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Method for synthesizing 2,3,3,3-tetrafluoropropene

A tetrafluoropropene and synthetic method technology, applied in the direction of halogen substitution preparation, organic chemistry, etc., can solve the problems of low yield and high price of the target product, and achieve the effects of low production cost, high yield and wide source of raw materials

Active Publication Date: 2015-10-21
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
[0019] 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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  • Method for synthesizing 2,3,3,3-tetrafluoropropene

Examples

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Effect test

example 1

[0034] Example 1: Preparation of 2-chloropropene

[0035] 200 mL of beta-zeolite was added to the fixed bed with a diameter of 25×1200 mm, and the two ends were sealed with quartz stones. The fixed bed is preheated to 240°C, then 1,2-dichloropropane is added at a rate of 0.5L / h, preheated to 180°C by a preheater, and then cracked in the fixed bed at 240°C. The cracked gas is cooled by a cooler. Enter the buffer bottle, condense the cleavage 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 as hydrochloric acid. After 2 hours of continuous cracking, 950 g of liquid was obtained, and sample analysis (chromatographic column SE-30, column temperature 30 ° C, hold for 3 minutes, then rise 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-ch...

example 2

[0036] Example 2: According to the same method and ratio, the pyrolysis temperature was increased to 260° C. After 2 hours of continuous pyrolysis, 830 g of liquid was obtained, and sampled for analysis. 1,2-Dichloropropane content 32%, cis-1-chloropropene 11%, trans-1-chloropropene 11%, 2-chloropropene 35.5%, 3-chloropropene 11.5%. The reduction of material discharge means that there is polymerization or carbonization. When the fixed bed is disassembled, it is found that there is carbonization. Therefore, the pyrolysis temperature should be less than 260 °C.

example 3

[0037] Example 3: Preparation of 2,3,3,3-tetrachloropropene

[0038]Take out the beta-zeolite, replace it with 200ml of granular ferric chloride, heat it to 220°C, preheat 1 mol of 2-chloropropene and 3mol of chlorine gas at 0.5L / h to 160°C and 120°C respectively through a preheater, and then reheat it. After mixing by a static mixer, it was passed into a fixed bed with a residence time of 20 seconds. The gas coming out is cooled by a 20-meter long coil cooler, and the non-condensable hydrogen chloride gas is absorbed from the top of the cooler into hydrochloric acid with water to obtain 105g of liquid. Sampling and analysis (chromatographic column SE-30, column temperature 80°C, hold for 3 minutes, then rise to 250°C at 30°C / min, vaporization temperature 250°C, detector temperature 250°C), 2,3,3,3-4 82% of chloropropene, 18% of 1,2,2,3,3,3-hexachloropropane, the fraction 2,3,3,3-tetrachloropropene at 71-72℃ was collected by vacuum fractionation to obtain 140g of product, con...

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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, in particular to a method for synthesizing 2,3,3,3-tetrafluoropropene. Background technique [0002] After 2008, with the implementation of the Montreal Protocol, the currently used second-generation refrigerant HFC-134a (GWP=143) has obvious greenhouse effect, so it is necessary to develop the third-generation low-greenhouse effect refrigerant. One of the options is HFO-1234yf is 2,3,3,3-tetrafluoropropene, referred to as tetrafluoropropene, its boiling point is -30℃, ODP=0, GWP=4, its excellent performance is suitable for automobile air-conditioning refrigerant. 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 its synthesis was rarely reported before, but in recent years, research and development have been strengthened all over the world. There are as many as more than a doz...

Claims

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Application Information

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Patent Type & Authority Applications(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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