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The synthetic method of 2,3,3,3-tetrafluoropropene

A technology of tetrafluoropropene and synthesis method, applied in halogen substitution preparation, organic chemistry and other directions, can solve problems such as high price and low yield of target product, and achieve the effects of low production cost, high yield and wide source of raw materials

Active Publication Date: 2016-09-28
山东联创产业发展集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The CAS of 2,3,3,3-tetrafluoropropene is 754-12-1. There were few reports on its synthesis before. In recent years, the whole world has strengthened its research and development
[0005] Each of the above synthetic routes has its own advantages and disadvantages, but there are common problems such as high price and low yield of the target product.

Method used

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  • The synthetic method of 2,3,3,3-tetrafluoropropene

Examples

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Effect test

example 1

[0020] Example 1: Preparation of 2-chloropropene

[0021] Add 200 mL of β-zeolite to the fixed bed with a diameter of 25×1200 mm, and seal both ends with quartz stones. Preheat the fixed bed to 240°C, then add 1,2-dichloropropane at a rate of 0.5L / h, preheat to 180°C through the preheater, enter the fixed bed and crack at 240°C, and the cracked gas is cooled by the cooler Enter the buffer bottle, condense the cracked product into a liquid through the reflux condenser on the buffer bottle, and the non-condensable hydrogen chloride gas comes out from the top of the condenser and passes into the water to become hydrochloric acid. After 2 hours of continuous cleavage, 950g of liquid was obtained, which was sampled and analyzed (chromatographic column SE-30, column temperature 30°C, kept for 3 minutes, then raised to 150°C at 10°C / min, vaporization temperature 150°C, detector temperature 150°C) , 1,2-dichloropropane content 45.5%, cis 1-chloropropene 12%, trans 1-chloropropene 12%...

example 2

[0022] Example 2: By the same method and proportioning, the pyrolysis temperature was increased to 260°C, and 830 g of liquid was obtained after continuous pyrolysis for 2 hours, which was sampled and analyzed. The content of 1,2-dichloropropane is 32%, cis-1-chloropropene is 11%, trans-1-chloropropene is 11%, 2-chloropropene is 35.5%, and 3-chloropropene is 11.5%. The decrease in output means that there is polymerization or carbonization. When the fixed bed is disassembled, carbonization is found, so the cracking temperature should be less than 260°C.

example 3

[0023] Example 3: Preparation of 2,3,3,3-tetrachloropropene

[0024] Take out the β-zeolite, replace it with 200mL granular ferric chloride, heat it up to 220°C, preheat 1mol of 2-chloropropene and 3mol of chlorine gas at 0.5L / h to 160°C and 120°C respectively through a preheater, and then After being mixed by a static mixer, it is passed into a fixed bed, and the residence time is 20 seconds. The gas that comes out is cooled by a 20-meter long coil cooler, and the non-condensable hydrogen chloride gas goes out from the top of the cooler and is absorbed by water to be hydrochloric acid to obtain 105 g of liquid. Sampling analysis (chromatographic column SE-30, column temperature 80°C, keep for 3 minutes, then rise to 250°C at 30°C / min, vaporization temperature 250°C, detector temperature 250°C), 2,3,3,3-four Chloropropene 82%, 1,2,2,3,3,3-hexachloropropane 18%, 71-72°C fraction 2,3,3,3-tetrachloropropene was collected by vacuum fractional distillation to obtain 140g of produc...

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Abstract

The invention discloses a method for synthesizing 2,3,3,3-tetrafluoropropene and belongs to the field of organic synthesis. The method comprises the following steps: (1) preparing 2-chloropropene from 1,2-dichloropropane, which serves as a raw material, through continuous catalytic cracking by adopting a fixed bed in the presence of beta-zeolite, which serves as a catalyst; (2) selectively chlorinating 2-chloropropene with chlorine gas under the catalysis of ferric chloride, so as to prepare 2,3,3,3-tetrachloropropylene; and (3) fluorating 2,3,3,3-tetrachloropropylene with hydrofluoric acid under the catalysis of SbF3 or SbF5, thereby obtaining 2,3,3,3-tetrafluoropropene. The synthesis route has the advantages that the source of raw materials is wide, the cost is low, and the product yield is high; and the obtained product can serve as an automotive air conditioning refrigerant and has a positive significance in reduction of greenhouse effect.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a synthesis method of tetrafluoropropene. Background technique [0002] After 2008, with the advancement of the implementation of the Montreal Protocol, the second-generation refrigerant HFC-134a (GWP=143) currently in use has a significant greenhouse effect, so it is necessary to develop a third-generation low-greenhouse effect refrigerant. One of the options is HFO-1234yf is 2,3,3,3-tetrafluoropropene, referred to as tetrafluoropropene, with a boiling point of -30°C, ODP=0, and GWP=4. Its excellent performance is suitable for use as a refrigerant for automobile air conditioners. Therefore, the development of this product has positive significance for reducing the greenhouse effect. [0003] The CAS of 2,3,3,3-tetrafluoropropene is 754-12-1, and there were few reports on its synthesis before. In recent years, the whole world has strengthened its research and develop...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C21/18C07C17/20
Inventor 李洪国李俊
Owner 山东联创产业发展集团股份有限公司
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