Preparation method of 3,3,3-trifluoro-1,2-propylene glycol

A technology of propylene glycol and trifluoropropylene oxide, applied in the field of fluorine chemical industry, can solve the problems of poor industrial application prospect, water or solvent consumption, poor safety, etc., and achieve the effects of short reaction time, few side reactions and mild reaction conditions

Pending Publication Date: 2021-08-31
SHANDONG HUAAN NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome technical deficiencies such as the need for a large amount of water or solvent consumption, high energy consumption, poor safety, and

Method used

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  • Preparation method of 3,3,3-trifluoro-1,2-propylene glycol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Put 300g of trifluoropropylene oxide and 6g of solid catalyst (the amount is 2% of the mass of trifluoropropylene oxide) into a 1L high-pressure reactor, seal the reactor, and replace the air in the reactor with carbon dioxide;

[0037] (2) Stir the reaction kettle to raise the temperature to 45°C, and the stirring speed is 200-300r / min;

[0038] (3) Continuously bubbling carbon dioxide into the reactor until the pressure inside the reactor is 2.0~2.5MPa and maintained;

[0039] (4) After reacting for 6 hours, the unreacted carbon dioxide was discharged by releasing the pressure to obtain the intermediate product trifluoromethylethylene carbonate;

[0040] (5) Add 129g of methanol into the reactor, raise the temperature until the material boils, and reflux for 4 hours;

[0041] (6) After the reaction is completed, the products are separated by rectification to obtain dimethyl carbonate and 3,3,3-trifluoro-1,2-propanediol respectively. After weighing and testing, th...

Embodiment 2

[0043] (1) Put 300g of trifluoropropylene oxide and 6g of solid catalyst (the amount is 2% of the mass of trifluoropropylene oxide) into a 1L high-pressure reactor, seal the reactor, and replace the air in the reactor with carbon dioxide;

[0044] (2) Stir the reaction kettle to raise the temperature to 45°C, and the stirring speed is 200-300r / min;

[0045] (3) Continuously bubbling carbon dioxide into the reactor until the pressure inside the reactor is 2.0~2.5MPa and maintained;

[0046] (4) After reacting for 6 hours, the unreacted carbon dioxide was discharged by releasing the pressure to obtain the intermediate product trifluoromethylethylene carbonate;

[0047] (5) Add 185g of ethanol to the reaction kettle, heat up to boiling, and reflux for 4 hours;

[0048] (6) After the reaction is completed, the products are separated by rectification to obtain diethyl carbonate and 3,3,3-trifluoro-1,2-propanediol respectively. After weighing and testing, the selectivity is 99.4%, ...

Embodiment 3

[0050](1) Put 300g of trifluoropropylene oxide and 6g of solid catalyst (the amount is 2% of the mass of trifluoropropylene oxide) into a 1L high-pressure reactor, seal the reactor, and replace the air in the reactor with carbon dioxide;

[0051] (2) Stir the reaction kettle to raise the temperature to 45°C, and the stirring speed is 200-300r / min;

[0052] (3) Continuously bubbling carbon dioxide into the reactor until the pressure inside the reactor is 2.0~2.5MPa and maintained;

[0053] (4) After reacting for 6 hours, the unreacted carbon dioxide was discharged by releasing the pressure to obtain the intermediate product trifluoromethylethylene carbonate;

[0054] (5) Add 242g of propanol into the reaction kettle, raise the temperature until the material boils, and reflux for 5 hours;

[0055] (6) After the reaction is completed, the products are separated by rectification to obtain dipropyl carbonate and 3,3,3-trifluoro-1,2-propanediol respectively. After weighing and test...

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Abstract

The invention relates to a preparation method of 3,3,3-trifluoro-1,2-propylene glycol, and belongs to the technical field of fluorine chemical industry. The preparation method of 3,3,3-trifluoro-1,2-propylene glycol comprises the steps: carrying out cycloaddition reaction on trifluoroepoxypropane serving as a raw material and carbon dioxide in the presence of a solid catalyst to obtain an intermediate product trifluoromethyl ethylene carbonate; and adding fluorine-free monohydric alcohol into a reaction kettle, and carrying out transesterification on the fluorine-free monohydric alcohol and trifluoromethyl ethylene carbonate to obtain diester carbonate and 3,3,3-trifluoro-1,2-propylene glycol. The related raw materials and process are safer, the reaction is carried out in the same reaction kettle in two times, but only one heterogeneous catalyst is needed, and the whole reaction is mild in condition, short in reaction time, high in yield, free of solvent and few in side reaction. The used catalyst is a heterogeneous solid catalyst, has high gas-liquid phase and liquid-liquid phase catalysis efficiency, can be repeatedly used, is easy to separate from a reaction system after the reaction is completed, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of 3,3,3-trifluoro-1,2-propanediol, which belongs to the technical field of fluorine chemical industry. Background technique [0002] Fluorine-containing alcohols are a class of compounds formed by replacing hydrogen atoms on carbon in organic alcohols with fluorine atoms. Compared with organic alcohols, fluorine-containing alcohol compounds show unique physical and chemical properties and physiological activities due to the existence of C-F bonds in their molecular structures, and can be used as raw materials, intermediates, solvents, and auxiliary agents in new medicines, pesticides, and dyes As well as the research and development of new materials, it can also be used as a lubricant and cleaning agent in the electronics industry, and can also be used as a fluorine-containing surfactant, a fabric finishing agent, a new solvent, etc., and is widely used. As a kind of fluorine-containing alcohol, 3,3,3-tri...

Claims

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Application Information

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IPC IPC(8): C07C29/12C07C31/42
CPCC07C29/12C07D317/36
Inventor 段琦魏刚王瑞英邹冉燕东崔传博田勇
Owner SHANDONG HUAAN NEW MATERIAL
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