Method for preparing tetrachloroethylene by liquid-phase catalysis of pentachloroethane

A technology of tetrachlorethylene and pentachloroethane, which is applied in the field of preparation of organic chlorinated hydrocarbons, can solve the problems of expensive catalysts, high production costs, and high material requirements, and achieve flexible production methods, convenient operation, and high material utilization. Effect

Active Publication Date: 2011-12-28
江西国宏化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the material requirements of gas-phase catalytic cracking equipment are high, the investment is huge, the reaction temperature is as high as 205 ° C ~ 290 ° C, the energy consumption is large, the catalyst is expensive, and the production cost is high.

Method used

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  • Method for preparing tetrachloroethylene by liquid-phase catalysis of pentachloroethane

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Experimental program
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Effect test

Embodiment 1

[0026] Embodiment 1: batch method

[0027] Reactor capacity is 4 liters, in reactor, add the pentachloroethane 2800ml (4662 grams) of purity 98%, by weight percentage, pentachloroethane: catalyst=1: 0.0031~0.005, add aluminum chloride 20.5 grams, Potassium chloride 2.3 grams, use a heating tube to heat up to 120 ° C, the pressure gauge is 0.01Mpa, reflux for 10 hours, monitor the composition of the reaction solution every 2 hours, when the pentachloroethane is less than 1%, the reaction is terminated, and the tail gas hydrogen chloride is recovered with water , Change the distillation operation to obtain 2278ml (3693 grams) of tetrachloroethylene crude product, through gas chromatography analysis, tetrachloroethylene content 95.01% in the sample, conversion rate 98.80%, selectivity 94.80%, yield 93.66%.

Embodiment 2

[0028] Embodiment 2: continuous method

[0029]Reactor capacity is 4 liters, and in reactor, adding purity is 2800ml (4520 grams) of tetrachlorethylene of 99.8% and is mother liquor, adds catalyzer by 1: 0.001~0.003 with raw material weight percentage, aluminum chloride 10.6 grams, cesium chloride 2.7 grams, heating the reaction solution with a heating tube to heat up to 80°C, adding pentachloroethane with a purity of 98%, pentachloroethane dripping at a flow rate of 1ml per minute, and continuing to heat up for 20 to 30 minutes. After the reaction temperature reaches 120°C, The pressure gauge is 0.01Mpa. Increase the amount of pentachloroethane added to 7.2ml per minute, keep the volume of the amount of pentachloroethane added and the amount of tetrachlorethylene distilled equal, and also keep the content of the catalyst unchanged, and absorb the hydrogen chloride in the tail gas with water for 5 hours Stop adding raw material afterward, total addition 2218ml (3693 grams), r...

Embodiment 3

[0030] Embodiment 3: batch method

[0031] at 30 meters 3 21 m of pentachloroethane with a purity of 98% was added to Reactor 1 3 (34.965 tons), add 119 kilograms of aluminum chloride, 21 kilograms of potassium chloride catalyzers by weight percentage, stir, heating pipe 5.6 logical steam is warming up to 120 ℃, gas phase outlet 8 accesses hydrochloric acid device, reflux reaction 12 hours, every Monitor the composition of the reaction solution for 2 hours, the content of pentachloroethane is less than 1% as the end point, change the distillation operation, and finally obtain 16.73 meters of crude tetrachlorethylene 3 (27.023 tons), analyzed by gas chromatography, the tetrachloroethylene content in the sample was 95.27%, the conversion rate was 98.70%, the selectivity was 92.85%, and the yield was 91.64%.

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Abstract

The invention relates to a method for preparing tetrachloroethylene through pentachloroethane liquid-phase catalysis, which comprises the following steps of: an intermittent method: by using high-purity pentachloroethane as a raw material, adding a metal halide as a catalyst according to the percentage by weight, stirring and heating in a reactor, and intermittently reacting and distilling under a normal pressure to obtain a crude tetrachloroethylene product; or a continuous method: by using the prepared crude tetrachloroethylene product as a mother solution, adding the metal halide as the catalyst, stirring, heating, then adding the high-purity pentachloroethane, maintaining the reaction, then heating to prepare the crude tetrachloroethylene product, and continuously adding the high-purity pentachloroethane to continuously produce the crude tetrachloroethylene products with the same volume; and carrying out water-alkali washing for the crude products prepared by the two methods to be neutral, separating, drying and rectifying to obtain a tetrachloroethylene finished product. The environmental-protection difficult problem of serious environmental pollution brought by traditional calcium-hydroxide saponification is radically solved, particularly the usage amount of the catalyst is small in the continuous method, materials are continuously fed and produced, the method is simpler and more labor-saving to operate, the cost is low, the method is suitable for large-batch production, the utilization ratio of the materials is high, and the purity of the prepared product reaches up to more than 99.8 percent.

Description

technical field [0001] The invention relates to a method for preparing organic chlorinated hydrocarbons, in particular to a method for preparing tetrachloroethylene by liquid-phase catalysis of pentachloroethane using pentachloroethane as an initial raw material. Background technique [0002] Tetrachlorethylene is an important organic chlorinated hydrocarbon, mainly used as organic solvent, dry cleaning agent, metal degreasing agent, and also used as an anthelmintic drug. In addition, tetrachlorethylene can be used as fat extractant, refrigerant F The intermediates of -113, HCFC-123 and HCFC-124 can also be used as the main raw materials for the production of HFC134a and R125, which are substitutes for chlorofluorocarbons. , Reducing the emission of ozone-depleting substances (ODS) is steadily advancing under the synergy of countries all over the world. At present, the refrigerants R22 and R502, which are used in the largest amount in the refrigeration industry, have been c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/12C07C17/25
Inventor 汪国良黄志强
Owner 江西国宏化工有限公司
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