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A kind of solid superacid and its preparation method and application

A solid super acid, molar ratio technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of difficult to achieve large-scale continuous production, poor product batch stability, monomer Serious polymerization risk and other problems, to achieve the effect of strong positive ionization ability, great social and economic benefits, and simple steps

Active Publication Date: 2018-08-28
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the loading of silicotungstic acid is 30wt%, the molar ratio of acrylic acid / cyclohexene is 3, the amount of catalyst is 7% of the total mass of acrylic acid and cyclohexene, the reaction temperature is 95°C, and the reaction time is 9h, the conversion of cyclohexene is 83.3%, the selectivity of cyclohexene acrylate is 96.2%, but the reaction time of this process is long, the reaction temperature is high, the risk of monomer polymerization is more serious, and the adhesion of oligomers will cause the catalyst to stick together and eventually reduce the catalyst activity. , even causing the reaction to fail
Moreover, the process uses an intermittent kettle-type process, the product batch stability is not good, and it is difficult to achieve large-scale continuous production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1) Add sodium p-vinylphenolate to N,N dimethylformamide, stir evenly, add tetrabutylammonium bromide, and then add ClCF 2 Cl, of which sodium vinylphenolate and ClCF 2 The molar ratio of Cl is 1:3, and the catalyst is sodium vinylphenate and ClCF 2 Cl weight and 1 wt%, react at 30°C for 4 hours, extract and purify to obtain styrene fluoride.

[0055] 2) Mix vinyltrimethoxysilane, styrene fluoride, tetrafluoroethylene, 1,4-butanediol diacrylate, decane, and azobisisobutyronitrile in a molar ratio of 1:1:0.2: 0.05:0.2:0.01 for feeding, using suspension polymerization at 80°C to prepare polymer microspheres;

[0056] 3) Swell the polymer microspheres in methanol for 4 hours, then add concentrated sulfuric acid with a molar ratio of 1:0.5, sulfonate at 40°C for 5 hours, filter and wash with water to obtain 1# solid superacid.

[0057] 4) 1# solid superacid is analyzed by BET specific surface area detection method, and its specific surface area is 525m 2 / g, pore volume ...

Embodiment 2

[0060] 1) Add potassium p-vinylphenate to N,N dimethylacetamide, stir evenly, add tetrabutylammonium iodide, and then add Br(CF 2 ) 6 Br, where potassium vinylphenate and Br(CF 2 ) 6 The molar ratio of Br is 1:2, and the catalyst is potassium vinylphenate and Br(CF 2 ) 6 0.5wt% of Br weight and 0.5wt%, and finally reacted at 10°C for 6 hours, extracted and purified to obtain the fluoride of styrene.

[0061] 2) Vinyl triethoxysilane, styrene fluoride, tetrafluoroethylene, 1,6-hexanediol diacrylate, n-undecane, and ammonium persulfate in a molar ratio of 1:0.2:5: 0.5:2.0:0.02 for feeding, using suspension polymerization at 100°C to prepare polymer microspheres;

[0062] 3) Swell the polymer microspheres in ethanol for 3 hours, then add chlorosulfonic acid with a molar ratio of 1:5, perform sulfonation reaction at 100°C for 5 hours, filter and wash with water to obtain 2# solid superacid.

[0063] 4) 2# solid superacid is analyzed by BET specific surface area detection met...

Embodiment 3

[0066] 1) Add sodium p-vinylphenolate in dichloromethane, stir well and add tetrabutylammonium bromide, then add I(CF 2 ) 3 I, where sodium vinylphenolate and I(CF 2 ) 3 The molar ratio of I is 1:3, and the catalyst is sodium vinylphenate and I(CF 2 ) 3 3wt% of 1 weight and 3wt%, react between 50 ℃ for 2 hours at last, extract and purify, obtain the fluoride of styrene.

[0067] 2) Vinyl triphenoxysilane, styrene fluoride, tetrafluoroethylene, 1,6 hexanediol dimethacrylate, n-eicosane, and potassium persulfate in a molar ratio of 1:0.2:2 : 0.1:1:0.01 for feeding, using suspension polymerization at 85°C to prepare polymer microspheres;

[0068] 3) Swell the polymer microspheres in ether for 6 hours, then add sodium sulfite with a molar ratio of 1:3, perform sulfonation reaction at 70°C for 7 hours, filter and wash with water to obtain 3# solid superacid.

[0069] 4) 3# solid superacid is analyzed by BET specific surface area detection method, and its specific surface area...

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Abstract

The invention relates to a solid super acid and its preparation method and application. The solid super acid is a fluoride containing siloxane containing double bonds, tetrafluoroethylene and styrene as monomers, and under the action of a crosslinking agent, a porogen and an initiator, the monomers are polymerized and polymerized. It is obtained by preparing polymer microspheres after the steps such as forming the material into spheres, then removing the porogen, and then undergoing sulfonation treatment. The solid super acid is suitable for preparing the corresponding ester compound through acid-ene addition reaction of (meth)acrylic acid and olefin. On the one hand, the solid super acid can effectively reduce the reaction time and reaction temperature of the acid-ene addition process;

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a solid superacid suitable for catalyzing the synthesis of (meth)acrylic acid ester compounds by catalyzing an acid-alkene addition process. Background technique [0002] Different from the traditional esterification or transesterification method to prepare acrylates, the acid-ene addition method is a green chemical process with 100% atom utilization. The acid-ene addition process is often carried out by fixed bed and batch tank Craft achieved. Wherein (meth) tert-butyl acrylate is to be raw material with isobutylene, because the tertiary carbon ion of isobutene is more stable, whole reaction speed is fast, so (meth) tert-butyl acrylate is often prepared with continuous fixed-bed process. [0003] CN101155771A discloses a kind of synthetic method of (meth) tert-butyl acrylate, this method is with sulfuric acid etc. [0004] Solid acid is used as a catalyst, and a large amount of waste ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/36C08F230/08C08F212/14C08F214/26C08F222/14C08F2/18B01J31/10B01J31/06B01J35/10C07C67/04C07C69/54
CPCC07C67/04C08F2/18C08F8/36C08F212/14C08F214/26C08F230/08B01J31/06B01J31/10B01J35/1023B01J35/1042B01J35/1061B01J2231/32C07C69/54C08F222/102
Inventor 郭华王明永黎源鞠昌迅郑京涛赵文娟
Owner WANHUA CHEM GRP CO LTD