CN105949051A

CN105949051A - Crystalizing process of chloroacetic acid

Info

Publication number: CN105949051A
Application number: CN201610342723.9A
Authority: CN
Inventors: 范红奎; 徐书建; 韩志涛; 孙晓峰; 韩金豹; 张晓林; 韩根长
Original assignee: Henan Hdf Chemical Co Ltd
Current assignee: Henan Hdf Chemical Co Ltd
Priority date: 2016-05-23
Filing date: 2016-05-23
Publication date: 2016-09-21

Abstract

The invention discloses crystalizing process of chloroacetic acid and relates to the field of chemical raw material production. The crystalizing process includes: adding acetic acid and sulfur powder into a reaction kettle, and feeding chlorine when the temperature of the reaction kettle rises to 85-90 DEG C; ending the reaction to be ready for crystallization when the temperature of liquid in the reaction kettle is 80 DEG C; pumping materials, with qualified ratio, of a chlorination reaction kettle or crude chloroacetic acid reaction kettle into a 2000L crystallization reaction kettle, adding mother solution, stirring, adding seed crystal and clear water, keeping constant temperature for 4 hours, pumping the mother solution into a mother solution reaction kettle in a vacuum manner, taking out, and packaging. By the crystalizing process, the problems that existing chloroacetic acid crystalizing process is long in crystalizing time, low in efficiency, small and uneven in product particle size, and the like are solved, product particle size can be controlled effectively, and product quality and quality stability can be increased.

Description

A kind of chloroacetic crystallization processes

Technical field

The present invention relates to industrial chemicals production field, be specifically related to a kind of chloroacetic crystallization processes.

Background technology

Monoxone is a kind of important industrial chemicals and intermediate, and range of application constantly expands, and has been directed to pesticide, doctor The various aspects such as medicine, dyestuff, organic synthesis, the monoxone extensive application when synthesizing many important Organic chemical products, for it The exploitation of downstream derivative thing and use provide unprecedented condition, development prospect is the most wide, but due to monoxone Production technology many employings sulfur method or acetic anhydride method technique, Technology falls behind, and unit scale is little, especially crystallizing chloroacetic acid mistake Journey, continues to use the process units level of the eighties in last century always, belongs to intermittently operated, there is crystalline particle granularity little and can not Control, monoxone purity is difficult to improve, the problems such as quality is on the low side, more cannot meet food stage glycine and carboxymethyl cellulose is raw Produce the required chloroacetic prescription of food stage.

Improving the important step that monoxone product quality is monoxone industry development, crystallization workshop section is to determine monoxone product The key factor of quality, at present, domestic primary crystalline method is different with the fusing point of dichloroacetic acid by chloroacetic acid, uses Batch (-type) suspension decrease temperature crystalline technology makes chloroacetic acid crystallize, and this method for crystallising was for up to more than 30 hours, and temperature Experienced by from 70 DEG C to 25 DEG C be widely varied, crystal grain is little and uneven, and the product quality of different batches is inconsistent, because of This finds a kind of efficient and rational method for crystallising is the main path improving product quality.

Summary of the invention

Instant invention overcomes above-mentioned shortcoming, and a kind of chloroacetic crystallization processes is provided.

It is an object of the invention to provide a kind of chloroacetic crystallization processes, comprise the following steps: by acetic acid and sofril Put in reactor in the ratio of 1:1 ~ 1.2, when question response still is warming up to 85 DEG C ~ 90 DEG C, be passed through chlorine；When liquid in reactor When temperature is 80 DEG C, reaction reaches terminal, and extraction material is to monoxone crude product reactor, to be crystallized；By chlorinating container or chlorine The material that acetic acid crude product reactor proportion is qualified is evacuated to 2000 L crystallization reaction stills, adds mother solution, stirring, rises high-temperature to 80 DEG C, add crystal seed 3.5 kg and add clear water 4 kg, after constant temperature 4h, the product of advantages of good crystallization being put into nutsch filter, with vacuum by mother Liquid is drawn in mother solution reactor, and now, crystallizing chloroacetic acid is stayed in nutsch filter, takes out and packs.

Preferably, the mass ratio of described acetic acid and sofril is 1:1.1.

Preferably, in described chloroacetic crystallization reaction, temperature of reaction kettle is 88 DEG C.

Preferably, described acetic acid and sofril are AG raw material.

Preferably, described packaged crystal is positioned at shady and cool ventilation.

