Clean production method for perfluoroalkyl acrylate

A perfluoroalkyl acrylate, clean production technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., to achieve the effects of stable reaction, high conversion rate of acrylic acid, and sufficient reaction

Inactive Publication Date: 2011-11-02
山东中氟化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem of producing a large amount of waste water in the above perfluoroalkyl acrylate preparation process, the present invention provides a simple and economical process that can make the reaction process reach zero discharge A method for the clean production of perfluoroalkyl acrylate without producing a large amount of waste water in the post-treatment process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] On the 1L four-necked glass bottle, configure a negative pressure water separator, a stirrer, a thermometer, and a condenser. Add 728 g (2 mol) of perfluorohexyl ethanol, 115 g (1.6 mol) of acrylic acid, and 7.3 g of catalyst potassium hydrogen sulfate in sequence. Inhibitor hydroquinone 1.2g, 4-methoxyphenol 0.5g. Stir and heat up, control the temperature in the bottle to 110-120°C, and the pressure to -0.04--0.08Mpa, carry out the reaction, control the top temperature of the water separator ≥ 60°C, use the water separator to carry the water produced by the reaction during the reaction From the reaction body, the raw material fluoroalcohol taken out is put back into the bottle. After 8 hours, no more water was produced and the reaction was stopped. Measure out 28g of moisture. The reaction solution was cooled to room temperature, the catalyst was precipitated, and the catalyst was removed by filtration to obtain the crude product of perfluoroalkyl ethyl acrylate. Th...

Embodiment 2

[0030] Adjust the molar ratio of the reactant perfluorohexyl ethanol to acrylic acid to 1:1, and the weight ratio of perfluorohexyl ethanol to the catalyst to 1:0.01, and carry out the reaction. The process is the same as in Example 1, and 31.5 g of water is taken out by metering. The content of each component in the crude product of perfluorohexyl ethyl acrylate is shown in Table 2

[0031] Table 2 Reaction product component analysis results

[0032] name Content (%) perfluorohexylethanol 8.50 acrylic acid 1.55 perfluorohexyl ethyl acrylate 87.6

[0033] The conversion rate of acrylic acid was calculated to be 90.96%.

Embodiment 3

[0035] Adjust the molar ratio of the reactants perfluorohexyl alcohol to acrylic acid to 1:0.8, and the weight ratio of perfluorohexyl alcohol to the catalyst to 1:0.03, and carry out the reaction. The process is the same as in Example 1. The contents of each component in the crude perfluorohexyl ethyl acrylate are shown in Table 3.

[0036] Table 3 Reaction product component analysis results

[0037] name Content (%) perfluorohexylethanol 17.21 acrylic acid 0.15 perfluorohexyl ethyl acrylate 79.51

[0038] The conversion rate of acrylic acid was calculated to be 98.94%.

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PUM

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Abstract

The invention relates to a clean production method for perfluoroalkyl acrylate, which belongs to the field of preparation of intermediates containing fluorine. The technical scheme for the method is as follows: in a reaction vessel with a negative pressure water separator, under the condition of a negative pressure of -0.04 to -0.085 Mpa and a temperature of 110 to 120 DEG C, under the action of an alkali metal acid salt catalyst and a polymerization inhibitor, perfluoro alcohol reacts with acrylic acid or homologues thereof to generate perfluoroalkyl acrylate, wherein perfluoro alcohol refers to fluorine-containing alcohol which has a general formula of F(CF2CF2)n(CH2)mOH, n therein is a positive integer from 1 to 10, m therein is 1 or 2 or 3, and alkali metal acid salt is potassium bisulfate or sodium bisulfate. According to the invention, the negative pressure water separator is used to separate resultant moisture in time, which enables a more adequate reaction and a high conversion rate of acrylic acid; no azeotropic organic solvent is used and water generated in the reaction can be recycled directly; after the reaction ends, the catalyst precipitates with the decrease of temperature and can be removed by merely filtering, thereby achieving the purpose of clean production.

Description

technical field [0001] The invention relates to the field of preparation of fluorine-containing intermediates, in particular to a method for clean production of perfluoroalkyl acrylates. Background technique [0002] Perfluoroalkyl acrylates are key intermediates in the synthesis of fluorine-containing fabric finishes. It is reported in the literature that under the catalysis of p-toluenesulfonic acid, benzene, toluene and the water produced by the reaction are used to form an azeotrope, thereby taking the water out, so that the reaction can be carried out more fully. There are many patent documents in this regard, so it is not Enumerated, but, in the post-treatment process of this reaction, need water to wash away the catalyst of reaction—p-toluenesulfonic acid, produce a large amount of waste water, and after benzene, toluene and water slip off azeotropically, also need to carry out further Separation can be discharged or recycled, which increases the cost of the post-t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/653C07C67/08
Inventor 何日兴肖玉岭张立亭洪娟
Owner 山东中氟化工科技有限公司
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