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Continuous preparation method for producing chlorohydrocarbon through carbon tetrachloride and olefins

A technology of carbon tetrachloride and chlorinated hydrocarbons, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, and chemical recovery, etc. It can solve the problems of iron powder or iron filler activity, production continuity, destructiveness, and difficulty in removal, etc. problems, to avoid mutual adhesion and agglomeration, improve reaction effect, and improve production efficiency

Active Publication Date: 2016-01-06
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the olefin self-polymer accumulates in the reactor for a long time, it will wrap the iron powder or iron filler, causing the iron powder or iron filler to stick to each other and agglomerate, so it will be very unfavorable to the activity of iron powder or iron filler Impact
Moreover, it is not easy to remove the iron powder or iron filler wrapping sticking to the wall of the kettle or the stirring paddle, which will have a destructive effect on the continuity of production.

Method used

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  • Continuous preparation method for producing chlorohydrocarbon through carbon tetrachloride and olefins
  • Continuous preparation method for producing chlorohydrocarbon through carbon tetrachloride and olefins

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preparation example Construction

[0028] The present invention is a kind of continuous preparation method that is used for carbon tetrachloride and olefin production chlorinated hydrocarbon, comprises the following steps:

[0029] (1) Iron powder or iron filler, catalyst auxiliary agent alkyl phosphate and carbon tetrachloride are continuously added in the first ferrous complex catalyst preparation kettle, and iron filler includes iron material, such as iron ring, Iron wire, iron filings, even stainless steel, carbon steel, etc., as long as they are iron-containing substances, make iron fillers easier to obtain and reduce costs. Catalyst additives are selected from triethyl phosphate, tributyl phosphate, trimethyl phosphate One or more mixtures of alkyl phosphates such as esters and triphenyl phosphate, through the use of catalyst aids, the reaction efficiency is accelerated, and the ratio of the amount of carbon tetrachloride to olefins is 1 to 10 : 1, the mass percentage that catalyst auxiliary agent account...

Embodiment 1

[0033] Such as figure 1 shown

[0034] Carbon tetrachloride, iron powder (80 mesh) and triethyl phosphate are mixed and transported to a 100 liter ferrous complex catalyst preparation kettle through a slurry pump. The reaction temperature in the kettle is 100 ° C, and the reaction pressure is 0.15 MPa. The time is 1h, and the material mixture after the reaction is transported in the second 100 liters of chlorinated hydrocarbon synthesis reactors quickly through the filter, the distance between the two stills is 1.5m, and the inner diameter of the delivery pipe is 75mm, vinyl chloride (VCM) from The lower part is passed into the chlorinated hydrocarbon synthesis reactor and carbon tetrachloride for telomerization reaction. The ratio of carbon tetrachloride, vinyl chloride and triethyl phosphate is 70:14:1, and iron powder accounts for 1% of the mixed material. The mass percentage is 0.1wt%, the reaction temperature is 100°C, the reaction pressure is 0.2MPa, and the reaction re...

Embodiment 2

[0038] Such as figure 2 shown

[0039] Carbon tetrachloride, iron powder (80 mesh) and triethyl phosphate are mixed and transported to a 100-liter chlorinated hydrocarbon synthesis reaction kettle through a paddle pump, and vinyl chloride is passed into the chlorinated hydrocarbon synthesis reaction kettle and carbon tetrachloride from the lower part. Telomerization reaction, the ratio of carbon tetrachloride, vinyl chloride, and triethyl phosphate is 70:14:1, the mass percentage of iron powder in the mixed material is 0.1wt%, the reaction temperature is 100°C, and the reaction pressure is 0.2MPa, and the reaction residence time is 1h.

[0040] The reaction product is sent to the thin-film evaporator for flash evaporation after passing through the filter to remove iron powder. Light components such as carbon tetrachloride, vinyl chloride and chlorinated hydrocarbons (HCC240fa) enter the primary distillation tower, and the unreacted product is extracted from the top of the to...

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Abstract

The invention discloses a continuous preparation method for producing chlorohydrocarbon through carbon tetrachloride and olefins. The method includes the following steps that firstly, iron powder or iron filler, alkyl phosphate as catalyst promoters and carbon tetrachloride are continuously added into a first ferrous complex catalyst preparation kettle; secondly, materials obtained after reaction of the first step fast pass a filter, then are conveyed to a second chlorohydrocarbon synthesis reaction kettle, and react with olefins continuously introduced into the chlorohydrocarbon synthesis reaction kettle at the same time; thirdly, chlorohydrocarbon crude products obtained in the second step are introduced into a later separation system, and final target chlorohydrocarbon products are purified and collected. According to the method, it is designed that a ferrous complex catalyst preparation reaction and a chlorohydrocarbon synthesis reaction are isolated, and it is avoided that olefins autopolymer adheres to iron, and consequently the catalytic activity of iron powder or iron filler is reduced. The method is simple in technology, by controlling temperature, time, pressure and the like of reactions, reaction efficiency is further improved, meanwhile, the yield of reaction products is higher, and selectivity is better.

Description

technical field [0001] The invention relates to a continuous preparation method for producing chlorinated hydrocarbons from carbon tetrachloride and olefins. Background technique [0002] The structural formula in this field is CCl 3 CH 2 Chlorinated hydrocarbon (such as 1,1,1,3,3-pentachloropropane) preparation method of CHnClm (n=0~2, m=3-n) The current patent report mainly adopts batch reaction preparation and continuous reaction to prepare two In this process, the catalytic system adopts cuprous chloride complex catalytic system and iron catalytic system respectively. When adopting batch reaction to prepare chlorinated hydrocarbons, the production efficiency is low, and it is not suitable for industrialized mass production of products. An obvious defect in the use of cuprous chloride complex catalyst system is that the complex catalyst of cuprous salt cannot be recycled, because when recycling chlorinated products, the catalyst and catalyst additives must be removed b...

Claims

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Application Information

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IPC IPC(8): C07C19/01C07C17/278
CPCY02P20/584
Inventor 李宏峰马利勇周强
Owner JUHUA GROUP TECH CENT
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