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Method for synthesizing tetrapion by electric catalytic membrane

A technology for synthesizing sodium tetrafluoropropionate and sodium tetrafluoropropionate, applied in chemical instruments and methods, membrane technology, electrolysis process, etc., can solve problems such as high energy consumption, hindrance of new reactions, separation of reactants and products, etc. Achieve the effect of simple process, wide application prospect and high selectivity

Active Publication Date: 2012-08-15
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Although organic electrochemistry has its unique features, there are also some shortcomings: (1) Electrochemical synthesis cannot separate reactants and products in time after the reaction, which will lead to side reactions such as further oxidation of products, Ultimately affect the selectivity of the reaction and the yield of the target product; (2) The reactant can only be transferred from the solution body to the electrode surface by the action of the electric field, and then the electrochemical reaction occurs, and the product cannot leave the electrode surface in time after the reaction is completed. This hinders the progress of new reactions, so organic electrochemical synthesis still has the problems of low current efficiency and high energy consumption.
However, in the process of membrane separation, membrane fouling has always been the bottleneck restricting the wide application of membrane separation technology.

Method used

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  • Method for synthesizing tetrapion by electric catalytic membrane
  • Method for synthesizing tetrapion by electric catalytic membrane
  • Method for synthesizing tetrapion by electric catalytic membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Prepare 2.0g / L tetrafluoropropanol aqueous solution and place it in the membrane reactor, add the same molar concentration of Na 2 CO 3 as an electrolyte. Under normal temperature and pressure, the working voltage is 3.0V, and the current density is 1mA / cm 2 And the flux is 2.0L / m 2 Under the condition of h, sodium tetrafluoropropionate was synthesized by catalytic oxidation of tetrafluoropropanol with titanium-based electrocatalytic membrane. Qualitative and quantitative detection of the raw liquid and permeated liquid of the reactor was carried out by high-performance liquid chromatography, and the results were as follows: figure 1 shown. Depend on figure 1 The conversion of reactants and the yield of products can be calculated. In this experiment, the conversion rate of tetrafluoropropanol was 93.2%, and the yield of sodium tetrafluoropropionate was 90.5%.

Embodiment 2

[0030] Prepare a 5.0 g / L tetrafluoropropanol aqueous solution and place it in a membrane reactor, and add NaOH with the same molar concentration as the electrolyte. Under normal temperature and pressure, the working voltage is 5.0V, and the current density is 10mA / cm 2 And the flux is 0.5L / m 2 Under the condition of h, sodium tetrafluoropropionate was synthesized by catalytic oxidation of tetrafluoropropanol with titanium-based electrocatalytic membrane. Qualitative and quantitative detection of the raw liquid and permeated liquid of the reactor was carried out by high-performance liquid chromatography, and the conversion rate of the reactant and the yield of the product were obtained. In this experiment, the conversion rate of tetrafluoropropanol was 96.5%, and the yield of sodium tetrafluoropropionate was 22.6%.

Embodiment 3

[0032] Prepare a 1.0g / L tetrafluoropropanol aqueous solution and place it in a membrane reactor, add NaHCO with the same molar concentration 3 as an electrolyte. Under normal temperature and pressure, the working voltage is 1.5V, and the current density is 0.1mA / cm 2 And the flux is 5.0L / m 2Under the condition of h, sodium tetrafluoropropionate was synthesized by catalytic oxidation of tetrafluoropropanol with titanium-based electrocatalytic membrane. Qualitative and quantitative detection of the raw liquid and permeated liquid of the reactor was carried out by high-performance liquid chromatography, and the conversion rate of the reactant and the yield of the product were obtained. In this experiment, the conversion rate of tetrafluoropropanol was 90.3%, and the yield of sodium tetrafluoropropionate was 89.6%.

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Abstract

The invention relates to the field of organic electrochemistry synthesis technology, and in particular relates to a method for synthesizing tetrapion by an electric catalytic membrane. The method is characterized by synthesizing the tetrapion in a way of integrating reaction and separation. The invention has the technical scheme that the titanium-based electric catalytic membrane is taken as an anode, and an auxiliary electrode is a cathode to form an electric catalytic membrane reactor; the reactant or feed liquid is mixed water solution of tetrafluoropropanol and sodium salt; under the condition with certain working voltage and current density, the tetrafluoropropanol is converted into an intermediate product tetrafluoropropanoic acid by catalytic oxidation on the surface of the membrane; then, the tetrafluoropropanoic acid and electrolyte sodium salt in the feed liquid have reaction, so that the tetrapion can be generated; meanwhile, a peristaltic pump is used for sucking under the condition with a certain membrane permeation flux; the reactant tetrafluoropropanol can be separated from the product tetrapion in real-time in an on-line way; and the pH value is adjusted to be about 7-8 by collecting membrane permeation liquid, and obtaining the tetrapion product by concentration. Compared with the traditional technology, the method has the advantages of being efficient and environment-friendly, being high in selectivity and simple in operation and the like, thus being suitable for industrialized implementation; and a new method is provided for preparing the efficient herbicide tetrapion and the method has wide application prospects.

Description

technical field [0001] The invention relates to the technical field of organic electrochemical synthesis, in particular to a method for synthesizing sodium tetrafluoropropionate through an electrocatalytic membrane. Background technique [0002] Fluorine chemical products are widely used in military industry, chemical industry, machinery and other fields due to their excellent properties such as chemical resistance, high and low temperature resistance, aging resistance, low friction, and insulation. At present, the total amount of fluorine chemical products in the world is about 2.5 million tons, with sales exceeding US$21 billion. The annual growth rate of domestic demand for fluoride has reached more than 12%, and the fluorine chemical industry has become one of the fastest growing industries in my country. [0003] Fluorine-containing fine chemicals are high-end applications in the fluorine chemical industry, mainly including fluorine-containing medicines, fluorine-conta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/02B01D61/00C25B3/23
Inventor 王虹杨阳李建新王会
Owner TIANJIN POLYTECHNIC UNIV
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