Method for continuously synthesizing 1, 1, 1, 3, 3-pentachloropropane

A synthesis method and technology of pentachloropropane, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, preparation of halogenated hydrocarbons, etc., can solve low production efficiency, difficulty in large-scale production, and environmental damage And other issues

Pending Publication Date: 2022-06-10
SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Disadvantages of this process: (1) The telomerization reaction is a pressurized reaction, and it is difficult to design such a gap reaction. The output of a single kettle is too large, and the operation risk is high; (2) The reaction cycle is usually 5-10 hours, and the production efficiency is low. , the content of by-products is high, and the separation of iron powder catalyst is difficult, which affects the product quality and increases the cost of separation; (3) the reaction adopts mechanical stirring, which consumes a lot of electric energy
Patent 201410709721.X discloses a continuous reaction in a tubular reactor, but the main catalyst requires a composite iron material, and the co-catalyst is a phosphate or phosphite compound, and phosphorus will ca

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  • Method for continuously synthesizing 1, 1, 1, 3, 3-pentachloropropane

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0048] Example 1:

[0049] Weigh 500g of carbon tetrachloride raw materials, ethyl phosphite and vinyl chloride, and mix them evenly. The amount of ethyl phosphite is 2%, and the molar ratio of vinyl chloride to carbon tetrachloride is 1:2. The reactants are preheated to 90°C. Begin to enter the tubular reactor, the volumetric space velocity of vinyl chloride is 50h -1 . The reaction tube is a quartz tube with an inner diameter of 20 mm, and is filled with fine iron balls according to 70% of the volume of the reactor, the reaction temperature is controlled to 90 ° C, the reaction pressure is 0.4 MPa, and the reaction time is 40 minutes. 1,1,3,3-pentachloropropane, and the separated carbon tetrachloride is refluxed into the reaction feed liquid to continue the reaction. The conversion rate of vinyl chloride is 80.5%, and the selectivity of 1,1,1,3,3-pentachloropropane is 96.5%.

Example Embodiment

[0050] Example 2:

[0051] Weigh 500g of carbon tetrachloride raw materials, butyl phosphate and vinyl chloride are fully mixed, the amount of butyl phosphate is 5%, and the molar ratio of vinyl chloride and carbon tetrachloride is 1:3. The reactants are preheated to 60 ° C and begin to enter Tubular reactor with vinyl chloride volume space velocity of 120h -1 . The reaction tube adopts a quartz tube with an inner diameter of 20mm, and is filled with iron filings according to 70% of the volume of the reactor. The reaction temperature is controlled to 60°C, the reaction pressure is 0.7MPa, and the reaction time is 60 minutes. The crude product is collected by cold trap, and the crude product is analyzed by gas chromatography 1,1 , 1,3,3-pentachloropropane, and the separated carbon tetrachloride is refluxed to the reaction feed liquid to continue the reaction. The conversion rate of vinyl chloride is 65.5%, and the selectivity of 1,1,1,3,3-pentachloropropane is 97.5%.

Example Embodiment

[0052] Example 3:

[0053] Weigh 500g of carbon tetrachloride raw material, butyl phosphite and vinyl chloride are fully mixed, the amount of butyl phosphite is 3%, the molar ratio of vinyl chloride to carbon tetrachloride is 1:1, and the reactant is preheated to 120 ° C Begin to enter the tubular reactor, the volumetric space velocity of vinyl chloride is 80h -1 . The reaction tube adopts a quartz tube with an inner diameter of 20 mm, and is filled with Pall rings according to 70% of the volume of the reactor, and the reaction temperature is controlled at 120 ° C, the reaction pressure is 0.5 MPa, and the reaction time is 30 minutes. 1,1,3,3-pentachloropropane, and the separated carbon tetrachloride is refluxed into the reaction feed liquid to continue the reaction. The conversion rate of carbon tetrachloride is 85.5%, and the selectivity of 1,1,1,3,3-pentachloropropane is 95.5%.

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Abstract

The invention discloses a method for continuously synthesizing 1, 1, 1, 3, 3-pentachloropropane, which comprises the following steps: uniformly mixing carbon tetrachloride and vinyl chloride raw materials according to a certain ratio, pumping the mixture into a tubular reactor filled with an iron catalyst by using a pump, cooling the reaction discharged material by using a cold trap, collecting a reaction crude product, and distilling and rectifying the crude product to obtain the product, namely the 1, 1, 1, 3, 3-pentachloropropane. Unreacted materials enter the reactor to be recycled. Compared with the existing kettle-type intermittent or continuous reaction process, the method has the advantages of high catalytic reaction activity, low catalyst cost, wider selection, short reaction time, low by-product content, no need of subsequent separation of the catalyst, simple reaction process and equipment, and suitability for continuous industrial production.

Description

technical field [0001] The present invention relates to a preparation method of 1,1,1,3,3-pentachloropropane with molecular formula, in particular to the preparation of 1,1,1,3, Method for 3-Pentachloropropane. Background technique [0002] 1,1,1,3,3-Pentachloropropane is the raw material for the synthesis of 1,1,1,3,3-Pentafluoropropane (HFC-245fa), HFC-245fa is a new generation of environmentally friendly fluoride with an ODP value Zero, no potential damage to the atmosphere, can be used in a new generation of foaming agents, refrigerants and cleaning agents, and even can produce trifluoropropylene as a monomer for fluorosilicone rubber materials. HFC-245fa can eliminate hydrogen fluoride to obtain HFO-1234ze (1,3,3,3-tetrafluoropropene), which is also a new generation of environmentally friendly fluorohydroolefins with zero ODP value and no potential damage to the atmosphere. It is used as a new generation of refrigeration It can replace trifluoromethane and tetrafluoro...

Claims

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Application Information

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IPC IPC(8): C07C17/278C07C17/383C07C19/01B01J23/745B01J31/02B01J31/28
CPCC07C17/278C07C17/383B01J23/745B01J31/0235B01J31/0259B01J31/0258B01J31/0244B01J31/28C07C19/01
Inventor 姜标沈兆兵邢萍秦叶军
Owner SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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