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Preparation method of porous perfluorinated sulfonic acid resin for catalysts

A perfluorosulfonic acid resin and catalyst technology, which is applied in the preparation of organic compounds, the preparation of carboxylic acid esters, chemical instruments and methods, etc., can solve the problems of loss of effective components, decreased service life of catalysts, and increased difficulty of catalyst preparation.

Active Publication Date: 2015-07-15
SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sol-gel method and the loading method need to prepare the hydroalcoholic solution of the sulfonic acid resin. As far as the high-molecular-weight perfluorosulfonic acid resin with poor solubility is concerned, this process undoubtedly increases the difficulty of preparing the catalyst. method can not fundamentally solve the problem of loss of effective components, resulting in a decline in the service life of the catalyst

Method used

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  • Preparation method of porous perfluorinated sulfonic acid resin for catalysts
  • Preparation method of porous perfluorinated sulfonic acid resin for catalysts
  • Preparation method of porous perfluorinated sulfonic acid resin for catalysts

Examples

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preparation example Construction

[0008] A kind of preparation method of porous perfluorosulfonic acid resin for catalyst, comprises the steps:

[0009] (1) Mix the porogen with the dispersion medium, the mass ratio of the porogen to the dispersion medium is 1:(2~32), keep the temperature at 80~150℃ and the pressure 0.1~1.0MPa at a constant temperature of 2~8 hour, the porogen dispersion was obtained;

[0010] (2) Mix the porogen dispersion prepared in step (1) with perfluorosulfonyl vinyl ether, solvent, and initiator, and the porogen dispersion, perfluorosulfonyl vinyl ether, solvent, and initiator The mass ratio is (1~20):(3~19):(0~14):(2×10 -5 ~2×10 -4 ), feed tetrafluoroethylene to maintain a reaction pressure of 200 to 2000kpa, and conduct a polymerization reaction for 1 to 8 hours at a reaction temperature of 10 to 80°C to obtain a polymer feed liquid;

[0011] (3) Add deionized water and dispersant to the polymer liquid prepared in step (2), heat to 90-100°C, stir and distill for 1-4 hours, and filt...

specific Embodiment approach

[0034] Now, the present invention will be described in further detail with reference to the following examples, but the present invention is not limited to these examples.

[0035] In the following examples, all percentages are by weight unless otherwise stated. In the present invention, the EW value of the product is measured by an acid-base titration method, the melt index of the product is measured by a melt indexer, the pore size is measured by a scanning electron microscope, and the particle size is determined by a sieving method. The thermal decomposition temperature of the product was analyzed by thermogravimetric method.

[0036] raw material source

[0037] The porogen A described in the embodiment has an Ew of 870, a molecular weight of 100,000, and a structural formula as follows:

[0038]

[0039] The preparation method of porogen A:

[0040] Add 150g of perfluorosulfonyl vinyl ether (LSPSVE), 650g of water (which contains 2g of perfluorooctanoic acid ammoniu...

Embodiment 1

[0053] A kind of preparation method of porous perfluorosulfonic acid resin for catalyst, comprises the steps:

[0054] (1) Take 125g of perfluoroheptane and 25g of porogen A into a 300ml autoclave, stir and heat in an oil bath to 120°C, keep the temperature for 1 hour, and cool to room temperature to obtain a solid content of 17wt%. Color transparent porogen A dispersion;

[0055] (2) Add 450g of perfluorosulfonyl vinyl ether (LSPSVE) to a 2L stainless steel reactor at room temperature, add 150g of porogen A dispersion, 1g of isopropyl peroxydicarbonate, and add 900g of perfluoroheptane. Replace with nitrogen and then replace with TFE, then pass through TFE (tetrafluoroethylene) to pressurize, raise the temperature to 70°C, adjust the pressure to keep the pressure of TFE at 650kpa, react for 1.5 hours, cool down, exhaust and discharge, and obtain a polymer Material liquid;

[0056] (3) Add 4000g of water and 100ml of polyvinyl alcohol solution with a mass percentage of 3% to...

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PUM

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Abstract

The invention relates to a preparation method of porous perfluorinated sulfonic acid resin for catalysts, wherein the preparation method comprises that perfluoro(sulfonyl vinyl)ether and tetrafluoroethylene are polymerized under the condition of co-existence of a solvent, a pore-forming agent and an initiating agent to obtain the product, the perfluorinated sulfonic acid resin having low equivalent weight and low molecular weight is used as the pore-forming agent, the solvent is recycled by a way of adding deionized water and a dispersant and carrying out distillation, at the same time, the resin is molded, after further drying, a granular material is obtained, and moreover, a mixture of one or more of perfluorinated hydrocarbon / perfluorinated cyclic ether / chlorofluorocarbon are used as an extraction agent for extracting the pore-forming agent so as to form a porous structure. The method has simple operating conditions, has no need for high temperature and high pressure, and solves the problem in the prior art that effective catalytic component loss is difficult to overcome during a using process, and the service life of the catalyst is increased; and at the same time, due to the existence of the porous structure, the specific surface area is increased, and the active component utilization rate is improved.

Description

technical field [0001] The invention relates to a method for preparing a porous perfluorosulfonic acid resin used as a catalyst, in particular to a method for synthesizing a perfluorosulfonic acid resin type porous strong-acid cation exchange resin catalyst by using a low-molecular polymer as a porogen. Background technique [0002] Since the perfluorosulfonic acid resin was prepared in the 1960s by American DuPont scientist Connolly, it has been widely used as a fuel cell membrane, a diaphragm for electrolysis experiments in the chlor-alkali industry, and a solid polymer electrolyte. At the same time, it is found that it is used as a solid superacid catalyst in organic synthesis, such as alkylation, acylation, nitration, sulfonation, phosphorylation, polymerization, condensation, etherification, esterification, hydration and rearrangement reactions. catalytic effect. Compared with liquid acid catalysis, perfluorosulfonic acid resin has the advantages of non-corrosion, no w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F216/14C08F214/26C08J9/26B01J31/10B01J35/10C07C67/08C07C69/14
Inventor 王丽王凯滕培峰
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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