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Method for preparing 1,1,1-trifluoroacetone

A technology of trifluoroacetone and ethyl trifluoroacetoacetate, which is applied in the field of preparation of 1,1,1-trifluoroacetone, can solve problems such as difficulty in industrialization and expensive catalysts, and achieve reduction of three wastes emissions, safe and reliable production process, Simple operation effect

Inactive Publication Date: 2012-05-30
SINOCHEM LANTIAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] PCT patent application WO0236536A1 and U.S. patent US2004054234 reported acetic acid and trifluoroacetic acid in CeO 2 / ThO 2 A method for preparing a mixture of trifluoroacetone, acetic acid, trifluoroacetic acid and water under high-temperature catalysis. The starting materials of this method are easy to obtain and cheap, but the catalyst is expensive and industrialization is difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add methanesulfonic acid (100.9g, 1.05mol) into a 150mL cold trap equipped with an electric stirring device, a thermometer, a constant pressure dropping funnel and a reflux condenser (the reflux condenser is connected to tap water, and the upper outlet is connected to a 150mL cold trap at -40°C) in a 250mL four-neck flask to collect the product). The methanesulfonic acid was heated to 100°C within 30 minutes, and ethyl 4,4,4-trifluoroacetoacetate (92.1 g, 0.5 mol) in a constant pressure dropping funnel was added dropwise to the methanesulfonic acid, During the dropwise addition, 1,1,1-trifluoroacetone was generated and collected in a cold trap at -40°C. After dripping, keep at 100°C for 1 hour, then rise to 110°C for 2 hours and then stop the reaction. 52.2g of colorless liquid is obtained as the product 1,1,1-trifluoroacetone with a purity of 99.1% (GC area Normalization method), the reaction yield was 92.4%.

[0031]

Embodiment 2

[0033] Add methanesulfonic acid (505g, 5.25mol) into a 500mL container equipped with an electric stirring device, a thermometer, a constant pressure dropping funnel and a reflux condenser (the reflux condenser is connected to tap water, and the upper outlet is connected to -40°C with a tube). Secondary cold trap to collect the product) in a 1 L four-necked flask. The methanesulfonic acid was heated to 100°C within 60 minutes, and ethyl 4,4,4-trifluoroacetoacetate (460.5 g, 2.5 mol) in the constant pressure dropping funnel was added dropwise into the methanesulfonic acid, During the dropwise addition, 1,1,1-trifluoroacetone was generated, which was collected in a secondary cold trap at -40°C. After dripping, keep at 100°C for 2 hours, and then rise to 110°C for 3 hours to stop the reaction. Receive 199.5g in the first-stage cold trap and 63.8g in the second-stage cold trap, a total of 263.3g of colorless liquid is The product 1,1,1-trifluoroacetone has a purity of 99.0% (G...

Embodiment 3

[0036] Add methanesulfonic acid (96g, 1.0mol) into a 150mL cold trap equipped with an electric stirring device, a thermometer, a constant pressure dropping funnel and a reflux condenser (the reflux condenser is connected to tap water, and the upper outlet is connected to a 150mL cold trap at -40°C) to collect the product) in a 250mL four-necked flask. The methanesulfonic acid was heated to 100°C within 30 minutes, and ethyl 4,4,4-trifluoroacetoacetate (100 g, 0.54 mol) in the constant pressure dropping funnel was added dropwise to the methanesulfonic acid, and During the addition process, 1,1,1-trifluoroacetone was generated and collected in a cold trap at -40°C. After dripping, keep at 100°C for 1 hour, and then rise to 110°C for 2 hours to stop the reaction. 49.7g of colorless liquid is obtained as the product 1,1,1-trifluoroacetone with a purity of 99.4% (GC area Normalization method), the reaction yield was 88.2%.

[0037]

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PUM

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Abstract

The invention discloses a method for preparing 1,1,1-trifluoroacetone, which is used for preparing the 1,1,1-trifluoroacetone by reacting 4,4,4-trifluoroethyl acetoacetate and organic acid in an anhydrous state. Compared with the prior art, the method overcomes the risk in exploding trifluoroacetone hydrate easily generated in a water reaction environment in air, and has a safe and reliable production process; meanwhile, both the product purity and the yield are higher; furthermore, the organic acid as a raw material can be recycled; the method is low in three-waste pollution, low in production cost and simple to operate; and the prepared 1,1,1-trifluoroacetone can be used for producing a plurality of important fine chemical intermediates.

Description

technical field [0001] The invention relates to a preparation method of 1,1,1-trifluoroacetone. Background technique [0002] Trifluoroacetone (TFK) is a very useful fluorine-containing fine chemical and one of the most valuable products in fluorine-containing ketones. A variety of important fine chemical intermediates can be derived from trifluoroacetone, such as hydrogenation reduction to obtain trifluoropropanol; and aromatic compounds to generate tertiary alcohols; bromination in the presence of sulfuric acid to obtain universal synthetic building block tribromide Fluoroacetone, reacts with m-nitroaniline to generate photographic coupler, etc. The reduction product trifluoropropanol is used as a solvent and catalyst in the synthesis of various polymers and fine chemicals, and is widely used in dyes, photosensitive materials, liquid crystal display materials, aerospace technology, pesticides, medicine, polymer materials and other fields. It is an important intermediate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/167C07C45/67
Inventor 任洪春杨汪松蒋四春
Owner SINOCHEM LANTIAN
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