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Method for preparing perfluoroalkyl iodine through catalytic distillation telomerization

A perfluoroalkyl iodide and catalytic distillation technology, which is applied in chemical instruments and methods, preparation of halogenated hydrocarbons, chemical industry, etc., can solve problems affecting the normal operation of industrial devices, catalysts cannot be recycled, and the content of hydrogen-containing by-products is large. problems, to achieve the effect of avoiding hydrogen-containing by-products, avoiding difficulties in solid-liquid separation, and good product composition distribution

Active Publication Date: 2014-06-25
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the product discharged from the reactor in liquid state contains a large amount of catalyst, which needs to be separated from liquid and solid, and the catalyst cannot be recycled, and the cost is high. The tubular reactor is easy to cause the accumulation of reaction heat, which makes it difficult to control the telomerization reaction.
The disadvantage is that the carbon chain distribution of the process product is wide
The disadvantage is that the process has hydrogen-containing by-products, which are not easy to purify
[0007] The telomerization process adopted by the above patents and known technologies all has deficiencies: or adopt a tubular reactor, the reaction efficiency is low, and the operation is difficult; or adopt a tank reactor, the telomerization reaction is difficult to control, and the product carbon number distribution is too high wide; or use peroxide initiator at the same time, the content of hydrogen-containing by-products is large; or use copper powder catalyst with small particles, which will cause shortcomings such as large bed resistance, which will affect the normal operation of industrial devices

Method used

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  • Method for preparing perfluoroalkyl iodine through catalytic distillation telomerization
  • Method for preparing perfluoroalkyl iodine through catalytic distillation telomerization

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Effect test

Embodiment 1

[0027] The inner diameter of the catalytic distillation tower is φ1000mm, the reaction section 2 is divided into three sections, and each section is filled with phosphor bronze wire mesh corrugated packing Xiangshi Huaxing Chemical Equipment Packing Co., Ltd. Production, model 125, specific surface area 125m 2 / m 3 , according to the mass percentage, the composition is: 2% tin, 0.4% phosphorus, 0.08% lead, and the rest is copper) 2m high, C 2 f 5 I is continuously added from the rectifying section 1 at the upper part of the reaction section 2, and gas-phase tetrafluoroethylene is continuously added from the stripping section 3 at the lower part of the reaction section 2. The reaction conditions are: C 2 f 5 The molar ratio of I and tetrafluoroethylene is 1:5; the reaction pressure is 1.0 MPa; the temperature of the reaction section is 70° C., the low-boiling fraction containing tetrafluoroethylene is extracted from the top of the tower, and the perfluoroalkyl iodide crude...

Embodiment 2

[0029] The inner diameter of the catalytic distillation tower is φ1000mm, the reaction section 2 is divided into five sections, and each section is filled with phosphor bronze wire mesh corrugated packing Xiangshi Huaxing Chemical Equipment Packing Co., Ltd. Production, model 250, specific surface area 250m 2 / m 3 , according to the mass percentage content: tin 3%, phosphorus 0.3%, lead 0.05%, the rest is copper) 1m high, C 2 f 5 I is continuously added from the rectifying section 1 at the upper part of the reaction section 2, and gas-phase tetrafluoroethylene is continuously added from the stripping section 3 at the lower part of the reaction section 2. The reaction conditions are: C 2 f 5 The molar ratio of I and tetrafluoroethylene is 1:3; the reaction pressure is 0.8MPa; the temperature of the reaction section is 80° C., the low-boiling fraction containing tetrafluoroethylene is extracted from the tower top, and the perfluoroalkyl iodide crude product is continuously ...

Embodiment 3

[0031] The inner diameter of the catalytic distillation tower is φ1000mm, the reaction section 2 is divided into one section, and each section is filled with phosphor bronze wire mesh corrugated packing Xiangshi Huaxing Chemical Equipment Packing Co., Ltd. Production, model 500, specific surface area 500m 2 / m 3 , according to the mass percentage, the composition is: 4% tin, 0.2% phosphorus, 0.1% lead, and the rest is copper) 5m high, C 2 f 5 I is continuously added from the rectifying section 1 at the upper part of the reaction section 2, and gas-phase tetrafluoroethylene is continuously added from the stripping section 3 at the lower part of the reaction section 2. The reaction conditions are: C 2 f 5The molar ratio of I and tetrafluoroethylene is 1:7; the reaction pressure is 0.6MPa; the temperature of the reaction section is 85° C., the low-boiling fraction containing tetrafluoroethylene is extracted from the tower top, and the perfluoroalkyl iodide crude product is c...

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Abstract

The invention discloses a method for preparing perfluoroalkyl iodine through catalytic distillation telomerization. A catalytic distillation tower adopted for preparation consists of a rectifying section, a reaction section, a stripping section and a tower vessel which are sequentially connected from a tower top to a tower bottom, and the reaction section is filled with a phosphor bronze gauze packing which serves as a catalyst; the preparation method comprises the following steps: (a) respectively continuously adding pentafluoroethyl iodide and tetrafluoroethylene from the rectifying section and the stripping section into the catalytic distillation tower for reaction at the reaction temperature of 70-100DEG C under the reaction pressure of 0.5-1.4MPa, wherein the mole ratio of pentafluoroethyl iodide to tetrafluoroethylene is 1:(2-10); and (b) continuously guiding a reaction product of the tower vessel out, to obtain the perfluoroalkyl iodine product. The method has the advantages of being simple in production equipment, easily controllable for technology parameters, good in operation safety, high in reaction efficiency, easy for product separation.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing fine chemical intermediates, in particular to a method for preparing perfluoroalkyl iodide by catalytic distillation telomerization. Background technique [0002] Perfluoroalkyliodides are key intermediates in the production of fluorinated fine chemicals. usually in C 2 f 5 I is an end group, and TFE (tetrafluoroethylene) is a telomerization monomer, which is obtained by telomerization reaction in the presence of an initiator, high temperature and high pressure, or a metal catalyst. Major international manufacturers of fluorochemicals produce and further process them into various brands of fluorosurfactants, which are widely used in the chemical, mechanical, textile and paper industries, as well as the ink coating industry and fire protection fields. In recent years, various companies have made great breakthroughs in the improvement of initiators, the improvement of reactor types, ...

Claims

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Application Information

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IPC IPC(8): C07C19/16C07C17/278
CPCY02P20/10
Inventor 王金明
Owner JUHUA GROUP TECH CENT
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