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A kind of industrial production method of octafluorocyclopentene

A technology for producing octafluorocyclopentene, which is applied in chemical instruments and methods, separation/purification of hydroxyl compounds, organic chemistry, etc., and can solve the problems of low product separation yield, many reaction steps, unsuitable raw materials, etc. Achieve the effect of high product purity, lower production cost and high yield

Active Publication Date: 2020-08-11
DALIAN JOIN KING FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] In summary, the current existing octafluorocyclopentene synthesis method has many reaction steps, unsuitable raw materials, a large amount of hydrogen fluoride is used, many reaction steps, and low product separation yield.

Method used

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  • A kind of industrial production method of octafluorocyclopentene
  • A kind of industrial production method of octafluorocyclopentene
  • A kind of industrial production method of octafluorocyclopentene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: the synthetic route of octachlorocyclopentene in this example, by following reaction formula:

[0033]

[0034] Experimental steps:

[0035] Add 68g (1mol, 97%) liquid cyclopentene to a 250ml four-port reaction kettle equipped with mechanical stirring and reflux condensing device, and connect to an alkaline tail gas absorption device;

[0036] When the internal temperature of the system is 25°C, chlorine gas is started to flow into the kettle. At this time, the temperature of the system will rise, and the temperature at reflux is 45°C (the normal pressure boiling point of cyclopentene is 44.2°C), and the addition reaction of chlorine gas occurs, and there is no gas at the beginning. Production, chlorine gas is absorbed completely, and along with the carrying out of reaction, reflux stops, and the aeration rate of chlorine gas is optimal with 1g / min. At this time, a sample was taken for gas phase analysis, and the raw material cyclopentene was less than...

Embodiment 2

[0039] Embodiment 2: the synthetic route of octachlorocyclopentene in this example is the enlargement of example 1

[0040]

[0041] Experimental steps:

[0042] Add 680g (10mol, 97%) liquid cyclopentene to a 2L four-port reactor equipped with mechanical stirring and reflux condensing device, and connect to an alkaline tail gas absorption device;

[0043] Begin to feed chlorine gas in the kettle at room temperature, and the temperature of the system will rise at this time, and the temperature during reflux is 45° C. (the normal pressure boiling point of cyclopentene is 44.2° C.). Addition reaction occurs in feeding chlorine gas, so there is no gas production at the beginning. Chlorine is absorbed completely, and along with the carrying out of reaction, backflow stops, and the aeration rate of chlorine is optimal with 1g / min. At this time, a sample can be taken for gas phase analysis, and the raw material cyclopentene is <2%. Then slowly raise the temperature of the system...

Embodiment 3

[0046] Embodiment 3: the synthetic route of octafluorocyclopentene in this example, according to following reaction formula:

[0047]

[0048] Experimental steps:

[0049] Add 290g of anhydrous potassium fluoride (5mol, 99%, 10eq) and 1012g of sulfolane to a 2L four-port reactor equipped with mechanical stirring and rectification condensing device, and stir to raise the temperature to 140°C.

[0050]After mixing 172g (98%, 0.5mol) of self-made octachlorocyclopentene with 180g of sulfolane, dropwise added to the above system, the dropwise addition time is 2h, the temperature of the system rises slowly during the dropwise addition process, and the heating rate is about 5°C / h, After the dropwise addition, the system refluxed obviously, and the product was extracted from the top of the rectifying tower. The normal pressure boiling point of the product octafluorocyclopentene is 27°C.

[0051] When the product fraction decreases, continue to increase the temperature of the syst...

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Abstract

The invention discloses an industrialized production method for 1,2,3,3,4,4,5,5-octafluorocyclopentene, and belongs to the field of synthesis of fine chemical intermediates. Cyclopentene, a chlorine gas and anhydrous potassium fluoride are used as raw materials, sulfolane is used as a solvent, chlorination is performed step by step through programmed heating, and the chlorinated product and the potassium fluoride are subjected to a high-temperature substitution reaction to form the 1,2,3,3,4,4,5,5-octafluorocyclopentene. According to the method provided by the invention, kettle residues afterseparation of the product can be reused after the solvent sulfolane is distilled out under reduced pressure; and the method provided by the invention has the advantages of simple production process steps, greenness, environmental protection, a high yield and low production cost, and the obtained product has high purity and is beneficial to a later application.

Description

technical field [0001] The invention relates to an industrial production method of octafluorocyclopentene, which belongs to the field of synthesis of fine chemical intermediates. Background technique [0002] 1,2,3,3,4,4,5,5-octafluorocyclopentene, referred to as octafluorocyclopentene or perfluorocyclopentene, is mainly used in the etching and cleaning of semiconductors, and can participate in the preparation of organic photochromic Material. Octafluorocyclopentene is considered to have competitive advantages as a next-generation etching gas and as one of the most attractive raw materials for electronic devices. Octafluorocyclopentene can also be used in the synthesis of high-end dyes. It has less impact on the environment and is a new type of fluorine-containing chemical. [0003] Most of the preparation methods in the literature use the fluorochloride of cyclopentene as the raw material, and are prepared through multi-step fluorination reactions. [0004] Takeo Furuta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/20C07C23/08C07D333/48C07C29/74C07C31/08
CPCC07C17/02C07C17/10C07C17/204C07C29/74C07D333/48C07C31/08C07C23/08
Inventor 刘磊李君宫本海刘钢
Owner DALIAN JOIN KING FINE CHEM CO LTD
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