyphosate amine salt soluble powder etc. replace, the production of other manufacturer's 41% glyphosate isopropylamine salt water solutions is to produce first the former powder finished product of 95% glyphosate at present, then take the former powder of 95% glyphosate as raw material, add a certain amount of water, add the isopropylamine allotment and form, the 41% glyphosate isopropylamine salt water solution production cost that the method is produced is high.

Summary of the invention

The purpose of this invention is to provide a kind of can cutting down the consumption of raw materials, energy consumption, the mass percent of environmental contamination reduction is the manufacturing process of 41% glyphosate isopropylamine salt water solution.

For achieving the above object, mass percent provided by the invention is the manufacturing process of 41% glyphosate isopropylamine salt water solution, and it comprises following steps:

(1) the raw material iminodiacetonitrile is added NaOH and water and carries out alkaline hydrolysis after, add PCl ₃Carry out acidification reaction with HCl, rear adding HCHO carries out condensation reaction, adds subsequently NaOH and water and carries out crystallization, adds water filtration again and obtains the intermediate PMIDA;

(2) the intermediate PMIDA obtains glyphosate and Mixture of Activated Carbon by air oxidation under the effect of activated-carbon catalyst, and described glyphosate and Mixture of Activated Carbon obtain glyphosate and activated charcoal solid mixture by decrease temperature crystalline, isolated by filtration;

(3) the isolated glyphosate of decrease temperature crystalline in the step (2) and activated charcoal solid mixture being added water and isopropylamine, to be deployed into mass percent be 46% the female medicine of glyphosate isopropyl amine salt, the mixture of glyphosate mother solution and active carbon, the mixture of gained was through filtering after allotment was finished, obtain mass percent and be 46% the female medicine of glyphosate isopropyl amine salt, glyphosate mother solution and active carbon, be that the female medicine of 46% glyphosate isopropyl amine salt adds water to be deployed into mass percent be 41% glyphosate isopropylamine salt water solution at last with mass percent, glyphosate mother solution and washing active carbon that filtration is obtained, filter, the glyphosate mother solution that obtains returns with isopropylamine and repeats allotment, and active carbon returns recycled in the step (2) as catalyzer.

Technique provided by the present invention, adopt advanced non-salt process, be the female medicine of 46% glyphosate isopropyl amine salt in the complete rear directly synthetic mass percent of oxidation reaction, be mixed with mass percent after the filtration of active charcoal and be 41% glyphosate isopropylamine salt water solution, further reduce cost.

The invention has the advantages that: related amination when the present invention has saved the former powder quality of production of present employing percentage and is 41% glyphosate isopropylamine salt water solution, acidifying, crystallization, centrifugal, the dry five processes that waits, greatly simplified the glyphosate isopropyl amine salt production technology, and process of the present invention can improve 8 percentage points of product yields, and having reduced mass percent is 41% glyphosate isopropylamine salt water solution production cost, cuts down the consumption of raw materials, energy consumes, environmental contamination reduction.

Description of drawings

Fig. 1 is process chart of the present invention.

Embodiment

The present invention is described in further detail below in conjunction with the drawings and specific embodiments.

As shown in the figure, after the raw material iminodiacetonitrile added NaOH and water and carry out alkaline hydrolysis, add PCl ₃Carry out acidification reaction with HCl, rear adding HCHO carries out condensation reaction, adds subsequently NaOH and water and carries out crystallization, adds water filtration again and obtains the intermediate PMIDA.

The intermediate PMIDA obtains glyphosate and Mixture of Activated Carbon by air oxidation under the effect of activated-carbon catalyst, described glyphosate and Mixture of Activated Carbon obtain glyphosate and activated charcoal solid mixture by decrease temperature crystalline, isolated by filtration;

The isolated glyphosate of decrease temperature crystalline and activated charcoal solid mixture are added water and isopropylamine, and to be deployed into mass percent be 46% the female medicine of glyphosate isopropyl amine salt, the mixture of glyphosate mother solution and active carbon, the mixture of gained was through filtering after allotment was finished, obtain mass percent and be 46% the female medicine of glyphosate isopropyl amine salt, glyphosate mother solution and active carbon, be that the female medicine of 46% glyphosate isopropyl amine salt adds water to be deployed into mass percent be 41% glyphosate isopropylamine salt water solution at last with mass percent, glyphosate mother solution and washing active carbon that filtration is obtained, filter, the glyphosate mother solution that obtains returns with isopropylamine and repeats allotment, and active carbon returns recycled as catalyzer.

Operation principle of the present invention: it is as primary raw material take iminodiacetonitrile, quality of production percentage is the technology of 41% glyphosate isopropylamine salt water solution, not by producing the former powder of glyphosate, but directly synthetic mass percent is the female medicine of 46% glyphosate isopropyl amine salt behind the air oxidation reaction, making mass percent after the filtration of active charcoal is 41% glyphosate isopropylamine salt water solution, thereby reduces production costs.

Claims (1)

1. a mass percent is the manufacturing process of 41% glyphosate isopropylamine salt water solution, and it comprises following steps:

(1) the raw material iminodiacetonitrile is added NaOH and water and carries out alkaline hydrolysis after, add PCl ₃Carry out acidification reaction with HCl, rear adding HCHO carries out condensation reaction, adds subsequently NaOH and water and carries out crystallization, adds water filtration again and obtains the intermediate PMIDA;

(2) the intermediate PMIDA obtains glyphosate and Mixture of Activated Carbon by air oxidation under the effect of activated-carbon catalyst, and described glyphosate and Mixture of Activated Carbon obtain glyphosate and activated charcoal solid mixture by decrease temperature crystalline, isolated by filtration;

(3) the isolated glyphosate of decrease temperature crystalline in the step (2) and activated charcoal solid mixture being added water and isopropylamine, to be deployed into mass percent be 46% the female medicine of glyphosate isopropyl amine salt, the mixture of glyphosate mother solution and active carbon, the mixture of gained was through filtering after allotment was finished, obtain mass percent and be 46% the female medicine of glyphosate isopropyl amine salt, glyphosate mother solution and active carbon, be that the female medicine of 46% glyphosate isopropyl amine salt adds water to be deployed into mass percent be 41% glyphosate isopropylamine salt water solution at last with mass percent, glyphosate mother solution and washing active carbon that filtration is obtained, filter, the glyphosate mother solution that obtains returns with isopropylamine and repeats allotment, and active carbon returns recycled in the step (2) as catalyzer.