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Continuous synthesis method of low-carbon-chain perfluoroalkyl iodide

A technique for the synthesis of perfluoroalkyl iodides, which is applied in chemical instruments and methods, preparation of halogenated hydrocarbons, and chemical recovery. It can solve the problems of limited application, accumulation of reaction heat, and high cost, and achieve simplified production processes and reduced production costs. Good effect of cost and composition distribution

Active Publication Date: 2014-01-22
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst-initiated production process is safe and controllable, with few by-products and low impurity content, and can obtain better product distribution. The disadvantage is that the catalyst-initiated process in the prior art adopts batch production in kettle or tubular reactors , the operation is cumbersome and the efficiency is low, which limits its application in industrial production, and tetrafluoroethylene is easy to self-polymerize at high temperature, and the conversion rate is low
The disadvantage is the use of intermittent production, cumbersome operation and low efficiency
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.

Method used

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  • Continuous synthesis method of low-carbon-chain perfluoroalkyl iodide
  • Continuous synthesis method of low-carbon-chain perfluoroalkyl iodide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] In packed tower 1, heat transfer oil containing 300 mesh copper powder (brand WD-350, Changzhou Changcheng Energy Equipment Co., Ltd.) is circulated from the top of the tower to the bottom of the tower, and the mass ratio of heat transfer oil to copper powder is 1:0.005. The heat conduction oil is heated up to 340° C. through the heater 3, and pentafluoroiodoethane and tetrafluoroethylene are continuously fed into the packed tower 1 through the flow meter, and the flow rates are 400ml / min and 50ml / min respectively. The product is continuously extracted from the top of the packed tower 1, cooled by the condenser 4 and analyzed by gas chromatography. The reaction results are shown in Table 1.

Embodiment 2

[0037] In the packed tower, heat transfer oil containing 250 mesh copper powder (brand WD-350, Changzhou Changcheng Energy Equipment Co., Ltd.) circulates from the top of the tower to the bottom of the tower. The mass ratio of heat transfer oil to copper powder is 1:0.01, which will conduct heat The oil is heated up to 300°C through the heater 3, and pentafluoroiodoethane and tetrafluoroethylene are continuously introduced into the packed tower 1 through the flowmeter, and the flow rates of pentafluoroiodoethane and tetrafluoroethylene are 400ml / min and 45ml / min respectively. min. The product is continuously extracted from the top of the packed tower 1, cooled by the condenser 4 and analyzed by gas chromatography. The reaction results are shown in Table 1.

Embodiment 3

[0039] In the packed tower, heat transfer oil containing 200 mesh copper powder (brand WD-350, Changzhou Changcheng Energy Equipment Co., Ltd.) is circulated from the top of the tower to the bottom of the tower. The mass ratio of heat transfer oil to copper powder is 1:0.05, which will conduct heat The oil is heated up to 280°C through the heater 3, and pentafluoroiodoethane and tetrafluoroethylene are continuously introduced into the packed tower 1 through the flowmeter, and the flow rates of pentafluoroiodoethane and tetrafluoroethylene are 400ml / min and 40ml / min respectively. min. The product is continuously extracted from the top of the packed tower 1, cooled by the condenser 4 and analyzed by gas chromatography. The reaction results are shown in Table 1.

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Abstract

The invention discloses a continuous synthesis method of low-carbon-chain perfluoroalkyl iodide, which comprises the following steps: (a) adding a heating medium and a catalyst in a mass ratio of 1:(0.005-0.1) into a filler tower; (b) leading the heating agent-catalyst mixture out of the bottom of the filler tower, heating by a heater through a circulating pump, returning to a circulating liquid inlet of the filler tower so that the heating agent containing the catalyst circularly flows from top to bottom in the filler tower, and meanwhile, continuously introducing pentafluoroethyliodide and tetrafluoroethylene in a volume ratio of (5-20):1 into the filler tower through the bottom to react at 200-370 DEG C; and (c) continuously leading the reaction product out of the top of the filler tower, and cooling by a condenser to obtain the low-carbon-chain perfluoroalkyl iodide. The method has the advantages of simple technique, high efficiency and favorable product composition distribution, and is safe and controllable; and the catalyst does not need to be separated and can be recycled.

Description

technical field [0001] The invention relates to a synthesis method of a fluorine-containing fine chemical intermediate, in particular to a continuous synthesis method of a low carbon chain perfluoroalkyl iodide. Background technique [0002] As we all know, the fluorine-containing fabric finishing agent prepared with C8 as the basic raw material has water and oil repellent properties unmatched by other types of fabric finishing agents, and is the mainstream of water and oil repellent fabric finishing agents. However, with the implementation of the EU ban, the market has to turn to the development of low-carbon chain perfluoroalkyl iodide products. Low-carbon chain perfluoroalkyl iodide refers to perfluorobutyl iodide (C4) and perfluorohexyl iodide (C6). The English abbreviations are PFBI and PFHI respectively. It is a colorless or red liquid at room temperature. At present, low-carbon chain perfluoroalkyl iodide is the main raw material to replace perfluorooctyl iodide (C8)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/16C07C17/278
CPCY02P20/584
Inventor 耿为利周强王树华兰喜平胡正吕秉达
Owner JUHUA GROUP TECH CENT
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