The invention has the beneficial effects as follows: the chloroacetic crystallization processes in the present invention, solve existing crystallizing chloroacetic acid work Crystallization time length that skill exists, efficiency is low, granularity is little and the problem such as uneven, it is possible to effectively controls the size of product granularity, carries The quality of high product and the stability of quality, low temperature, thermostatical crystallization, reduce the energy expenditure needed for monoxone cooling, shorten knot The brilliant time, improve crystalline rate.

Detailed description of the invention

Embodiment 1

Acetic acid 50 g and sofril 50 g is put in reactor, when question response still is warming up to 85 DEG C, is passed through chlorine；Work as reaction When in still, temperature of liquid is 80 DEG C, reaction reaches terminal, and extraction material is to monoxone crude product reactor, to be crystallized；Chlorination is anti- Answer still or the qualified material of monoxone crude product reactor proportion to be evacuated to 2000 L crystallization reaction stills, add mother solution, stirring, rise high temperature Degree, to 80 DEG C, adds crystal seed 3.5 kg and adds clear water 4 kg, after constant temperature 4h, the product of advantages of good crystallization being put into nutsch filter, with very Empty by liquor abstraction to mother solution reactor, now, crystallizing chloroacetic acid is stayed in nutsch filter, takes out and packs.

Embodiment 2

Acetic acid 50 g and sofril 50 g is put in reactor, when question response still is warming up to 88 DEG C, is passed through chlorine；Work as reaction When in still, temperature of liquid is 80 DEG C, reaction reaches terminal, and extraction material is to monoxone crude product reactor, to be crystallized；Chlorination is anti- Answer still or the qualified material of monoxone crude product reactor proportion to be evacuated to 2000 L crystallization reaction stills, add mother solution, stirring, rise high temperature Degree, to 80 DEG C, adds crystal seed 3.5 kg and adds clear water 4 kg, after constant temperature 4h, the product of advantages of good crystallization being put into nutsch filter, with very Empty by liquor abstraction to mother solution reactor, now, crystallizing chloroacetic acid is stayed in nutsch filter, takes out and packs.

Embodiment 3

Acetic acid 50 g and sofril 60 g is put in reactor, when question response still is warming up to 90 DEG C, is passed through chlorine；Work as reaction When in still, temperature of liquid is 80 DEG C, reaction reaches terminal, and extraction material is to monoxone crude product reactor, to be crystallized；Chlorination is anti- Answer still or the qualified material of monoxone crude product reactor proportion to be evacuated to 2000 L crystallization reaction stills, add mother solution, stirring, rise high temperature Degree, to 80 DEG C, adds crystal seed 3.5 kg and adds clear water 4 kg, after constant temperature 4h, the product of advantages of good crystallization being put into nutsch filter, with very Empty by liquor abstraction to mother solution reactor, now, crystallizing chloroacetic acid is stayed in nutsch filter, takes out and packs.

The ultimate principle of the present invention and principal character and advantages of the present invention, the technology of the industry have more than been shown and described Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and description The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become Change and improvement both fall within scope of the claimed invention, claimed scope by appending claims and Equivalent defines.

Claims

A kind of chloroacetic crystallization processes the most as claimed in claim 1, it is characterised in that comprise the following steps:

Acetic acid and sofril are put in reactor in the ratio of 1:1 ~ 1.2, when question response still is warming up to 85 DEG C ~ 90 DEG C, is passed through Chlorine；When in reactor, temperature of liquid is 80 DEG C, reaction reaches terminal, and extraction material, to monoxone crude product reactor, is waited to tie Brilliant；Material qualified to chlorinating container or monoxone crude product reactor proportion is evacuated to 2000 L crystallization reaction stills, adds mother solution, Stirring, liter high-temperature, to 80 DEG C, adds crystal seed 3.5 kg and also adds clear water 4 kg, after constant temperature 4h, put into by the product of advantages of good crystallization Nutsch filter, with vacuum by liquor abstraction to mother solution reactor, now, crystallizing chloroacetic acid is stayed in nutsch filter, takes out packaging i.e. Can.
The chloroacetic crystallization processes of one the most according to claim 1, it is characterised in that described acetic acid and the matter of sofril Amount ratio is 1:1.1.
The chloroacetic crystallization processes of one the most according to claim 1, it is characterised in that described chloroacetic crystallization reaction Middle temperature of reaction kettle is 88 DEG C.
The chloroacetic crystallization processes of one the most according to claim 1, it is characterised in that described acetic acid and sofril are AG raw material.
The chloroacetic crystallization processes of one the most according to claim 1, it is characterised in that described packaged crystal is placed At shady and cool ventilation.