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Method for preparation of sulfonate radical-functionalized large-specific surface area macroporous resin

A macroporous resin and resin technology, applied in the field of physical or chemical materials, can solve problems such as lack of pore structure, complicated steps, and pore size limitation, and achieve the effects of low cost, simple preparation method, and large specific surface area

Inactive Publication Date: 2017-03-22
SHAOXING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention firstly provides a macroporous resin, the macroporous resin realizes sulfonate functionalization through a one-step method, the preparation method is simple, and the cost is low, which overcomes the complicated steps, high cost, and lack of pore structure in the preparation process of traditional solid acid materials. At the same time, it solves the problem of acidic zeolite’s limitation of macromolecule catalytic pore size

Method used

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  • Method for preparation of sulfonate radical-functionalized large-specific surface area macroporous resin
  • Method for preparation of sulfonate radical-functionalized large-specific surface area macroporous resin
  • Method for preparation of sulfonate radical-functionalized large-specific surface area macroporous resin

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Effect test

Embodiment 1

[0017] The raw material resin selected in the following examples is the specific surface area of ​​XAD-4 macroporous resin is 1000m 2 / g, the average pore size is about 15nm, and the average particle size is 640μm.

[0018] The preparation method of macroporous resin comprises the following steps: a. disperse the purchased XAD-4 macroporous resin in dichloromethane and fully swell; b. add chlorosulfonic acid as sulfonating reagent in reaction system, macroporous resin and chlorine The mass ratio of sulfonic acid is controlled at 1 / 5-1 / 30, and the sulfonation time is adjusted between 12-36 hours; c. Disperse the sulfonated product in a large amount of water, filter it with suction, wash it, and dry it. obtaining a sulfonate-functionalized macroporous resin material; d. using the prepared sulfonate-functionalized macroporous resin to catalyze reactions such as esterification of acetic acid and cyclohexanol, condensation of benzaldehyde and ethylene glycol, and the like.

[0019...

Embodiment 2

[0025] Take 1.0 g of XAD-4 macroporous resin and disperse it in 15 g of dichloromethane to fully swell for 1 hour, then add 5 g of chlorosulfonic acid, sulfonate at 0°C for 12 hours, then disperse the product in a large amount of deionized water, and filter with suction , washed to neutral, and dried to obtain the product with a specific surface area of ​​800m 2 / g, the pore volume reaches 1.13cm 3 / g, the pore diameter is 25.2 nanometers, and the acid center content is 1.2mmol / g.

Embodiment 3

[0027] Disperse 1.0 g of XAD-4 macroporous resin in 30 g of dichloromethane and swell fully for 1 hour, then add 15 g of chlorosulfonic acid, sulfonate at 8°C for 24 hours, then disperse the product in a large amount of deionized water, and filter with suction , washed to neutral, dried to obtain the specific surface area of ​​the product product is 710m 2 / g, the pore volume reaches 1.0cm 3 / g, the pore diameter is 20.2 nanometers, and the acid center content is 2.8mmol / g.

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Abstract

The invention relates to a method for preparation of sulfonate radical-functionalized large-specific surface area macroporous resin and belongs to the technical field of physical or chemical materials. According to the method, polystyrene-polydivinylbenzene macroporous resin (XAD-4) as a raw material, methylene chloride as a solvent and chlorosulfonic acid as a sulfonation reagent undergo a reaction under mild conditions to produce the sulfonate radical-functionalized large-specific surface area macroporous resin and catalytic performances of the macroporous resin are detected in the typical acid catalyzed reaction. A mass ratio of the macroporous resin XAD-4 to chlorosulfonic acid is adjusted in a range of 1 / 5 to 1 / 30, a mass ratio of the macroporous resin to methylene chloride is adjusted in a range of 1 / 15 to 1 / 60 and a sulfonation temperature is adjusted in a range of 0 to 10 DEG C. The sulfonated product has a large specific surface area and pore volume, controlled sulfonate radical content and excellent catalytic performances in reactions such as catalyzed esterification of cyclohexyl acetate and condensation of benzaldehyde and ethylene glycol.

Description

technical field [0001] The invention relates to a preparation method of a macroporous resin with large specific surface area and sulfonate functionalization, belonging to the technical field of physical or chemical materials. Background technique [0002] As a kind of important catalytic process, acid catalysis has important application value in petrochemical and fine chemical industries. Common acid-catalyzed processes in industry mainly use liquid acids such as sulfuric acid, hydrochloric acid or hydrofluoric acid 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 acids instead of liquid acids in the catalytic reactions of various acids has become a hot topic in the research of green chemistry and sustainable chemistry in recent years. Compared wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/36C08L25/04B01J31/10C07C67/08C07C69/14C07D317/12
CPCB01J31/10B01J2231/49C07C67/08C07D317/12C08J9/36C08J2325/04C07C69/14
Inventor 柳菁
Owner SHAOXING UNIVERSITY
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