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Process for preparing trifluoroacetaldehyde hydrate from 1,1,1-halothane

A technology of trifluoroethane and trifluoroacetaldehyde, applied in the field of chemical engineering, can solve the problems of harsh reaction conditions, difficult to obtain, expensive raw materials, etc., and achieve the effects of low production cost, easy separation, and resource saving

Active Publication Date: 2017-01-25
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because it is gaseous at room temperature and easily combines with water to form hydrates, it is difficult to prepare, produce and transport. At present, there are few studies on the preparation of trifluoroacetaldehyde hydrate, and no mature products have been produced. Production Technology and Process
[0004] U.S. Patent US3038936 and Hideyuki Mimura's research group in Japan have successively reported the preparation of trifluoroacetaldehyde by oxidizing 2,2,2-trifluoroethanol. The raw material 2,2,2-trifluoroethanol used in this process is expensive and difficult , which makes the cost of preparing trifluoroacetaldehyde higher
In addition, Pierce and Kane et al. reported the preparation of trifluoroacetaldehyde by liquid-phase reduction of 2,2,2-trifluoroacetate. This process needs to be carried out under anhydrous and low temperature (-70°C) conditions, using LiAlH 4 As a reducing agent, the process has harsh reaction conditions and is not suitable for industrial production
[0005] The above-mentioned process has problems such as expensive raw materials, complex process, harsh reaction conditions, and high cost of product separation in the later stage.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The raw materials consisting of 1,1,1-trifluoroethane, oxygen, and nitrogen are mixed and preheated at a molar ratio of 1:1.5:1 and then injected into the fixed bed reactor with 8% Fe 2 O 3 / AlF 3 It is a catalyst and reacts under the conditions of 0.5MPa and 280°C. The reaction proceeds continuously. The outlet product is absorbed by water and trifluoroacetaldehyde hydrate is separated.

[0018] In this embodiment, the conversion rate of 1,1,1-trifluoroethane is 17.6%, the selectivity of trifluoroacetaldehyde hydrate is 21.1%, and the purity of the separated trifluoroacetaldehyde hydrate is 92.1%.

Embodiment 2

[0020] The raw materials consisting of 1,1,1-trifluoroethane, oxygen, and nitrogen are mixed and preheated at a molar ratio of 1:1.5:3, and then injected into the fixed bed reactor with 16% Fe 2 O 3 / AlF 3 It is a catalyst and reacts under the conditions of 2MPa and 360°C. The reaction continues continuously. The outlet product is absorbed with water and trifluoroacetaldehyde hydrate is separated.

[0021] In this example, the conversion rate of 1,1,1-trifluoroethane is 38.6%, the selectivity of trifluoroacetaldehyde hydrate is 9.4%, and the purity of the separated trifluoroacetaldehyde hydrate is 93.5%.

Embodiment 3

[0023] The raw materials consisting of 1,1,1-trifluoroethane, oxygen, and nitrogen are mixed and preheated at a molar ratio of 1:1.5:2 and then injected into the fixed bed reactor with 10% Fe 2 O 3 / AlF 3 It is a catalyst and reacts under the conditions of 0.1MPa and 320°C, and the reaction proceeds continuously. The outlet product is absorbed by water and trifluoroacetaldehyde hydrate is separated.

[0024] In this example, the conversion rate of 1,1,1-trifluoroethane was 30.6%, the selectivity of trifluoroacetaldehyde hydrate was 16.8%, and the purity of the separated trifluoroacetaldehyde hydrate was 95.2%.

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PUM

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Abstract

The invention discloses a process for preparing trifluoroacetaldehyde hydrate from 1,1,1-halothane. The process comprises the following steps of preheating a raw material mixture consisting of 1,1,1-halothane, oxygen gas and nitrogen gas; then, injecting the mixture into a fixed bed reactor; using Fe2O3 / AlF3 or CuO / AlF3 as a catalyst; performing reaction at 0.1 to 3 mPa at 100 to 500 DEG C, wherein the reaction is continuously performed; adsorbing products at an outlet; and separating out the trifluoroacetaldehyde hydrate. The process for preparing the trifluoroacetaldehyde hydrate provided by the invention has the advantages that the conversion rate of the 1,1,1-halothane can reach 16 to 39 percent; the selectivity of the trifluoroacetaldehyde hydrate can reach 20 percent or higher; through the process, the 1,1,1-halothane can be directly converted into the trifluoroacetaldehyde hydrate; the reaction process is simple; the product can be easily separated; the purity of the obtained trifluoroacetaldehyde hydrate can reach 95 percent or higher. The trifluoroacetaldehyde hydrate capable of being applied to important chemical products can be prepared and produced at high efficiency and low cost.

Description

Technical field [0001] The invention belongs to the technical field of chemical engineering, and relates to a preparation process of trifluoroacetaldehyde hydrate, in particular to a process for preparing trifluoroacetaldehyde hydrate from 1,1,1-trifluoroethane. Background technique [0002] 1,1,1-trifluoroethane has been gradually banned as a third-generation refrigerant due to its high greenhouse effect potential. Therefore, how to convert it into higher value-added chemicals to solve its problem The current situation of large production capacity is an urgent problem to be solved. [0003] Because trifluoroacetaldehyde contains both trifluoromethyl and aldehyde groups in its molecule, it is widely used in synthetic resins, functional polymer materials, rubber, coatings, medicine, pesticides and other industries. However, because it is gaseous at room temperature and easily combines with water to form hydrates, it is difficult to prepare, produce or transport. At present, there a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/33C07C47/14
CPCC07C45/33C07C47/14
Inventor 涂东怀吕剑李扬谷玉杰白彦波王博
Owner XIAN MODERN CHEM RES INST
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