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Preparation method and application for supported catalysis/polymerization-inhibition macroporous resin microsphere

A macroporous resin, supported technology, which is applied in the field of preparation of supported catalytic/polymerization-inhibited macroporous resin beads, can solve the problems of easy self-polymerization of catalytic synthesis products, and achieve the effect of avoiding clogging and prolonging catalytic life.

Active Publication Date: 2018-11-23
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a new type of supported catalytic / polymerization-inhibiting macroporous resin pellets to solve the problem that the catalyzed synthesis product is easy to self-polymerize in the current alkenoic acid synthesis process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] In 8.6g methacrylic acid monomer and 104g styrene monomer, add 9.9g 1,4-butanediol diacrylate, 56g n-eicosane and 1.6g azobisisobutyronitrile (the molar ratio of above-mentioned substance is 0.1:1:0.05:0.2:0.01), suspended and polymerized into balls at 95° C., washed the balls with methanol to remove the porogen, and obtained 104 g of macroporous resin balls.

[0066] Beads are all dispersed in 100ml benzene, add 0.34g tetrabutyl titanate and 8.6g polymerization inhibitor 4-hydroxyl-2,2,6,6 tetramethylpiperidinyl oxygen free radicals (both and step (1 ), the molar ratios of styrene in ) were 0.001:1 and 0.05:1), and the esterification reaction was carried out at 100° C. for 2 h to obtain the supported polymerization inhibitor pellets.

[0067] Take 100g of load-type polymerization-inhibiting pellets and swell them in 100ml of acetone for 4 hours, add 200g of concentrated sulfuric acid (concentrated sulfuric acid: pellets = 1:0.5), perform sulfonation at 40°C for 5 hours...

Embodiment 2

[0077] In 43g of methacrylic acid monomer and 104g of styrene monomer, add 99g of 1,4-butanediol diacrylate, 704g of n-pentacane and 4.12g of azobisisoheptanonitrile (the molar ratio of the above substances is 0.5 :1:0.5:2:0.02), suspended and polymerized into balls at 70°C, washed the balls with ethanol to remove the porogen, and obtained 216g macroporous resin balls.

[0078] Beads are all dispersed in 250ml toluene, add 1.7g tetrabutyl titanate and 86g polymerization inhibitor 4-hydroxyl-2,2,6,6 tetramethylpiperidinyl oxygen free radicals (both and step (1) The molar ratios of styrene in the mixture were 0.005:1 and 0.5:1 respectively), and the esterification reaction was carried out at 130° C. for 5 hours to obtain the supported polymerization inhibitor pellets.

[0079] Take 150g of load-type inhibiting beads and swell in 200ml of n-hexane for 4h, add 30g of sodium sulfite (mass ratio, sodium sulfite:ball = 1:5), sulfonate at 100°C for 10h, filter and wash with water to o...

Embodiment 3

[0089] In 25.8g methacrylic acid monomer and 104g styrene monomer, add 67.8g 1,6-hexanediol diacrylate, 211g n-pentacane and 3.63g benzoyl peroxide (the molar ratio of above-mentioned substances is 0.3:1:0.3:0.6:0.015), suspended and polymerized into balls at 85° C., washed the balls with acetone to remove the porogen, and obtained 152 g of macroporous resin balls.

[0090] Beads are all dispersed in 150ml xylene, add 0.852g isopropyl titanate and 34.4g polymerization inhibitor 4-hydroxyl-2,2,6,6 tetramethylpiperidinyloxy free radicals (both with step ( The molar ratios of styrene in 1) were 0.003:1 and 0.2:1), and the esterification reaction was carried out at 115° C. for 4 hours to obtain supported polymerization inhibitor pellets.

[0091] Take 100g of supported polymerization-inhibiting pellets and swell them in 100ml of cyclohexane for 4h, add 50g of chlorosulfonic acid (mass ratio, chlorosulfonic acid: pellets = 1:2), perform sulfonation at 80°C for 5h, filter with water...

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PUM

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Abstract

The invention relates to a preparation method and application for a supported catalysis / polymerization-inhibition macroporous resin microsphere. The preparation method comprises the following steps that methacrylic acid and styrene serve as monomers, under the action of a cross-linking agent, a pore-forming agent and an initiator, monomer polymerization and polymer balling are carried out so as toobtain the macroporous resin microsphere, the microsphere is cleaned by using a solvent so as to remove the pore-foaming agent, then esterified modification is carried out with a polymerization inhibitor, and sulfonation treatment is carried out with a catalyst so as to obtain the supported catalysis / polymerization-inhibition macroporous resin microsphere. The microsphere simultaneously has the effects of catalyzing olefine acid synthesis and preventing product monomer self-polymerization, is suitable for synthesis of acrylate monomers and is particularly suitable for a fixed bed acid alkeneaddition technology.

Description

technical field [0001] The invention relates to the field of organic synthesis catalysis / inhibition of polymerization, in particular to a preparation method and application of a supported catalysis / inhibition of polymerization macroporous resin pellets. Background technique [0002] The preparation of acrylate by acid-ene addition method is a green chemical process, using a fixed-bed reactor, and the commonly used catalyst is sulfonic acid resin. CN104987288A discloses a method for synthesizing tert-butyl (meth)acrylate, and provides a special catalytic system composed of various strongly acidic cation exchange resins and polymerization inhibitors to catalyze the synthesis of tert-butyl (meth)acrylate. craft. However, (meth)acrylic acid and its products are easily polymerizable substances, and the formed oligomers adhere to the surface of the catalyst, resulting in a reduction in the activity and life of the above-mentioned catalyst. [0003] In order to reduce the polymer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38B01J31/10B01J35/10C07C69/54C07C67/08C08F8/36C08F8/14C08F212/08C08F220/06C08F222/14C08F2/18
CPCC07C67/08C08F2/18C08F8/36C08F212/08B01J31/10B01J31/38C07C2602/42B01J35/617B01J35/635B01J35/647C07C69/54C08F220/06C08F222/102C08F8/14
Inventor 郭华鞠昌迅崔纯燹郑京涛陆国太黎源
Owner WANHUA CHEM GRP CO LTD
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