Preparation method of 1,1,2,3-tetrachloropropene

A technology of tetrachloropropene and carbon tetrachloride, which is applied in the field of preparation of 1, chlorine-containing olefins, can solve the problems of large discharge of "three wastes", unrecoverable catalysts, and difficult availability of raw materials, etc., and achieves low separation cost and low cost , the effect of reducing production costs

Inactive Publication Date: 2019-11-29
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the raw materials are not easy to obtain, the catalyst cannot be recycled, and the cost is high
The disadvantages are low yield, high energy consumption, and large discharge of "three wastes"
The disadvantage is that the catalyst cannot be recycled and the discharge of "three wastes" is large
[0006] In summary, although there are many methods for preparing 1,1,2,3-tetrachloropropene at present, there are problems such as unavailable raw materials, low yield, high energy consumption, unrecoverable catalysts, and large discharge of "three wastes". or something like that

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Preparation of neodymium-containing synergist

[0043] In parts by weight, add 100 parts of ZSM-5 molecular sieves to a stirred reactor, add water and stir to obtain a slurry, add 200 parts of methanol with a mass concentration of 30% dropwise, filter, wash the filter cake to neutrality, dry, 500 Roast at ℃ for 4 hours, put it into a flask, then add 0.1 part of tris(1,10-phenanthroline) iron hexafluorophosphate, 300 parts of acetone, 0.07 part of neodymium (III) hexafluoro-2,4-acetylacetonate dihydrate , 5 parts of bis(bistrimethylsilyl)amine zinc, 11 parts of alkyl imidazoline phosphate, stirred and reacted for 4 hours, filtered and dried to prepare a neodymium-containing synergist for future use.

[0044] (2) preparation of carbon tetrachloride mixed solution

[0045] The neodymium-containing synergist that step (1) obtains, auxiliary agent tributyl phosphate, catalyzer 200 order iron powders are added in the carbon tetrachloride, stir to obtain the carbon tetrac...

Embodiment 2

[0053] (1) Preparation of neodymium-containing synergist

[0054] In parts by weight, add 100 parts of ZSM-5 molecular sieves to a stirred reactor, add water and stir to obtain a slurry, add 300 parts of methanol with a mass concentration of 20% dropwise, filter, wash the filter cake to neutrality, dry, 600 Roast at ℃ for 2 hours, put it into a flask, add 0.05 parts of tris(1,10-phenanthroline) iron hexafluorophosphate, 200 parts of acetone, 0.02 parts of neodymium(III) hexafluoro-2,4-acetylacetonate dihydrate , 1 part of bis(bistrimethylsilyl)amine zinc, 5 parts of alkyl imidazoline phosphate, stirred and reacted for 2 hours, filtered and dried to prepare a neodymium-containing synergist for future use.

[0055] (2) preparation of carbon tetrachloride mixed solution

[0056] The neodymium-containing synergist that step (1) obtains, auxiliary agent tributyl phosphate, catalyst 120 order iron powders are added in the carbon tetrachloride, stir to obtain the carbon tetrachlorid...

Embodiment 3

[0064] (1) Preparation of neodymium-containing synergist

[0065] In parts by weight, add 100 parts of ZSM-5 molecular sieves to a stirred reactor, add water and stir to obtain a slurry, add 150 parts of methanol with a mass concentration of 40% dropwise, filter, wash the filter cake until neutral, dry, 450 Roast at ℃ for 6 hours, put it into a flask, and then add 0.7 parts of tris(1,10-phenanthroline) iron hexafluorophosphate, 500 parts of acetone, and 0.5 parts of neodymium (III) hexafluoro-2,4-acetylacetonate dihydrate , 3 parts of bis(bistrimethylsilyl)amine zinc, 20 parts of alkyl imidazoline phosphate, stirred and reacted for 6 hours, filtered and dried to prepare a neodymium-containing synergist for future use.

[0066] (2) preparation of carbon tetrachloride mixed solution

[0067] The neodymium-containing synergist that step (1) obtains, auxiliary agent tributyl phosphate, catalyst 100 order iron powders are added in the carbon tetrachloride, stir to obtain the carbo...

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Abstract

The invention discloses a preparation method of 1,1,2,3-tetrachloropropene, and the method comprises the following steps: (1) preparing a neodymium-containing synergist for later use; (2) preparing acarbon tetrachloride mixed solution for later use; (3) continuously introducing the carbon tetrachloride mixed solution and ethylene into a second reactor for reaction to obtain a reaction product; (4) separating the reaction product to obtain a first stream and a second stream, and separating the second stream to obtain a third stream and a fourth stream; (5) rectifying the first stream and the third stream to obtain 1,1,1,3-tetrachloropropane and recovered carbon tetrachloride; (6) cracking the 1,1,1,3-tetrachloropropane, condensing and separating tail gas to obtain a cracking product; (7) performing gas phase chlorination on the cracking product, and condensing and separating tail gas to obtain a gas phase chlorination product; (8) cracking the gas phase chlorination product, collectingthe reaction product, condensing and separating tail gas to obtain the1,1,2,3-tetrachloropropene product. The preparation method has the advantages of simple process, high efficiency, low cost and environmental friendliness.

Description

technical field [0001] The invention relates to a preparation method of chlorinated olefins, which belongs to the field of organic synthesis, in particular to a preparation method of 1,1,2,3-tetrachloropropene. Background technique [0002] 1,1,2,3-Tetrachloropropene (TCP, also known as HCC-1230xa) is one of the main intermediates for the preparation of the chemical herbicide dicamba EC, and is also the main raw material for the pesticide product dicamba. 1,1,2,3-Tetrachloropropene can also be used as a raw material to produce CFC-1233xf, HFO-1234ze, HFC-245eb, HCFC-244bb, HFO-1234yf, 2,3-dichloro-1,1,1, - Trifluoropropane (HCFC-243db), etc., among which HFO-1234yf is a new generation of environmentally friendly fluorine refrigerant, which is typically characterized by a low GWP value (its value is 4), which is suitable for the large-scale use of automotive air-conditioning refrigeration Agents are a potential, economical and immediate alternative. The production methods o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/275C07C19/01C07C17/25C07C21/04C07C17/04C07C17/38B01J31/26
CPCB01J31/26C07C17/04C07C17/25C07C17/275C07C17/38C07C17/383C07C19/01C07C21/04
Inventor 王金明吕杨
Owner JUHUA GROUP TECH CENT
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