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Continuous production method of 1,1,1,3-tetrachloropropane

A tetrachloropropane and production method technology, applied in the field 1, can solve problems such as complex discharging, difficult feeding, frequent activation of catalysts, etc., and achieve the effects of simple process, reduction of three waste emissions, and easy process control

Pending Publication Date: 2020-04-24
NINGBO JUHUA CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the disadvantages of difficult feeding, complicated discharging and frequent catalyst activation in the background technology, and provide a simple process, easy to operate, and environmentally friendly 1,1,1,3-tetrachloropropane continuous production method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In this example, the telomerization reactor adopts an electrically heated tubular reactor with a pipe diameter of ∮30×2.0 mm and a length of 2 m. The process flow is as follows:

[0030] (1) Mix carbon tetrachloride and co-catalyst at a molar ratio of 1:0.01, and preheat to 90°C, wherein the co-catalyst is tributyl phosphate;

[0031] (2) The preheated carbon tetrachloride, co-catalyst and ethylene are simultaneously and continuously entered into the telomerization reactor equipped with an iron catalyst with a particle size of 2-3mm, wherein the molar ratio of carbon tetrachloride and ethylene is 1:1. Under the conditions of pressure 0.85MPa, temperature 105°C, and residence time 120min, carry out telomerization to obtain crude 1,1,1,3-tetrachloropropane;

[0032] (3) Put the crude product of 1,1,1,3-tetrachloropropane into the first-stage vacuum rectification tower for separation, the rectification temperature is 60°C, the pressure is -0.08MPa, carbon tetrachloride and...

Embodiment 2

[0036] In this embodiment, the telomerization reactor adopts an electrically heated tubular reactor with a pipe diameter of ∮30×2.0mm and a length of 2m, and its technological process is as follows:

[0037] (1) Mix carbon tetrachloride and co-catalyst with a molar ratio of 1:0.005, and preheat to 80°C, wherein the co-catalyst is tributyl phosphate;

[0038] (2) The preheated carbon tetrachloride, co-catalyst and ethylene are simultaneously and continuously entered into the telomerization reactor equipped with a wire catalyst with a diameter of 2-3 mm, wherein the molar ratio of carbon tetrachloride and ethylene is 1.2:1, and the Under the conditions of MPa, temperature 95°C, and residence time 150min, carry out telomerization reaction to obtain 1,1,1,3-tetrachloropropane crude product;

[0039] (3) Put the 1,1,1,3-tetrachloropropane crude product into the first-stage vacuum rectification tower for separation, the rectification temperature is 70°C, the pressure is -0.06MPa, ca...

Embodiment 3

[0043] In this embodiment, the telomerization reactor adopts an electrically heated tubular reactor with a pipe diameter of ∮30×2.0mm and a length of 2m, and its technological process is as follows:

[0044] ] (1) Mix carbon tetrachloride and co-catalyst at a molar ratio of 1:0.01, and preheat to 95°C, wherein the co-catalyst is triethyl phosphate;

[0045](2) The preheated carbon tetrachloride, co-catalyst and ethylene are simultaneously and continuously entered into the telomerization reactor equipped with a ferric chloride / alumina catalyst with a particle size of 2-3mm, wherein the molar ratio of carbon tetrachloride to ethylene is 1.5: 1. Under the conditions of reaction pressure 1.1MPa, temperature 105°C, and residence time 50 minutes, carry out telomerization to obtain crude 1,1,1,3-tetrachloropropane;

[0046] (3) Put the crude product of 1,1,1,3-tetrachloropropane into a first-stage vacuum rectification tower for separation, the rectification temperature is 80°C, the p...

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Abstract

The invention discloses a continuous production method of 1,1,1,3-tetrachloropropane, wherein the method comprises the steps: (1) under the action of a main catalyst, preheating a mixture of carbon tetrachloride and a cocatalyst, and simultaneously and continuously introducing the preheated mixture and ethylene into a reactor for telomerization reaction to obtain a reaction product; (2) feeding the reaction product obtained in the step (1) into a first vacuum distillation tower, and separating to obtain tower top fraction and tower bottom liquid; and (3) separating the tower bottom liquid obtained in the step (2) in a second vacuum distillation tower to obtain a 1,1,1,3-tetrachloropropane product and a high-boiling residue. The method has the advantages that the process is simple and environmentally friendly, the catalyst does not need to be independently activated, and totally-enclosed integrated continuous production is achieved.

Description

technical field [0001] The invention relates to a production method of chlorinated alkanes, in particular to a continuous production method of 1,1,1,3-tetrachloropropane. Background technique [0002] 1,1,1,3-Tetrachloropropane, referred to as HCC-250fb, is an important fine chemical that can be used as a paint remover, degreasing agent and raw material for organic synthesis, such as for the preparation of 1-chloro-3, 3,3-trifluoropropane, 3,3,3-trifluoropropene or 1,1,1,2,3-pentachloropropane (HCC-240db). [0003] There are many ways to synthesize 1,1,1,3-tetrachloropropane, and most of them use iron or its compounds and organophosphorus compounds as catalysts. [0004] For example, WO2009 / 85862 discloses a continuous kettle-type process for preparing 1,1,1,3-tetrachloropropane, using iron powder, ferric chloride, and tributyl phosphate as a catalyst. Since iron powder is used as a solid material in this process, It is not easy to continuously quantitatively add to the re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/278C07C19/01C07C17/383
CPCC07C17/278C07C17/383C07C19/01
Inventor 周强钟骏良夏林兵涂德
Owner NINGBO JUHUA CHEM TECH CO LTD
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