Preparation method of trifluoroisopropanol

A technology for trifluoroisopropanol and trifluoroacetaldehyde is applied in the preparation of 1,1,1-trifluoro-2-propanol and in the field of preparation of trifluoroisopropanol, which can solve the problems of unsuitable industrial production and raw materials. Inflammable and explosive, large equipment investment and other problems, to achieve the effect of high yield, short reaction process and simple preparation process

Active Publication Date: 2021-10-01
SHANDONG HUAAN NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome technical defects such as flammable and explosive raw materials, large equipment investment, high cost, and unsuitability for industrial production in the prior art, the present invention provides a gas phase preparation method of 1,1,1-trifluoro-2-propanol, which The method has the advantages of simple process, mild reaction conditions, high conversion rate of raw materials, and easy industrialization.

Method used

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  • Preparation method of trifluoroisopropanol

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Embodiment 1

[0024] In the dry reaction kettle, 11.4g (0.075mol) of cesium fluoride was added under the protection of nitrogen, the temperature was lowered to -10°C, and 900ml (1.8mol) of 2.0mol / L tetrahydrofuran solution of methylmagnesium chloride was added under stirring, and then three A mixture of 147.03g (1.50mol) of fluoroacetaldehyde and 375mL of tetrahydrofuran. After dropping, slowly warm up to 0°C and react for 10h. Add 3ml of water to quench the reaction and purify to obtain 160.33g of colorless liquid namely 1,1,1-trifluoro-2-propanol, GC purity 99.2% (area normalization method), yield 95.01%

Embodiment 2

[0026] The ratio of methylmagnesium chloride to trifluoroacetaldehyde was changed to 1:1, and the others were the same as in Example 1 to synthesize 1,1,1-trifluoro-2-propanol with a yield of 95.20%.

Embodiment 3

[0028] The ratio of methylmagnesium chloride to trifluoroacetaldehyde was changed to 1:1.2, and the others were the same as in Example 1 to synthesize 1,1,1-trifluoro-2-propanol with a yield of 96.34%.

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Abstract

The invention relates to a preparation method of trifluoroisopropanol, in particular to a preparation method of 1, 1, 1-trifluoro-2-propanol, and belongs to the technical field of fluorine chemical industry. According to the preparation method of the 1, 1, 1-trifluoro-2-propanol, disclosed by the invention, the 1, 1, 1-trifluoro-2-propanol is prepared by taking a methylmagnesium chloride Grignard reagent and trifluoropropionaldehyde as reactants through Grignard reaction. The preparation process of the raw materials trifluoropropionaldehyde and methylmagnesium chloride has mild reaction conditions. The reaction yield is high, the conversion rate of trifluoropropionaldehyde reaches 98% or above, and the selectivity of 1, 1, 1-trifluoro-2-propanol reaches 95% or above. The method is short in reaction process, simple in preparation process, safe, environment-friendly and few in side reaction. Continuous feeding can be realized, and large-scale industrial co-production is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of trifluoroisopropanol, in particular to a preparation method of 1,1,1-trifluoro-2-propanol, which belongs to the technical field of fluorine chemical industry. Background technique [0002] The molecular formula of 1,1,1-trifluoro-2-propanol is C3H5F3O, the molecular weight is 114.07, the CAS number is 374-01-6, the density is 1.235g / cm3, the boiling point is 67.0°C, and the flash point is 38.8°C. Its structural formula is as follows: [0003] [0004] 1,1,1-Trifluoro-2-propanol is a new type of fluorine-containing compound. It is a highly polar solvent that is easily mixed with water and many organic solvents. It has good thermal stability and is resistant to ultraviolet light. The permeability is good. These properties make 1,1,1-trifluoro-2-propanol an ideal solvent in many polymerization systems; 1,1,1-trifluoro-2-propanol is used as an intermediate for pharmaceuticals ( For example: 1,1,1-Trifl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/38C07C29/32
CPCC07C29/32C07C31/38Y02P20/584
Inventor 王瑞英李丕永王永千张丽平邹冉
Owner SHANDONG HUAAN NEW MATERIAL
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