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A novel sulfonic acid polystyrene-silicon oxide hybrid solid acid catalyst and its preparation method

A solid acid catalyst, polystyrene technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the complex process, time-consuming, composition and structure adjustment Difficulties and other problems, to achieve the effects of low reaction temperature, low energy consumption, and unique catalytic properties

Inactive Publication Date: 2018-09-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of the present invention can effectively overcome the shortcomings of the existing preparation technology such as complex process, long time consumption, and difficulty in adjusting the composition and structure.

Method used

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  • A novel sulfonic acid polystyrene-silicon oxide hybrid solid acid catalyst and its preparation method
  • A novel sulfonic acid polystyrene-silicon oxide hybrid solid acid catalyst and its preparation method
  • A novel sulfonic acid polystyrene-silicon oxide hybrid solid acid catalyst and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Disperse 0.20 g of CTAB and 0.10 g of PS in 60 mL of deionized water and ethanol solution under stirring at 50 °C, and then add NH 3 .H 2 O to adjust the pH value of the solution, add 3mmol TEOS after stirring, continue stirring for 3h, and crystallize at 100°C for 12h. After the product was filtered, washed with water and dried, it was extracted with absolute ethanol solution dissolved in concentrated hydrochloric acid at 70°C for 12 hours; after the product was filtered, washed with water and dried, a white light powder was obtained. The samples were confirmed to be hollow nanospheres by TEM characterization. Mix the above materials with chlorosulfonic acid at 0°C, stir for 12 hours, return to room temperature, wash with a large amount of water until the filtrate becomes neutral, then wash with ethanol, filter and dry to obtain light yellow powder . TEM results show that the obtained product is a nanomaterial with a hollow sphere structure, with uniform particle si...

Embodiment 2

[0049] The preparation process of Example 1 was adopted, except that the mass of PS added was 0.15 g. Finally, light yellow light powder was obtained. The representation method is the same as above. TEM results show that the obtained product is a hollow spherical nanomaterial with uniform particle size and good dispersion. The overall size of the obtained hollow spherical nanoparticle is 410nm, and the outer wall thickness is 80nm. The BET specific surface area after sulfonation is 338.6m 2 / g; the pore volume is 0.32cm 3 / g; the acid content is 1.65mmol H + / g. ( figure 2 )

Embodiment 3

[0051] The preparation process of Example 1 was adopted, except that the mass of PS added was 0.20 g. Finally, light yellow light powder was obtained. The representation method is the same as above. TEM results show that the obtained product is a nano material with a hollow sphere structure, with uniform particle size and good dispersion. The overall size of the obtained hollow sphere nanoparticles is 500nm, and the outer wall thickness is 110nm. The BET specific surface area after sulfonation is 270.2m 2 / g; the pore volume is 0.28cm 3 / g; the acid content is 1.8mmol H + / g. ( image 3 )

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Abstract

The invention relates to a sulfonic acid polystyrene-silicon oxide hybrid solid acid catalyst and a preparation method. Specifically, it is a sulfonic acid functionalized polystyrene-silicon oxide composite nano hollow sphere, which consists of sulfonic acid polystyrene and silicon oxide [polystyrene: silicon oxide is = (5-50wt%): (50- 95wt%)]; has a hollow spherical shape; the acid content is between 0.5-3.0mmol / g H+, the specific surface area is 50-600m2 / g, and the pore volume is 0.1-0.4cm3 / g. The specific preparation steps are as follows: under alkaline system, cationic surfactant is used as structure directing agent, polystyrene is used as co-template agent, sodium silicate (Na2SiO3) or orthomethyl silicate (TMOS) or orthosilicate Ethyl ester (TEOS) was used as the source of inorganic silicon. After stirring, filtering and drying, polystyrene-silica nano hollow spheres were obtained. The obtained polystyrene-silicon oxide nano hollow spheres are reacted with a sulfonating agent, filtered, and dried to finally obtain a sulfonic acid polystyrene-silicon oxide hybrid solid acid catalyst. The method has few steps and takes a short time.

Description

technical field [0001] The invention relates to a sulfonic acid polystyrene-silicon oxide hybrid solid acid catalyst and a preparation method thereof, in particular to a sulfonic acid functionalized polystyrene-silicon oxide composite nano hollow sphere. Background technique [0002] Liquid inorganic acids such as sulfuric acid, nitric acid, and hydroiodic acid are commonly used industrial acid catalysts, but they corrode equipment during use, the separation of products and catalysts is difficult, and the generation of a large amount of waste acid causes serious pollution to the environment. Therefore, the development of new solid acid catalysts is currently under pressure Widespread concern. A wide variety of solid acid catalysts such as zeolite molecular sieves and heteropolyacids have been developed so far, many of which have also been used in industrial production. Among them, cation exchange resin is a kind of widely used solid acid catalyst, but its specific surface a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/10B01J35/10
Inventor 杨启华张晓敏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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