Process

A technology of reaction mixture and tetrachloropropane, applied in the field of compositions containing such compounds, can solve the problems of difficult separation, reduced catalyst effectiveness or working life, etc., and achieve the effect of continuous production

Inactive Publication Date: 2017-08-01
SPOLEK PRO CHEMICKOU A HUTNI VYROBU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In particular, the presence of impurities, especially those that are not easily separated from the target compound (e.g. due to close or higher boiling points) or reduce the effectiveness or working life of catalysts used in downstream processes can be problematic

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0407] Example 1 - Demonstration of Catalytic Capability of Recovered Catalyst Using Water Treatment.

[0408] Ethylene and carbon tetrachloride are reacted to produce 1,1,1,3-tetrachloropropane in the presence of a catalyst i) recovered from the reaction mixture using conventional distillation techniques, or ii) using the method described herein for The inventive water treatment step of the catalyst is recovered from the reaction mixture. The reaction mixture additionally contains 1,1,1,3-tetrachloropropane (present in the recycle stream) and tetrachloropentane (usually formed as a by-product in the presence of a telomerization reaction between carbon tetrachloride and ethylene chlorinated alkanes impurity).

[0409] These test examples show that catalyst performance is significantly higher using a water treatment step to recover catalyst compared to catalyst recovered using conventional distillation techniques.

[0410] The progress of the reaction was monitored using gas ...

Embodiment 1-2

[0418] 90.1 g containing 63.7% TeCPa, 22.8% TeCPna and 7.49% Bu 3 PO 4 The distillation residue was extracted with 370 g of 5% HCl. The bottom organic layer was filtered and mixed with 400 g TeCM. Then, the mixture was introduced into an autoclave to which 5.0 g of iron had been added. After rinsing with ethylene, the mixture was heated to 110°C in an autoclave. At this temperature and an ethylene pressure of 9 bar, the reaction mixture was allowed to react for 4.5 hours. The first sample was taken after 3 hours. The concentration of residual TeCM at the end of the experiment was 5.5% (24.6% after 3 hours).

Embodiment 1-4 and 1-5

[0422] Examples 1-4 and 1-5 were performed using the same conditions as used in Example 1-2, except that different concentrations of carbon tetrachloride and tributyl phosphate were used.

[0423] The results of Comparative Example 1-1 and Example 1-2, and Comparative Example 1-3 and Examples 1-4 and 1-5 are shown in the following table. It can be seen that in Examples 1-2, 1-4 and 1-5, tetrachloropropane converted to 1,1,1,3-tetrachloropropane The percentage of chlorinated carbons was significantly higher, suggesting that the conduct of the water treatment step has a profoundly positive effect on the system when the catalyst is recovered. This is due to the high activity of the catalyst recovered from the distillate residue, and possibly also due to the removal of impurities (such as oxygen-containing impurities) from the reaction mixture that might otherwise retard the reaction.

[0424]

[0425] Continuous configuration:

[0426] The same stainless steel autoclave as d...

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Abstract

Disclosed is a process for preparing a highly pure 1,1,1,2,3-pentachloropropane product. The method comprises 1-a) providing a reaction mixture comprising ethylene, carbon tetrachloride and a catalyst in a principal alkylation zone to produce 1,1,1,3-tetrachloropropane in the reaction mixture; 1-b) treating the reaction mixture obtained in step 1-a) to obtain a 1,1,1,3-tetrachloropropane feedstock; 2-a) contacting the 1,1,1,3-tetrachloropropane feedstock with a catalyst in a dehydrochlorination zone to produce a reaction mixture comprising 1,1,1,3-tetrachloropropane and 1,1,3-trichloropropene; 2-b) treating the reaction mixture obtained in step 2-a) to obtain a 1,1,3-trichloropropene feedstock; 3-a) contacting the 1,1,3-trichloropropene feedstock with chlorine in a reaction zone to produce a reaction mixture containing 1,1,1,2,3-pentachloropropane and 1,1,3-trichloropropene, the reaction zone being different from the dehydrochlorination zone; and 3-b) treating the reaction mixture obtained in step 3-a) to obtain the highly pure 1,1,1,2,3-pentachloropropane product.

Description

technical field [0001] The present invention relates to a process for the preparation of very high purity 1,1,1,2,3-pentachloropropane, as well as compositions comprising such compounds. Background technique [0002] Haloalkanes are useful in a range of applications. For example, halogenated hydrocarbons are widely used as refrigerants, blowing agents, and blowing agents. The use of chlorofluoroalkanes grew exponentially during the second half of the twentieth century until the 1980s, when concerns were raised about their environmental impact, especially with regard to the depletion of the ozone layer. [0003] Subsequently, HFCs such as perfluorocarbons and hydrofluorocarbons have been used in place of chlorofluoroalkanes, but recently environmental concerns have been raised regarding the use of these compounds and legislation has been enacted in the EU and elsewhere to reduce their use . [0004] Emerging environmentally friendly halocarbons are emerging and being inves...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/02C07C19/01C07C17/25C07C17/20C07C21/18C07C21/04
CPCC07C17/02C07C17/20C07C17/25C07C17/275C07C19/01C07C21/04C07C19/08C07C19/10C07C21/18C07C17/04C07C17/38C07C17/383Y02P20/582C07C17/266C07C17/087
Inventor 兹德涅克·昂德鲁斯帕维尔·库比切克卡雷尔·菲拉斯彼得·斯拉德切克
Owner SPOLEK PRO CHEMICKOU A HUTNI VYROBU
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