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Inorganic solid silicon-based sulfonic acid and/or phosphoric acid catalyst, and preparation method and application thereof

A technology of solid acid catalysts and phosphoric acid catalysts, applied in physical/chemical process catalysts, inorganic chemistry, chemical instruments and methods, etc., can solve the problems of high cost, unstable sulfonic acid group, easy to fall off, etc.

Active Publication Date: 2021-09-14
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of this type of catalytic material is complicated, the cost is high, and its structure still contains alkyl chains, which have certain swelling properties in organic reactions, making its sulfonic acid group unstable, easy to fall off and inactivated

Method used

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  • Inorganic solid silicon-based sulfonic acid and/or phosphoric acid catalyst, and preparation method and application thereof
  • Inorganic solid silicon-based sulfonic acid and/or phosphoric acid catalyst, and preparation method and application thereof
  • Inorganic solid silicon-based sulfonic acid and/or phosphoric acid catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0156]Fully dissolve 50 g of sodium silicate nonahydrate in 400 mL of deionized water to obtain a sodium silicate solution. Then add 1.8mol / L hydrochloric acid solution 200mL (the molar ratio of sodium silicate to hydrochloric acid is 0.5) in sodium silicate solution, carry out ion exchange reaction at room temperature, control pH value to be 5~6, obtain ortho silicic acid (H 4 SiO 4 )gel. Then the gel was left to stand at 60°C for 12 hours to crystallize, then filtered and washed until the filtrate was neutral. Finally, the obtained gel solid was vacuum-dried at 110° C. for 12 hours to obtain solid powder metasilicate (H 2 SiO 3 ), measuring its specific surface area to be 293m 2 / g. Add 5 g of metasilicate powder with an average particle size of 90 μm into 100 mL of concentrated sulfuric acid (concentration 98 wt%), stir, sulfonate at 130 ° C for 6 h, then cool to room temperature, filter, and wash the filter cake with deionized water until The filtrate became neutral,...

Embodiment 2

[0158] Drop 280mL of 1.8mol / L hydrochloric acid solution into 21g of tetraethylorthosilicate (0.1mol) in ethanol solution (the molar ratio of silicate to hydrochloric acid is 0.2), carry out the hydrolysis reaction at 20°C, and control the pH value to 5 ~6, to get orthosilicic acid (H 4 SiO 4 )gel. Then the gel was left to stand at 60°C for 12 hours to crystallize, then filtered and washed until the filtrate was neutral. Finally, the obtained gel solid was vacuum-dried at 110° C. for 12 hours to obtain solid powder metasilicate (H 2 SiO 3 ), measuring its specific surface area to be 305m 2 / g. Add 5 g of metasilicate powder with an average particle size of 88 μm into 100 mL of concentrated sulfuric acid, stir, sulfonate at 130 ° C for 6 h, then cool to room temperature, filter, and wash the filter cake with deionized water until the filtrate becomes neutral. The obtained white solid powder was vacuum-dried at 110°C for 5 hours, and finally, the dried sulfonated solid pow...

Embodiment 3

[0161] Embodiment 3 (application embodiment-catalyst stability)

[0162] Study on the Stability of Inorganic Solid Silicon-based Sulfonic Acid Catalytic Materials. The inorganic solid silicon-based sulfonic acid catalytic material in Example 1 of the present invention was selected to be used in the cyclohexanone oxime liquid-phase Beckmann rearrangement reaction system, and its service life was investigated. After running for 136 hours, the conversion rate of cyclohexanone oxime and the selectivity of caprolactam did not decrease significantly. The conversion rate of cyclohexanone oxime was maintained at 98%, and the selectivity of caprolactam was maintained at 99%, and the acid content was almost not decreased after the reaction.

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Abstract

The invention discloses a preparation method and application of a novel pure inorganic solid silicon-based sulfonic acid and / or phosphoric acid catalytic material. The pure inorganic solid silicon-based sulfonic acid and / or phosphoric acid catalytic material is obtained by taking metasilicic acid rich in hydroxyl groups on the surface as a raw material and bonding a sulfonic acid group and / or a phosphoric acid group to an inorganic silicon material by using a sulfonating reagent and / or phosphoric acid through a chemical bonding method. The catalytic material can be widely applied to many acid-catalyzed organic reaction fields such as isomerization reaction, esterification reaction, alkylation reaction, olefin hydroamination reaction, condensation reaction, nitration reaction, etherification reaction, multi-component reaction, oxidation reaction and the like. The inorganic solid silicon-based sulfonic acid and / or phosphoric acid catalytic material disclosed by the invention has the advantages of high acid content, high activity, good hydrothermal stability, no swelling, simple preparation process, low cost, no pollution, no corrosion, easiness in separation, reusability and the like.

Description

technical field [0001] The invention relates to a pure inorganic solid silicon-based sulfonic acid and / or phosphoric acid catalytic material with high acid content, its preparation method and application. Background technique [0002] According to statistics, about 85% of chemicals are produced through catalytic processes, and the development and application of a large number of catalytic materials has enabled the rapid development of the chemical industry. In the past, the manufacturing process, activity, lifespan and cost of new catalytic materials were developed, but hidden factors such as the environment were rarely considered. Since the beginning of the 21st century, the combination of scientific and technological innovation and environmental protection, and the simultaneous growth and sustainable development of high-efficiency enterprises and high social benefits have gradually become the goals pursued by people. Therefore, the development of green catalytic technology...

Claims

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Application Information

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IPC IPC(8): B01J27/02B01J35/10C01B33/00C01B33/113
CPCB01J27/02C01B33/00C01B33/113B01J35/617B01J35/638B01J35/615B01J35/647B01J27/182Y02P20/584B01J27/14B01J21/06B01J27/053B01J37/009B01J37/0236B01J37/036B01J37/06B01J37/08B01J37/20B01J37/28B01J37/30B01J37/343B01J37/346C07D223/10B01J35/50B01J35/613B01J35/651
Inventor 罗和安游奎一曾伊白文敬滨张雅晴袁欣雅艾秋红
Owner XIANGTAN UNIV
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