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Process for preparing 1, 1, 1-trifluoroethane and 1, 1, 1-difluoro chloroethane

A technology for chlorodifluoroethane and trifluoroethane, which is applied in the field of preparing halogenated hydrocarbons, can solve the problems of decreased catalyst activity, increased production cost, decreased reaction yield and the like, and achieves the effect of inhibiting the generation of tar-like substances

Inactive Publication Date: 2005-07-06
苏州联氟化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has obvious defects in industrial implementation. The main reason is that under the reaction conditions, the raw material vinylidene chloride is very easy to polymerize and crack, generating a large amount of polymers and tar-like substances. The generation of this tar-like substances leads to The decline in reaction yield, on the other hand, pollutes the catalyst, causing the activity of the catalyst to drop rapidly, resulting in the interruption of the production process; and the formation of tar-like substances occupies the volume of the reactor, which makes the space-time yield of the reactor drop significantly.
These factors will lead to frequent interruptions of industrial production processes, resulting in increased production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: Preparation of 1.1.1-trifluoroethane (R143a) and 1.1.1-chlorodifluoroethane (R142b) with p-diphenol as additive

[0021] Add 1 gram of p-diphenol and 100 grams of tin tetrachloride to a 2L steel reactor with a reflux tower, then add 500 grams of hydrogen fluoride, and then heat until the inner temperature is 60-65 ° C, starting with 95-100 grams Feed vinylidene chloride at a speed of 60-65 g / h, and simultaneously feed hydrogen fluoride at a speed of 60-65 g / h, draw the reaction product from the top of the reflux tower, the reaction product is a mixture of R143a, R142b and HCl, and maintain the reaction pressure at 13 bar Left and right, the product is regularly detected by gas chromatography after washing with water and alkali. At the end of the reaction, the content of R143a in the product was 58.5%, and the content of R142b was 40.3%.

[0022] When the feeding amount of vinylidene chloride reaches about 2000 grams, stop feeding, and drain the low boilin...

Embodiment 2

[0024] The present embodiment adopts the same operating method and equipment as in Example 1, and the additions and products in the operating process are listed below.

[0025] The additive is 2 gram p-diphenol, the catalyst is 100 gram tin tetrachloride, and the addition of vinylidene chloride is 1953 grams, and the feeding is stopped; the amount of tar produced by adding 100 grams of vinylidene chloride in this embodiment is 0.91 grams.

Embodiment 3

[0027] The present embodiment adopts the same operating method and equipment as in Example 1, and the additions and products in the operating process are listed below.

[0028] The additive is 2 grams of tert-butylphenol, the catalyst is 100 grams of tin tetrachloride, and the addition of vinylidene chloride stops feeding when the amount of vinylidene chloride is 1912 grams; the amount of tar produced by adding 100 grams of vinylidene chloride in this embodiment is 0.92 grams.

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PUM

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Abstract

The present invention discloses a method for preparing 1,1,1-trifluoroethane and 1,1,1-difluorochloroethane. In the existence of liquid phase fluorinated catalyst and additive, VDC and hydrogen fluoride are reacted in liquid phase. The liquid phase fluorinated catalyst is selected from halide of metal antimony, tin, titanium, tantalum, niobium or fluorosulfuric acid or chlorosultonic acid. The additive comprises at least one kind of phenolic compound, and can be added with organic phosphorus compound. The inventive method can effectively reduce tarry matters generation, thereby prolonging useful life of the catalyst and improving its efficiency.

Description

technical field [0001] The invention relates to a method for preparing halogenated hydrocarbons, in particular to a method for preparing 1.1.1-trifluoroethane and 1.1.1-chlorodifluoroethane through a liquid-phase fluorination method. Background technique [0002] 1.1.1-Trifluoroethane (i.e. R143a) and 1.1.1-chlorodifluoroethane (i.e. R142b) are widely used compounds, which can be used as refrigerants, foaming agents, propellants, cleaning agents, etc. , can be used as an environmentally compatible substitute for Freon because it has not been found to have adverse effects on the ozone layer. [0003] Using vinylidene chloride and hydrogen fluoride in the presence of catalysts such as tin tetrachloride to prepare R143a and R142b by liquid phase fluorination is a technology that has already been disclosed. The commonly used catalysts include metal antimony, metal tin, metal titanium, metal Halides such as niobium, and fluorosulfonic acid, chlorosulfo...

Claims

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Application Information

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IPC IPC(8): C07C17/08C07C19/08C07C19/12
Inventor 尤来方
Owner 苏州联氟化学有限公司
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