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Super-macroporous fluorine-containing superacid catalytic resin and synthesis method thereof

A technology of catalytic resin and synthesis method, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc. It can solve the problems of unstable pores, expensive perfluorinated porous catalytic resins, blocked pores, etc.

Pending Publication Date: 2022-02-01
上海漫关越水处理有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And because the perfluoroalkyl chain is very soft, even without the swelling of organic solvent, the perfluoroalkyl superacid resin with porous structure is very easy to deform and block the pores
[0017] CN1337891A has introduced the preparation method of porous perfluorosulfonic acid resin catalyst in detail, adopts SO 2 or CO 2 Heating the mixture of high-pressure gas and Nafion perfluorosulfonic acid resin to 150~300℃, and then depressurizing and bursting to prepare porous superacid catalytic resin, the porous specific surface area can reach 0.1~5M 2 / g, such a small comparative area, a large amount of difluoromethanesulfonic acid is not exposed in the catalytic pores, and the catalytic efficiency is very poor; because the matrix resin is the Nafion perfluorosulfonic acid resin that adopts the chemical structure of formula F perfluorosulfonic acid monomer , without cross-linking structure, in organic solvents heated to ≥100°C, the pores of this porous catalytic resin will swell and disappear, losing catalytic performance
There are various defects in the existing superacid catalytic resins. The perfluorinated materials are too soft, and the pores of the porous superacid catalytic resins without crosslinking structure are unstable, easily deformed and blocked, and the catalytic life is not long; and the perfluorinated porous catalytic resins Very expensive and difficult to use in large quantities

Method used

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  • Super-macroporous fluorine-containing superacid catalytic resin and synthesis method thereof
  • Super-macroporous fluorine-containing superacid catalytic resin and synthesis method thereof
  • Super-macroporous fluorine-containing superacid catalytic resin and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0056] (1) Add 1000g pure water, 5g sodium dodecylbenzenesulfonate and 30g polyvinyl alcohol particles into a 2000ml Erlenmeyer flask, stir to dissolve and become transparent under heating, cool to ≤10°C, and then pour into a 3000ml stainless steel autoclave , add 105g (0.5mol) of pentafluoropropenyl hydroxyethyl sulfide, 9g (0.03mol) of bis(4-isopropenylphenyl) sulfone, 160g of tert-butylbenzene and 2g of diacyl tert-butane peroxide, seal and pump Vacuum to ≤20mmHg, then add 150g of hexafluoropropylene (1.0mol), stir slowly and keep at 30~50r / min, heat up to 50°C to initiate polymerization, the reaction is exothermic, and the inner coil is cooled by water to keep the autoclave material The temperature is lower than 70°C, the polymerization reaction ends after 2 hours, the pressure is released after cooling, and the white polymer microspheres are collected by suction filtration. Pour the white spherical particles into a 2000ml three-neck flask, add 1000ml of pure water, heat a...

Embodiment 2

[0061] 180g (1.2mol) of hexafluoropropylene was introduced, and other specific feeding and synthesis operations were the same as in Example 1;

[0062] After the chromatographic column was washed with pure water until the pH was neutral, the polymer microspheres were poured out and dried in a vacuum oven at 80°C / 20mmHg under reduced pressure to obtain 308g of white polymer microspheres, which were ultra-macroporous fluorine-containing superacid-catalyzed Resin, particle size 0.4~1.5mm, pore size 40nm~180nm, ion exchange capacity 1.6mmol / g, specific surface area 32M 2 / g

Embodiment 3

[0064] 225g (1.5mol) of hexafluoropropylene was introduced, and other specific feeding and synthesis operations were the same as in Example 1;

[0065] After the chromatographic column was washed with pure water until the pH was neutral, the polymer microspheres were poured out and dried in a vacuum oven at 80°C / 20mmHg under reduced pressure to obtain 355g of white polymer microspheres, which were ultra-macroporous fluorine-containing superacid catalyzed Resin, particle size 0.4~1.5mm, pore size 40nm~220nm, ion exchange capacity 1.4mmol / g, specific surface area 36M 2 / g.

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Abstract

The invention relates to super-macroporous fluorine-containing superacid catalytic resin with a three-dimensional cross-linked structure. The super-macroporous fluorine-containing superacid catalytic resin has super acidity of difluoromethane sulfonic acid. Due to a stable three-dimensional cross-linked structure, the super-macroporous polymer can tolerate swelling of a high-temperature organic solvent for a long time, the super-macroporous structure is very stable, the long-term stable super acid catalysis capability is kept, and the super-macroporous polymer has the huge advantages of high-efficiency cleaning, long-term repeated use and low cost in organic synthesis reactions such as esterification, etherification, epoxy group ring opening and acid catalysis rearrangement.

Description

technical field [0001] The invention is a super-macroporous fluorine-containing super strong acid catalyst resin, which is applied in the chemical industry field of organic synthesis, green and high-efficiency catalysis. Background technique [0002] Superacid is an acid whose acid strength is stronger than 98% concentrated sulfuric acid, and it is a very efficient catalyst; in a large number of organic synthesis reactions, such as esterification, etherification, rearrangement cracking or epoxy ring-opening etherification In unit organic reactions, strong acid catalysis is required. The stronger the acid strength of the catalyst, the higher the yield and the milder the reaction conditions. Compared with small molecular liquid strong acids such as sulfuric acid, the existing macroporous strong acid resin can be recycled and reused. Although the acid strength is much weaker than 98% sulfuric acid, it is clean, environmentally friendly, non-corrosive to equipment and low in cos...

Claims

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Application Information

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IPC IPC(8): C08F214/28C08F214/18C08F212/14C08F8/06C08F4/34C08F2/38B01J31/10B01J35/10C07C41/03C07C43/13C07C45/00C07C49/16
CPCC08F214/28C08F8/06C08F4/34C08F2/38B01J31/10C07C41/03C07C45/00C08F214/18C08F212/14B01J35/60C07C43/13C07C49/16
Inventor 王永军王海军王贝越
Owner 上海漫关越水处理有限公司