Preparation method for amino-functionalized macroporous styrene resin with large specific surface

A technology of amino functionalization and macroporous styrene, applied in the field of material science, can solve the problems of macromolecular catalytic pore size limitation, lack of pore structure, and complicated steps, and achieve improved catalytic performance and regeneration ability, simple preparation, and low cost. Effect

Inactive Publication Date: 2017-02-01
刘天泽 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention realizes the preparation of amino functionalized macroporous styrene resin material in one step, the preparation method is simple and the cost is low, overcomes the disadvantages such as complex steps, high cost and lack of pore structure in the preparation process of traditional solid alkali materials, and simultaneously solves the problem of The pore size limitation of basic zeolites on macromolecular catalysis

Method used

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  • Preparation method for amino-functionalized macroporous styrene resin with large specific surface

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Experimental program
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Effect test

Embodiment 1

[0017] Under room temperature, 1.0 gram of XAD-4 macroporous resin (purchased by Sigma-Aldrich, white spherical particles) was dispersed in 30 gram of concentrated nitric acid solution and 60 gram of concentrated sulfuric acid solution, the mass fraction of concentrated nitric acid was 35%, concentrated The mass fraction of sulfuric acid was 98%, and it was nitrated at 10°C for 72 hours, then the product was dispersed in a large amount of deionized water, washed with suction to neutrality and then dried. The obtained product had a mass of 1.5 grams.

[0018] The dried product (1.5 g) was dispersed in a mixed aqueous solution of 40 g of concentrated hydrochloric acid (37.5% by mass fraction) and 5 g of tin protochloride at room temperature for 72 hours with stirring and reduction, and the product was washed with a large amount of water and dried, and the resulting product quality was 1.46 g .

[0019] Disperse 1.46 g of the above product in 30 ml of n-butylamine and stir at roo...

Embodiment 2

[0021] Get 1.0 grams of XAD-4 macroporous resin and disperse in 5 grams of concentrated nitric acid solution (mass fraction is 35%) and 15 grams of concentrated sulfuric acid solution (mass fraction is 98%), nitrate under the condition of 0 ℃ for 12 hours, then the product is dispersed In a large amount of deionized water, filter and wash to neutrality and then dry, the obtained product has a mass of 1.53 g. The dried product was then dispersed in a mixed aqueous solution of 10 grams of concentrated hydrochloric acid (37.5% by mass) and 1 gram of stannous chloride and reduced for 12 hours at room temperature. The product was washed with a large amount of water and then dried. The resulting product had a quality of 1.54 grams. Then be dispersed in 30 milliliters of n-butylamines and activate 2 times (operating procedure is the same as embodiment 1), dry after suction filtration and obtain the specific surface area of ​​product product is 800m 2 / g, the pore volume reaches 1.13c...

Embodiment 3

[0023] Get 1.0 gram of XAD-4 macroporous resin and be dispersed in 15 gram nitric acid solution (mass fraction is 35%) and 40 gram sulfuric acid solution (mass fraction is 98%), nitrate under the condition of 5 ℃ for 50 hours, then product is dispersed in a large amount of In deionized water, suction-filtered and washed until neutral, and then dried, the obtained product had a mass of 1.61 g. The dried product was then dispersed in a mixed aqueous solution of 20 grams of concentrated hydrochloric acid (37.5 percent by mass) and 2.5 grams of stannous chloride and reduced for 56 hours at room temperature. The product was washed with a large amount of water and then dried. The resulting product had a quality of 1.52 grams. Then disperse in 30 milliliters of n-pentylamine and activate twice, dry to obtain the specific surface area of ​​the product product after suction filtration is 710m 2 / g, the pore volume reaches 1.0cm 3 / g, the pore diameter is 20.2 nanometers, and the amino...

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Abstract

The invention provides a preparation method for amino-functionalized macroporous styrene resin with a large specific surface, belonging to the technical field of material science. According to the invention, an amino-functionalized macroporous styrene resin material is successfully prepared by using a one-step method; an amino group is immobilized on the skeleton of the hydrophobic macroporous styrene resin material (XAD-4); and the material with abundant pore structures, a large specific surface area and the unique hydrophobic and lipophilic skeleton substantially overcomes problems caused by scarcity of pore structures of traditional solid alkali and hydrophilicity of skeletons in the prior art, and the excellent acid and alkali resistance of the polymer skeleton improves the stability of the material in catalytic process. The preparation method provided by the invention is of important theoretical research significance and practical application value to development of novel highly-efficient renewable solid alkali materials.

Description

technical field [0001] The invention belongs to the technical field of material science, and in particular relates to a preparation method of a large specific surface and amino functionalized macroporous styrene resin. Background technique [0002] As a kind of important catalytic process, base catalysis has important application value in the fields of petrochemical industry and fine chemical industry. Common acid-catalyzed processes in industry mainly use sodium hydroxide, potassium hydroxide, etc. as catalysts. Although it has excellent catalytic performance, it has a series of disadvantages such as: strong corrosion, difficult recycling, and environmental pressure caused during use, which greatly limit its wide application in industry. In recent years, the use of solid bases to replace traditional base catalysts in many types of base-catalyzed reactions has become a hot topic in the research of green chemistry and sustainable chemistry in recent years. Compared with con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F12/08C08F8/32B01J31/06C07C253/30C07C255/34
CPCC08F8/32B01J31/06B01J35/1023B01J35/1042B01J35/1047B01J35/1061B01J2231/4205C07C253/30
Inventor 刘天泽王晓玲
Owner 刘天泽
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