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Synthesis method of 1,1,2-trichloro-3-fluoropropylene

A synthetic method and technology of fluoropropene, applied in 1 field, can solve the problems of high reaction temperature, low conversion rate and selectivity, and no reaction data given, and achieve the effect of high conversion rate and good selectivity

Active Publication Date: 2012-07-25
山东华安近代环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the patent does not provide specific relevant reaction data. From the disclosed content, it can be seen that the reaction temperature of this method is high, and the conversion rate and selectivity are low.

Method used

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  • Synthesis method of 1,1,2-trichloro-3-fluoropropylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 5.0g (0.028mol) of 1,1,2,3-tetrachloropropene and 30mL of diethylene glycol to a 50mL dry three-neck flask equipped with a magnetic stirrer, a thermometer, and a condensing device, start stirring, and heat up to 120 After ℃, add 8.1g (0.069mol) potassium fluoride to the reaction solution, react for 1 hour, the reaction solution is cooled to room temperature, filter the reaction solution to obtain 7.4g white solid, the filtrate is subtractively distilled, under vacuum 5kPa, collect 40~48 °C fractions to obtain 1,1,2-trichloro-3-fluoropropene, the conversion rate of 1,1,2,3-tetrachloropropene was 96.4%, the selection of 1,2-trichloro-3-fluoropropene sex 92.2%.

[0021] Product Structure Characterization:

[0022] bp: 135°C

[0023] MS: m / z 163.95 (M + )

[0024] 1 H-NMR (CDCl 3 , 500MHz) δ: 5.195(s, 1H), 5.101(s, 1H), J H-F =47Hz

[0025] 13 C-NMR (CDCl 3 , 500MHz) δ: 127.112-127.246 (d, 1C, J C-F =67Hz), 124.724-124.811 (d, 1C, J C-F =43.5Hz), 80.343-80.7...

Embodiment 2～4

[0028] The operation is basically the same as in Example 1, except that the reaction temperature and the reaction time are different, and the reaction results are shown in Table 1.

[0029] Table 1

[0030] Example Reaction temperature / ℃ Reaction time / h Conversion rates / % selectivity / % 1 110 1.5 96.4 92.2 2 120 1.0 98.7 90.0 3 100 4 98.9 93.1 4 90 10 70.1 94.5

Embodiment 5～9

[0032] The operation is basically the same as in Example 1, except that the solvent of Examples 5 to 9 is ethylene glycol, the reaction time is 4h, and the mol ratio of KF and 1,1,2,3-tetrachloropropene is respectively 1:1 , 1.5:1, 2:1, 2.5:1, 5:1, the reaction results are shown in Table 2.

[0033] Table 2

[0034] Example KF:TCP / (mol:mol) Conversion rates / % selectivity / % 5 1.0 65.3 92.1 6 1.5 85.7 92.4 7 2.0 95.4 92.2 8 2.5 98.2 91.8 9 5.0 99.2 92.5

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Abstract

The invention provides a synthesis method of 1,1,2-trichloro-3-fluoropropylene, comprising the following step: in the presence of a polyalcohol solvent, carrying out a reaction on 1,1,2,3-tetrachloropropene and an alkali metal fluoride at 90-120 DEG C for 1.0-10h to obtain 1,1,2-trichloro-3-fluoropropylene. The molar ratio of the alkali metal fluoride to 1,1,2,3-tetrachloropropene is (1-5):1, wherein the alkali metal fluoride is sodium fluoride, potassium fluoride or cesium fluoride; and the polyalcohol is glycol, 1,2-propanediol, 1,3-propanediol, 2,3-butanediol, diethylene glycol, triethylene glycol, tetraethylene glycol or glycerol. The synthesis method provided by the invention is mainly applied to preparing 1,1,2-trichloro-3-fluoropropylene.

Description

technical field [0001] The present invention relates to a kind of synthetic method of 1,1,2-trichloro-3-fluoropropene, especially a kind of using 1,1,2,3-tetrachloropropene (TCP) and alkali metal fluoride as raw materials, in A synthetic method for obtaining 1,1,2-trichloro-3-fluoropropene by liquid-phase fluorination in an alkali metal fluoride-polyol system. Background technique [0002] The ozone depletion potential of 2,3,3,3-tetrafluoropropene (HFO-1234yf) is zero, the greenhouse effect potential is 4, and its environmental performance is excellent. It is considered to be an ideal substitute for HFC-134a. 1,1,2-Trichloro-3-fluoropropene can be used as a raw material for the preparation of HFO-1234yf. [0003] Patent WO2010045104 discloses the preparation method of 1,1,2-trichloro-3-fluoropropene, which uses tetrachloroethylene and fluoromethane as the reaction raw materials, in chlorine, carbon tetrachloride, trichlorotoluene, hexachloroethyl In the presence of free r...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C17/35
Inventor 马辉吕剑张伟谷玉杰曾纪珺韩升郝志军杨志强王伟
Owner 山东华安近代环保科技有限公司
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