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Device and process for preparing 1,1,1,3-tetrachloropropane

A tetrachloropropane and process technology, applied in the field of organic halide preparation, can solve problems such as reducing the amount of gum oil-like substances generated, and achieve the effects of avoiding collisions, avoiding safety risks, and reducing manufacturing costs

Pending Publication Date: 2020-09-15
浙江佳汇新材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the problem of producing gum oil in the process of preparing 1,1,1,3-tetrachloropropane by reacting carbon tetrachloride and ethylene in the prior art, the present invention reduces the amount of gum oil generated by improving the reaction device

Method used

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  • Device and process for preparing 1,1,1,3-tetrachloropropane
  • Device and process for preparing 1,1,1,3-tetrachloropropane
  • Device and process for preparing 1,1,1,3-tetrachloropropane

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Embodiment 1

[0027] A 5000L stainless steel reactor with an aspect ratio of 3, exhaust air, add catalyst ferric chloride 5kg, reduced iron powder 32kg, cocatalyst tributyl phosphite 25kg, carbon tetrachloride 3750kg, feed ethylene through the ethylene feed port , so that the ethylene pressure in the reactor reaches 0.20MPa; start the oil-free ethylene compressor, the pressure difference between the exhaust port and the inlet port is less than or equal to 1.2MPa, and the displacement of the ethylene compressor is 17.5Nm 3 / min, ethylene is drawn from the upper part of the reactor, pressurized by the ethylene compressor, and then pressed into the reactor from the lower part of the reactor, and the ethylene pressed into the reactor is distributed into the reaction system through a gas distributor, which is a multi-layer sintered metal Stencil, average pore diameter 0.45μm, porosity 38%, gas distributor area 65% of the cross-sectional area of ​​the reactor; heat up to 95°C for reaction, supplem...

Embodiment 2

[0029] Control the ethylene pressure in the reactor to be 0.46~0.50MPa, other is the same as embodiment 1, take a sample and carry out gas chromatography analysis, 1,1,1,3-tetrachloropropane 85.4%, carbon tetrachloride 13.9%, secondary addition The by-product is 0.7%, the equivalent carbon tetrachloride conversion rate is 84.0%, and the selectivity of 1,1,1,3-tetrachloropropane is 99.3%.

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Abstract

The invention discloses a reaction device for preparing 1,1,1,3-tetrachloropropane. The reaction device comprises a reaction kettle, wherein an ethylene circulating system is arranged outside the reaction kettle, a gas distributor is arranged at the bottom of the reaction kettle, the ethylene circulating system comprises an ethylene extraction pipe arranged at the upper portion of the reaction kettle, an ethylene press-in pipe arranged at the lower portion of the reaction kettle, and an ethylene compressor arranged between the ethylene extraction pipe and the press-in pipe, and the ethylene press-in pipe is communicated with the gas distributor. The invention also discloses a process for preparing 1,1,1,3-tetrachloropropane by utilizing the reaction device to react carbon tetrachloride with ethylene. By adopting the process provided by the invention, the generation amount of colloidal oily by-products in the process of preparing 1,1,1,3-tetrachloropropane by reacting carbon tetrachloride with ethylene is reduced, the selectivity of the main product 1,1,1,3-tetrachloropropane is improved, the reaction kettle does not need a stirring device, and the pressure of ethylene in the reaction kettle is reduced at a similar reaction rate.

Description

technical field [0001] The invention relates to the field of preparation of organic halides, in particular to a device and a process for preparing 1,1,1,3-tetrachloropropane. Background technique [0002] 1,1,1,3-Tetrachloropropane is the key raw material for the synthesis of trichloropropene and trifluoropropene, and it can also be used in paint removers, degreasers and solvents. The synthesis methods of 1,1,1,3-tetrachloropropane mainly include peroxide method (CA691213A), electromagnetic radiation method (CA807638A), metal complex and cocatalyst method, wherein peroxide method and electromagnetic radiation method are due to the synthesis Low efficiency or harsh reaction conditions are not suitable for industrial production. The method of metal complexes and co-catalysts is suitable for industrialization because of mild reaction conditions and high synthesis efficiency, but it is inevitable to generate gluey oily substances that adhere to the inner wall of the reactor and ...

Claims

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Application Information

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IPC IPC(8): B01J8/08C07C17/275C07C19/01
CPCB01J8/08C07C17/275C07C19/01
Inventor 李家才王亮何邦友
Owner 浙江佳汇新材料有限公司
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