Prepn process of phosphorous acid and lower alkane halide

A technology of chlorinated alkanes and phosphorous acid, which is applied in the preparation of halogenated hydrocarbons, phosphorous acid, chemical instruments and methods, etc., can solve the problems of high cost of raw materials, prone to explosion, large investment in production equipment, etc., and achieve high atom utilization , low chlorine content and simple installation

Inactive Publication Date: 2004-04-07
李建兵
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Avoid the problems of high technical difficulty, large investment in production equipment and high cost of raw materials for the synthesis of low-level chlorinated alkanes (chloromethane, ethyl chloride) by the direct reaction of lower alkyl alcohols (methanol, ethanol, etc.) and hydr...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1: in the reaction kettle with stirrer, one-time addition 1000g methyl alcohol (31.25mol) in the reactor of thermometer, stirs, slowly add concentration again and be the phosphorous trichloride 1439.5g (10.41mol) of 99.5%, the control temperature of reaction is 10-40°C. After reacting for about 3 hours, 1426 g of methyl chloride (with a small compressor and a cryogenic device) were obtained, and the yield was 95%. 98.2% phosphorous acid 850g, the yield is 97.8%.

Embodiment 2

[0037] Embodiment 2: in the reaction kettle with stirrer, one-time addition 962g methyl alcohol (30.06mol) in the reaction kettle of thermometer, stirs, then slowly add concentration dropwise and be the phosphorus trichloride 1439.5g (10.02mol) of 99.5%, the control reaction temperature is 50-80°C. After reacting for about 3 hours, 1480 g of methyl chloride (with a small compressor and a cryogenic device) were obtained, and the yield was 97.6%. Add 60g of hydrochloric acid (content 0.5%) to 825g of phosphorous acid-containing liquid, control the reaction temperature at 90±5°C, stir and keep warm for 2 hours, stir rapidly to promote the escape of methyl chloride, and the reaction is over when no bubbles are generated, and cool to 30°C . After suction filtration, 130 g of mother liquor was obtained, and 750 g of phosphorous acid with a content of 99% was obtained, and the yield was 91%.

Embodiment 3

[0038] Example 3: Add 130 g of the mother liquor of Example 2 to the reaction solution of Example 1, stir and cool to 25° C. for crystallization, and suction filtration to obtain 851 g of phosphorous acid with a content of 99%, and the yield is 99.9%.

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PUM

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Abstract

The present invention is the production process of phosphorous acid and lower alkane halide with phosphorous trichloride and alkyl alcohol (phenol) as material. Phosphorous trichloride and alkyl alcohol (phenol) are reacted to produce phosphorous acid and lower alkane halide. The lower alkane halide is separated via proper method and the product is concentrated and crystallized to obtain phosphorous acid, with the mother liquor being circularly used. The phosphorous acid is used in producing other product. The production process is simple and low in cost.

Description

technical field [0001] The invention relates to a method for preparing phosphorous acid and lower chlorinated alkanes, more specifically a method for producing phosphorous acid by using lower alkyl alcohols and phosphorus trichloride and producing lower chlorinated alkanes by-product. Background technique [0002] There are many ways to produce lower chlorinated alkanes, and the reaction can be carried out in gas phase or liquid phase. Chlorinating agents include chlorine, hydrogen chloride and many organic and inorganic chlorides such as phosgene, phosphorus pentoxide and sulfuryl chloride. The reaction is generally facilitated by the use of heat, light and / or catalysts. [0003] The most commonly used method is through the chlorination of alkanes, especially methyl chloride is an important raw material for organic synthesis, mainly used for the production of organosilicon monomers (ie, methylchlorosilane). At present, the raw material methyl chlo...

Claims

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Application Information

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IPC IPC(8): C01B25/163C07C17/16C07C19/00
Inventor 李建兵
Owner 李建兵
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