Unlock instant, AI-driven research and patent intelligence for your innovation.

Purification method of 1,1,3-trichloroacetone and application thereof

A technology of trichloroacetone and purification method, applied in the separation/purification of carbonyl compounds, organic chemistry and other directions, can solve problems such as potential safety hazards and potential quality risks of folic acid

Inactive Publication Date: 2019-03-26
江西天新药业股份有限公司
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a 1,1,3-three The purification method of chloroacetone and its application, the method does not introduce organic solvents, and the high-chlorine impurities are removed during the purification process, there is no quality risk to the quality of folic acid, and the purification method uses water as the crystallization solvent, and the purified The aqueous solution of 1,1,3-trichloroacetone is directly used in the production of folic acid, which reduces side reactions, improves the yield of folic acid, and can obtain high-quality folic acid; in addition, the purification method involves layered extraction, crystallization Filtration and other operations can be carried out in a closed system, the working environment is friendly, and the generation of waste water is greatly reduced, and waste organic solvents and organic waste gases are not generated.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] This example illustrates 1,1,3-trichloroacetone prepared by the purification method of the present invention.

[0047] The purification process is carried out in a 50-liter reactor with a filter sieve plate at the bottom.

[0048] First, mix 20Kg of 1,1,3-trichloroacetone with a purity of 65% by weight and 10Kg of water in a reactor, and stir at 24°C for 12 minutes, wherein the stirring rate is 200r / min. During the stirring process Water was added, and the water was added at a rate of 300 ml / min, then the mixture was allowed to stand for 10 minutes, and the lower oil layer was separated to remove high-chlorine impurities;

[0049] Next, lower the temperature of the layered upper layer solution to 5° C., and stir for 2 hours at a stirring rate of 100 r / min;

[0050] Then, use nitrogen pressure filtration, the pressure is 0.1Mpa, directly pass through the sieve plate at the bottom of the reactor to obtain solid crystals, and then spray and wash with 1Kg of cold water at ...

Embodiment 2

[0054] This example illustrates 1,1,3-trichloroacetone prepared by the purification method of the present invention.

[0055] The purification process is carried out in a 50-liter reactor with a filter sieve plate at the bottom.

[0056] First, mix 20Kg of 1,1,3-trichloroacetone with a purity of 50% and 4Kg of water in a reactor, and stir at 45°C for 15 minutes, wherein the stirring speed is 300r / min, and during the stirring process, add Water, the water was added at a rate of 300 ml / min, then the mixture was allowed to stand for 15 minutes, and the lower oil layer was separated to remove high-chlorine impurities;

[0057] Next, lower the temperature of the layered upper layer solution to 20° C., and stir for 0.5 hours at a stirring rate of 200 r / min;

[0058] Then, use nitrogen pressure filtration, the pressure is 0.2Mpa, directly pass through the sieve plate at the bottom of the reaction kettle to obtain solid crystals, and then spray and wash with 1Kg of cold water at 25°C...

Embodiment 3

[0062] This example illustrates 1,1,3-trichloroacetone prepared by the purification method of the present invention.

[0063] The purification process is carried out in a 50-liter reactor with a filter sieve plate at the bottom.

[0064] First, mix 20Kg of 1,1,3-trichloroacetone with a purity of 60% and 40Kg of water in a reactor, and stir at 15°C for 30 minutes, wherein the stirring speed is 100r / min, and during the stirring process, add Water, the water was added at a rate of 500 ml / min, then the mixture was allowed to stand for 30 minutes, and the lower oil layer was separated to remove high-chlorine impurities;

[0065] Next, lower the temperature of the upper layer solution after stratification to 10° C., and stir for 10 hours at a stirring rate of 100 r / min;

[0066] Then, use nitrogen pressure filtration, the pressure is 0.2Mpa, directly pass through the sieve plate at the bottom of the reaction kettle to obtain solid crystals, and then spray and wash with 1Kg of cold ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention belongs to the technical field of compound purification, and in particular relates to a purification method of 1,1,3-trichloroacetone and an application thereof. The method comprises thefollowing steps: (1) mixing a 1,1,3-trichloroacetone coarse product with water and leaving the mixture to stand; (2) recrystallizing the upper solution left to stand; and (3) filtering and washing the recrystalized solid crystals, wherein the weight ratio of dosages of the 1,1,3-trichloroacetone coarse product and water is 1: (0.1-2). The method is environment-friendly to work, reduces generationof wastewater greatly and is free of waste organic solvents and organic exhaust gas. In addition, an aqueous solution of 1,1,3-trichloroacetone purified by the purification method is directly used for producing folic acid and reduces side reactions, can improve the total yield of folic acid by 5wt% and the purity is over 99.2wt%, and high quality folic acid can be obtained.

Description

technical field [0001] The invention belongs to the technical field of compound purification, relates to the technical field of organic compound purification, and specifically relates to a method for purifying 1,1,3-trichloroacetone. The aqueous solution of 1,1,3-trichloroacetone purified in the present invention is directly used for The production of folic acid improves the yield of folic acid and at the same time can obtain high-quality folic acid. Background technique [0002] 1,1,3-Trichloroacetone is an important industrial raw material, which can be used in the synthesis of various raw materials and intermediates. 1,1,3-Trichloroacetone is also an important raw material for the production and synthesis of folic acid, namely vitamin B9. At present, the industrial production of 1,1,3-trichloroacetone is mainly prepared by chlorination of acetone as a raw material with chlorine gas, and the production process obtains a 1,1,3-trichloroacetone content of 50-65% by weight. ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/78C07C49/16
CPCC07C45/78C07C49/16
Inventor 李生炎熊文泉张宏伟吴安飞郭军
Owner 江西天新药业股份有限公司