Method for preparing chlorohydrocarbon

A technology for chlorinated hydrocarbons and chlorinated alkanes, which is applied in the field of telomerization to prepare chlorinated hydrocarbons, which can solve problems such as poor solubility of catalysts, blockage of equipment and pipelines, and complicated operations, so as to facilitate continuous industrial production and improve reaction efficiency. The effect of speed and simple equipment structure

Active Publication Date: 2006-04-26
BEIJING YUJI SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are that the amount of catalyst and co-catalyst required for the reaction is relatively large, there are many wastes that are not easy to recycle during the post-treatment process, the solubility of the catalyst is not good, it is difficult to form a homogeneous phase, the reaction efficiency is not high, and the time required for the reaction is relatively long. long
[0003] Patent US6313360 reports adding iron powder and tributyl phosphate to catalyze the preparation of HCC-240fa in the reaction. The reaction time is as long as 9 hours. The problem of uniform dispersion of iron powder in the solution and blockage of equipment and pipelines during catalyst recovery is not easy to solve
[0004] The preparation process reported in the above-mentioned documents is all completed in a polytetrafluoroethylene-lined autoclave, the equipment manufacturing cost is high, the operation is complicated, the reaction time is long (the residence time of the material is several hours or even longer), and the production efficiency is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: Add 2.24 grams of dimethylformamide (DMF), 46.85 grams of carbon tetrachloride, and 25.7 grams of vinyl chloride successively in a stainless steel container with a valve that is equipped with a volume of 120 milliliters, shake well, and use it as a mixed raw material; A 30 cm long, 1 / 8 inch diameter PFE tube was used as the reactor, and 304 stainless steel annular packing was placed inside, and heated to 100°C in an electric furnace. With the flow rate of 0.2 ml / min, mixed raw materials are squeezed into the reactor with a metering pump. After the stable reaction pressure was stabilized, the reaction product was collected in a cold trap, and the product composition was measured by GC, wherein the selectivity of HCC-240fa was 98.6%. Based on carbon chloride, the yield of HCC-240fa was 62.5%.

Embodiment 2

[0021] Embodiment 2: Add DMF0.70 gram, carbon tetrachloride 52.57 grams, vinyl chloride 17.49 grams successively in the stainless steel container that volume is 120 milliliters that valve is housed, shake shake, as mixing raw material; Use length 30 centimeters, diameter A 1 / 8-inch PFE tube is used as a reactor, and 316 stainless steel annular packing is placed inside, and heated to 120°C in an electric furnace. Use a metering pump to inject the mixed raw materials into the reactor at a flow rate of 0.2 ml / min. The stable reaction pressure is 0.50 MPa. After the reaction is stable, the cold trap collects the reaction product, and the product composition is determined by GC. The selectivity of HCC-240fa is 99.2 %, based on carbon tetrachloride, the yield of HCC-240fa is 67.1%.

Embodiment 3

[0022] Embodiment 3: Feed amount, reactor and filler were carried out according to Embodiment 2, and the reactor was heated to 90° C. in an electric furnace. Use a metering pump to inject the mixed raw materials into the reactor at a flow rate of 0.4 ml / min. The stable reaction pressure is 0.40 MPa. After the reaction is stable, the cold trap collects the reaction product, and the product composition is determined by GC. The selectivity of HCC-240fa is 97.1 %, based on carbon tetrachloride, the yield of HCC-240fa is 60.3%.

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Abstract

The present invention relates to chlorohydrocarbon preparing process, and is especially one telomerization process of preparing chlorohydrocarbon in the molecular expression CCl3CH2CHnClm, where n is 0, 1 or 2, and m=3-n, inside a tubular reactor, with chloroalkane or chloroalkene as main material and in the presence of composite Fe, Cr and Ni metal catalyst and dimethyl formamide as co-catalyst. The reacted mixture may be distilled to recover un-reacted material and co-catalyst and is decompression distilled to obtain final chlorohydrocarbon product. The telomerization process is simple, high in reaction efficiency and suitable for continuous industrial production.

Description

technical field [0001] The present invention relates to molecular formula is CCl 3 CH 2 CH n Cl m , (where n is 0, 1 or 2, m=3-n), a preparation method of chlorinated hydrocarbons, in particular to a method for preparing chlorinated hydrocarbons by telomerization reaction of chlorinated alkanes and olefins under the action of a catalyst. Background technique [0002] The chlorinated hydrocarbon can produce 3,3,3-trifluoropropene, 1,1,1,3,3-pentafluoropropane (HFC-245fa), 1,1,1,3,3,3- Hexafluoropropane (HFC-236fa); 3,3,3-trifluoropropene is an important intermediate of fluorine-containing rubber; the ODP value of HFC-245fa and HFC-236fa is zero, and it is an important substitute for Freon. Foaming, cleaning, fire extinguishing and other industries. Preparation of CCl in the prior art 3 CH 2 CH n Cl m The most common reaction is telomerization, that is, the addition of halogenated hydrocarbons to olefins, and try to control the addition of single molecules to reduce t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/08C07C19/01
Inventor 张小玲鲍鹏陈飞
Owner BEIJING YUJI SCI & TECH
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