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Method for producing dichlorhydrin by means of glycerin hydrochlorination

A technology of dichloropropanol and hydrochlorination, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve the problems of difficult wastewater treatment, cumbersome operation, low recovery rate, etc., and achieve low production cost, The effect of simple process and easy separation

Active Publication Date: 2012-06-13
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The recovery rate of this organic catalyst is low, and catalysts such as carboxylic acid, carboxylic acid anhydride, and carboxylic acid chloride are easy to react with glycerin and cause the catalyst to lose activity
[0004] Chinese patent CN101029000A then adopts aliphatic nitrile or aromatic nitrile as catalyzer, but before passing into hydrogen chloride gas in glycerol, catalyst organic nitrile needs to be activated at reaction temperature in 30% hydrochloric acid solution, and operation is loaded down with trivial details, and organic nitrile catalyst is activated after reaction. The raffinate contains highly toxic CN-, causing serious environmental pollution and difficult wastewater treatment
[0005] Chinese patent CN101215223A discloses a method for compounding polyaryl ether sulfone ether ketone ketone resin with carboxyl side groups and carboxylic acid to catalyze the highly selective synthesis of dichloropropanol from glycerin. Although the resin catalyst can be reused, the preparation of the resin catalyst higher cost
[0007] Above-mentioned method that adopts glycerin as raw material to adopt organic acid, organic nitrile, phosphomolybdic acid etc. to catalyze the synthesis of dichloropropanol all exists that catalyst easily generates various by-products with raw material, causes separation process complexity, and catalyst recovery difficulty is big, makes production High cost and high environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 50g of commercially available 280-200mesh coal-based powdered activated carbon, add 50g of commercially available hydrogen peroxide (the mass fraction of hydrogen peroxide is 27%), heat to 70°C, stir for 12h, filter after cooling, and wash the activated carbon with deionized water to medium properties, vacuum-dried at 80°C for 10 hours, and placed in a desiccator for later use after drying. The particle size of the hydrogen peroxide modified activated carbon does not change, and the specific surface area is 500m2 measured by the BET method 2 / g, pore volume 0.65m 3 / g.

Embodiment 2

[0029] Weigh 50g of commercially available 200-mesh woody powdery activated carbon, add 200g of commercially available concentrated hydrochloric acid (hydrochloric acid mass fraction is 36.5%), heat to 60°C, stir for 6h, filter after cooling, wash the activated carbon to neutral with deionized water, Vacuum dry at 100° C. for 8 hours, and put it in a desiccator for later use after drying. The particle size of activated carbon modified by concentrated hydrochloric acid does not change, and the specific surface area measured by BET method is 1000m 2 / g, pore volume 0.7m 3 / g.

Embodiment 3

[0031] Weigh 50 g of commercially available coal-based columnar activated carbon with a diameter of 1.5 mm, add 250 g of commercially available concentrated sulfuric acid (the mass fraction of sulfuric acid is 98%), heat to 60 ° C, stir for 4 h, filter after cooling, and wash the activated carbon with deionized water to medium properties, vacuum-dried at 100°C for 6 hours, and placed in a desiccator for later use. The particle size of activated carbon modified by concentrated sulfuric acid does not change, and the specific surface area measured by BET method is 800m 2 / g, pore volume 0.7m 3 / g.

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Abstract

The invention belongs to the field of chemical engineering, and discloses a catalyst and a method for producing dichlorhydrin by means of glycerin hydrochlorination. The method includes that the dichlorhydrin can be efficiently produced by means of reaction of glycerin and hydrogen chloride under the action of activated carbon or an activated carbon catalyst subjected to modification treatment of hydrogen peroxide, sulfuric acid and the like. The catalyst which is solid is high in activity, easy to be separated from a product and recyclable. The method has the advantages of simplicity in process and low production cost.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a catalyst and a method for producing dichloropropanol by hydrochlorination of glycerol, in particular to a method for producing dichloropropanol from glycerin under the action of an activated carbon catalyst. Background technique [0002] Dichloropropanol, also known as dichloroglycerin, is an important raw material for the synthesis of epichlorohydrin, crosslinking agent, water treatment agent, and medicine. The production methods of dichloropropanol mainly include propylene high-temperature chlorination method, propylene acetate method, and glycerin hydrochlorination method. The high-temperature chlorination of propylene and the propylene acetate method use propylene, a product of petroleum cracking, as the starting material. With the shortage of petroleum resources and the soaring price of petroleum, the production cost is getting higher and higher. In recent years, due to the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/36C07C29/62B01J21/18
Inventor 汤吉海乔旭王卫东周峰陈献崔咪芬杨雷周晓丽
Owner NANJING TECH UNIV