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Preparation method of 1, 1, 1, 3, 3, 3-hexafluoropropane

A technology of hexafluoropropane and hexafluoroisobutyric acid, which is applied in the preparation of organic compounds, the preparation of carboxylate, the preparation of halogenated hydrocarbons, etc., can solve the problems of complex preparation process, unfavorable industrialization, and difficulty in obtaining raw materials, etc. The preparation route is short, the industrialization prospect is broad, and the effect of improving the utilization rate of resources

Inactive Publication Date: 2019-04-19
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The raw materials of this method are not easy to obtain, the preparation process is complicated, and the yield is low, which is not conducive to industrialization

Method used

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  • Preparation method of 1, 1, 1, 3, 3, 3-hexafluoropropane
  • Preparation method of 1, 1, 1, 3, 3, 3-hexafluoropropane
  • Preparation method of 1, 1, 1, 3, 3, 3-hexafluoropropane

Examples

Experimental program
Comparison scheme
Effect test

example 1～23

[0037] Under normal pressure stirring conditions, in a 500ml four-necked round-bottomed flask with a condenser, first add a halogen-containing inorganic salt and an aprotic solvent, heat up to the reaction temperature, and then slowly add heptafluoroisobutenyl methyl ether through a constant flow pump to carry out After the reaction, water was added and stirred continuously for 5 minutes, the temperature was lowered and the fluoride salt was filtered off, and the filtrate was rectified to obtain recovered aprotic solvent and hexafluoroisobutyric acid. The test results under different conditions are shown in Table 1.

[0038] Table 1 Hexafluoroisobutyric acid preparation test parameters and results

[0039]

[0040]

[0041] Note: The amount of heptafluoroisobutenyl methyl ether is 106g (0.5mol), the amount of aprotic solvent is 200ml, the amount of water is 0.52mol, and the molar ratio and conversion rate are based on heptafluoroisobutenyl methyl ether.

[0042] Step 2:...

example 24～28

[0044] Take the hexafluoroisobutyric acid prepared in Examples 9-15 and Examples 18-21 respectively, put them in a 500ml three-necked round-bottomed flask with a condenser, heat and stir at the set temperature, and the gas phase products generated are cooled by two stages. , the two-stage cooling temperature is -50°C, and the cooling liquid is collected to obtain the HFC-236fa product. The test results of other different conditions are shown in Table 2.

[0045] Table 2 HFC-236fa preparation test parameters and results

[0046]

[0047] Note: The amount of hexafluoroisobutyric acid is 0.5mol.

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Abstract

The invention discloses a preparation method of 1, 1, 1, 3, 3, 3-hexafluoropropane. The method includes: (1) reacting a halogenated inorganic salt with heptafluoroisobutenyl methyl ether in an aproticsolvent, then adding water and performing stirring, conducting cooling and filtering, and rectifying the filtrate to obtain hexafluoroisobutyric acid; and (2) heating the hexafluoroisobutyric acid obtained in step (1), collecting the generated gaseous product and performing cooling to obtain the 1, 1, 1, 3, 3, 3-hexafluoropropane product. The method provided by the invention has the advantages ofsimple process, environmental friendliness, low cost, green and environmental protection.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of 1,1,1,3,3,3-hexafluoropropane. Background technique [0002] 1,1,1,3,3,3-Hexafluoropropane (referred to as HFC-236fa), colorless, odorless, low-toxic gas, CAS 690-39-1, molecular weight 152, boiling point -1.5°C, saturated vapor pressure 229.6 kPa (20°C). [0003] 1,1,1,3,3,3-Hexafluoropropane is a very useful fluorine-containing organic compound, which is widely used in the fields of cleaning agent, refrigerant, foaming agent, heat transfer medium and propellant. At the same time, because its boiling point and vapor pressure are similar to Halon fire extinguishing agent, it has the advantages of non-corrosion, non-conductivity, and no residue, so it is also used as an ideal substitute for Halon. The current industry mainly adopts the route of obtaining HFC-236fa by fluorination of 1,1,1,3,3,3-hexachloropropane as raw material. In addition, there are so...

Claims

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Application Information

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IPC IPC(8): C07C19/08C07C17/363C07C53/21C07C51/00
CPCC07C17/363C07C51/00C07C53/21C07C19/08
Inventor 吕杨李宏峰黄雪浩马利勇徐宇宁
Owner JUHUA GROUP TECH CENT
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