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System for preparing dichloropropanol by autocatalytic reaction of glycerol and hydrogen chloride

A technology of dichloropropanol and hydrogen chloride, applied in the chemical field, can solve the problems of increasing production cost, environmental pollution, increasing catalyst consumption, large catalyst consumption, etc., and achieves elimination of formation of high-boiling by-products and low production cost. , the effect of improving the selectivity of the reaction

Active Publication Date: 2013-07-31
NANTONG TIANSHI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN101029000A then adopts aliphatic nitrile or aromatic nitrile as catalyzer, this method needs to be passed into glycerin before hydrogen chloride gas, at reaction temperature organic nitrile is activated in 30% hydrochloric acid solution, loaded down with trivial details, simultaneously organic nitrile catalyst is in this reaction Under the same conditions, corresponding acids or carboxylic acid esters will also be generated, which will increase the consumption of catalysts.
[0006] The above-mentioned method of using glycerol as raw material and adopting organic acid or organic nitrile to catalyze the synthesis of dichloropropanol all has the problem that the catalyst reacts with the raw material or the product to generate various by-products, which leads to a large consumption of the catalyst, high energy consumption for separation, and increased production capacity. cost and environmental pollution

Method used

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  • System for preparing dichloropropanol by autocatalytic reaction of glycerol and hydrogen chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Add 0.5 mol glycerin (containing 99.5% glycerol) to the reaction device with a rectification column on the top of the bubbler reactor, react at normal pressure and 160°C, and continuously feed hydrogen chloride gas at a rate of 3L / h , continued for 8h, the reflux ratio was 3:1, the conversion rate of glycerol was 100% at the end of the experiment, the selectivity of monochloropropanediol was 46.4%, the selectivity of dichloropropanol was 53.2%, and the selectivity of heavy fraction diglycerol 0.4%.

Embodiment 2

[0040] In a magnetic stirred tank reactor, add 0.5mol glycerol (containing 99.5% glycerol), react under normal pressure and 105°C, and continuously feed hydrogen chloride gas at a rate of 0.6L / h for 50h. At the end of the experiment, glycerol The conversion rate is 89.8%, the selectivity of monochloropropanediol is 74.5%, the selectivity of dichloropropanol is 25.3%, and the selectivity of heavy fraction diglycerol is 0.2%.

Embodiment 3

[0042] Add 0.5 mol glycerin (containing 99.5% glycerol) to the reaction device with a rectification column on the top of the bubbler reactor, react at normal pressure and 140°C, and continuously feed hydrogen chloride gas at a rate of 3L / h , continued for 8h, the reflux ratio was 3:1, the conversion rate of glycerol was 100% at the end of the experiment, the selectivity of monochloropropanediol was 55.6%, the selectivity of dichloropropanol was 44.3%, the selection of heavy fraction diglycerol Sex is 0.1%.

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Abstract

The invention discloses a process for preparing dichloropropanol by an autocatalytic reaction of glycerol and hydrogen chloride. The process comprises the following steps: the glycerol and the hydrogen chloride gas perform the autocatalytic reaction at the temperature of between 105 and 160 DEG C and pressure of between 0.05 and 0.5MPa, and generated water is distilled and removed during the reaction. The invention also discloses a system for preparing the dichloropropanol by the autocatalytic reaction of the glycerol and the hydrogen chloride. The invention adopts the technology of the autocatalytic reaction of the glycerol and the hydrogen chloride without using a catalyst, so that the production cost is remarkably reduced, formation of high boiling side products is eliminated, and the reaction selectivity is improved. The invention has the advantages of simple process and low production cost. The system can ensure that the glycerol is completely converted and greatly improves the selectivity of the dichloropropanol, so that the purity of the finally prepared dichloropropanol is more than 99.5 percent.

Description

[0001] This application is a divisional application of an invention patent application with the filing date: September 9, 2008, the application number: 200810196436.7, and the title: a process and system for preparing dichloropropanol by autocatalytic reaction of glycerin and hydrogen chloride. technical field [0002] The invention belongs to the field of chemical industry, and in particular relates to a process for preparing dichloropropanol through autocatalytic reaction of glycerin and hydrogen chloride and a system thereof. Background technique [0003] Epichlorohydrin is an important raw material for the production of epoxy resin, chlorohydrin rubber, stabilizer, surfactant, flame retardant, oilfield chemicals and other products, and dichloropropanol is a key intermediate for its synthesis. The method for industrially producing dichloropropanol is mainly based on the method described in U.S. Patent No. 4,634,784. Two series steps of high-temperature chlorination of prop...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/36C07C29/62
Inventor 乔旭汤吉海陈献崔咪芬赵镇
Owner NANTONG TIANSHI CHEM
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