Method for producing dichloropropanol

A technology of dichloropropanol and derivatives, which is applied in the field of preparation of dichloropropanol and epichlorohydrin intermediates, can solve the problem of reducing the quality of waste acid, affecting product yield, and unavoidable dichloropropanol product belts. Sour water and other problems, to overcome the effect of product pollution

Inactive Publication Date: 2009-04-01
南通凯塔化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The catalyzers of these patents all adopt acetic acid or volatile larger carboxylic acid as catalyzer, and in the reaction process, part of the catalyst forms an azeotrope with the water, dichloropropanol and HCl generated by the reaction, resulting in a large amount of catalyst and increasing the separation of products. Difficulty, and these catalysts themselves are also solvents, and part of the dichloropropanol product is inevitably brought into the acid water during the separation process, which affects the product yield and

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Heat and stir the mixture of 657kg glycerin and 27kg phosphorous acid at 120°C, then blow anhydrous hydrogen chloride into the mixture at 4.1kmol / h for 2h, 3.2kmol / h for 4h, 2.1kmol / h for 4h, and finally 1.2kmol / h continued for 2 hours, a total of 31.8 kmol of hydrogen chloride was introduced, and the water and dichlorohydrin generated by the reaction were continuously removed during the process, and the conversion rate of glycerin was 99.2%. The total yield of dichloropropanol (1,3-dichloropropanol and 1,2-dichloropropanol) is 93.5%. The phosphorous acid content in the distillate is <0.001%.

Embodiment 2

[0026] Heat and stir the mixture of 709kg glycerin, 22kg phosphorous acid and 14kg adipic acid at 130°C, then blow anhydrous hydrogen chloride into the mixture, 3.8kmol / h for 2h, 3.6kmol / h for 4h, 2.8kmol / h for 2h 4h, the last 1.4kmol / h continued for 2h, a total of 36.0kmol hydrogen chloride was introduced, and the water and dichloropropanol produced by the reaction were continuously removed during the process, and the conversion rate of glycerin was 99.3%. The total yield of dichloropropanol (1,3-dichloropropanol and 1,2-dichloropropanol) is 93.3%. The phosphorous acid content in the distillate is <0.001%.

Embodiment 3

[0028] Heat and stir the mixture of 596kg of glycerin and 25kg of phosphorous acid at 100°C, then add 50kg of 25% hydrochloric acid dropwise, and then raise the temperature to 130°C, then blow anhydrous hydrogen chloride into the mixture at 3.2kmol / h for 2h, 3.0 kmol / h continued for 4h, 2.8kmol / h continued for 4h, and finally 1.4kmol / h continued for 2h. A total of 32.74kmol hydrogen chloride was introduced, and the water and dichloropropanol produced by the reaction were continuously removed during the process. The conversion rate of glycerol was 99.3%. The total yield of dichloropropanol (1,3-dichloropropanol and 1,2-dichloropropanol) is 93.7%. The phosphorous acid content in the distillate is <0001%.

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PUM

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Abstract

The invention provides a method for producing dichloropropanol, a chlorination agent and glycerol are adopted for reaction, and water generated by the reaction is continuously removed under the condition of taking a phosphorous acid derivative or a phosphoric acid derivative or a phosphorus chloride derivative as a catalyst, thereby obtaining the dichloropropanol. The method overcomes the shortcomings of product pollution, great separation difficulty and impact on yield which are caused by volatilization of carboxylic acid catalysts and the shortcomings of high price and lower catalytic efficiency of non-volatile organic acid catalysts in the prior art, reduces the using amount of the catalyst and simultaneously improves the product yield.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a preparation method of an epichlorohydrin intermediate, more specifically a method for preparing dichloropropanol from glycerin. Background technique [0002] Dichloropropanol is an important intermediate in the production of epichlorohydrin, which is an important organic chemical raw material and fine chemical product with a wide range of uses. The epoxy resin prepared from it has the characteristics of strong adhesion, resistance to chemical medium corrosion, low shrinkage, good chemical stability, high impact strength and excellent dielectric properties. It is used in coatings, adhesives, reinforcing materials, Industries such as casting materials and electronic laminates have a wide range of applications. Epichlorohydrin can also be used to synthesize nitroglycerin explosives, glass fiber reinforced plastics, electrical insulation products, surfactants, medicines, pesticides,...

Claims

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Application Information

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IPC IPC(8): C07C31/34C07C29/62
Inventor 成取林姚炎华
Owner 南通凯塔化工科技有限公司
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