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Process for producing saturated polychloralkane

A technology of polychlorinated alkanes and pentachloropropane, which is applied in the field of preparation of saturated polychlorinated alkanes, can solve complex problems such as processing, and achieve the effects of good reaction selectivity, complete conversion of raw materials, and high purity of products

Inactive Publication Date: 2009-07-29
杨海珍
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process needs to be completed in a special high-pressure reactor, and due to the use of catalyst copper salt and cocatalyst amines, the post-reaction treatment is complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a glass reactor, add 1 kg of carbon trichloride, 0.8 kg of 1,1,1,3-tetrachloropropane, 1.2 kg of trichloromethanesulfonyl chloride, and 14 g of benzoyl peroxide, stir and heat to 80°C , Incubate the reaction for 8 hours. The conversion rate of the raw materials was determined by gas chromatography. The saturated aqueous solution of sodium bisulfite was added to wash twice, 0.5 kg each time, and 1 kg water was added to wash once. The organic phase was distilled to recover carbon trichloride, and the residue was distilled to obtain the product (collected at 178 degrees Distillate). The conversion rate of the raw material 1,1,1,3-tetrachloropropane was 90.4% after analysis. Based on the raw material 1,1,1,3-tetrachloropropane, the selectivity of 1,1,1,3,3-pentachloropropane is 99.0%.

Embodiment 2

[0025] Ethylene glycol dimethyl ether and trifluorotrichloroethane were used as raw materials at a molar ratio of 1:1, and the catalyst was 3.4 g cyclohexanone peroxide. The reaction was carried out using the same steps as in Example 1. After the reaction was completed, The conversion rate of the raw material 1,1,1,3-tetrachloropropane analyzed by gas chromatography was 94.6%. Based on the raw material 1,1,1,3-tetrachloropropane, the selectivity of 1,1,1,3,3-pentachloropropane was calculated to be 99.1%.

Embodiment 3

[0027] In a glass-lined reactor, add 1 kg of chlorobenzene, 0.8 kg of 1,1,1,3-tetrachloropropane, 1.2 kg of dimethylsulfuryl chloride, 0.05 kg of phosphorus pentachloride, and 12.2 of azobisisoheptonitrile. G, stir and react at 0-40°C for 12 hours. The conversion rate of the raw materials was determined by gas chromatography. The saturated potassium thiosulfate aqueous solution was added to wash twice, 0.5 kg each time, and 1 kg water was added to wash once. The organic phase was distilled to recover chlorobenzene, and the residue was distilled to obtain the product. The conversion rate of the raw material 1,1,1,3-tetrachloropropane was 75% after analysis. Based on the raw material 1,1,1,3-tetrachloropropane, the selectivity to 1,1,1,3,3-pentachloropropane is 99.0%.

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PUM

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Abstract

The invention relates to a method for preparing saturated poly-chloralkane in the technical field of industrial organic chemical. The method comprises the steps as follows: 1, 1, 1, 1, 3-tetrachloropropane, inert organic solvent, a catalyst and a chlorinating agent are used as raw materials to prepare 1, 1, 1, 3, 3-pentachloropropane reaction liquid which is washed by reducing saturated aqueous solution; and solvent is distilled and recovered to prepared a pure product of 1, 1, 1, 3, 3-pentachloropropane. Compared with the prior art, the invention has the advantages of less investment on equipment, simple and easy operation, and being fit for mass production, etc. 1, 1, 1, 3, 3-pentafluoropropane (HFC-245fa for short) prepared from the 1, 1, 1, 3, 3-tetrachloropropane can be widely applied to the fields of solvent, cleaning, frothing, refrigerating, gaseous propellant and the like and has very high industrial value.

Description

Technical field [0001] The invention relates to a preparation method in the technical field of industrial organic chemicals, in particular to a preparation method of saturated polychlorinated alkanes. Background technique [0002] 1,1,1,3,3-pentachloropropane (referred to as 1,1,1,3,3-pentachloropropane) is the preparation of hydrofluoroalkane 1,1,1,3,3-pentafluoropropane (referred to as HFC -245fa) raw materials. HFC-245fa has physical properties very similar to monofluorodichloroethane (HCFC-141b) and monofluorotrichloromethane (CFC-11), and the ODP value (atmospheric ozone depletion potential) of HFC-245fa is Zero, there is no potential damage to the atmospheric ozone layer, so HFC-245fa is considered to be an ideal substitute for CFC-141b and CFC-11, which can be widely used in solvents, cleaning, foaming, refrigeration, gas propellants, etc. A new type of environmentally friendly product. The development and preparation of 1,1,1,3,3-pentachloropropane (1,1,1,3,3-pentachlorop...

Claims

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Application Information

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IPC IPC(8): C07C19/01C07C17/10
Inventor 杨海珍
Owner 杨海珍
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