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Sulfonic acid-functionalized ordered mesoporous polymer-silicon oxide composite material and synthetic method thereof

A technology of sulfonic acid functionalization and composite materials, which is applied in the field of novel sulfonic acid functionalized ordered mesoporous polymer-silicon oxide composite materials and its synthesis, can solve the problems affecting the contact ability of organic functional groups and adsorbed substances, organic groups Uneven distribution, expensive and other problems, to achieve the effect of low price, adjustable surface acid content, and adjustable hydrophilicity and hydrophobicity

Active Publication Date: 2012-09-12
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is easy to cause organic functional groups to be randomly anchored on the mesoporous walls, and the distribution of organic groups is uneven, which is easy to cause pore enrichment, which greatly affects the contact ability between organic functional groups and adsorbed substances.
When the content of organic components increases, it is easy to cause phase separation to obtain disordered materials. At the same time, due to the relatively expensive price of the bridged organofunctionalized silicon source, the cost of synthesis increases and is uneconomical.

Method used

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  • Sulfonic acid-functionalized ordered mesoporous polymer-silicon oxide composite material and synthetic method thereof
  • Sulfonic acid-functionalized ordered mesoporous polymer-silicon oxide composite material and synthetic method thereof
  • Sulfonic acid-functionalized ordered mesoporous polymer-silicon oxide composite material and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] At 40°C, 1.60g of F127 (0.13mmol) was dissolved in 10.00g of absolute ethanol, and stirred for 1 hour to obtain solution A; 0.405g of organosilicon source 3-mercaptopropyltriethoxysilane (1.7mmol) and 1.729g Inorganic silicon source TEOS (8.3 mmol) was hydrolyzed under 1.0 g (0.2 mol / L) hydrochloric acid for 30 minutes to obtain solution B; mix the two solutions, add 1.0 g soluble resole phenolic resin (2.5 mmol), and stir at 40 ° C 2 hours. Then spread the mixed solution evenly in a petri dish, and place it at room temperature for 7 hours to volatilize the organic solvent; then transfer it to an oven at 100°C, and after 24 hours, reflux the product in a solution of 48wt% sulfuric acid for 48 hours to remove surface activity. agent; finally oxidized in 30wt% hydrogen peroxide for 24 hours, and acidified in 1mol / L sulfuric acid solution for 2 hours to obtain a sulfonic acid functionalized ordered mesoporous polymer-silicon oxide composite material. The obtained material...

Embodiment 2

[0044] At 40°C, dissolve 2.0g of F127 (0.16mmol) in 10.00g of absolute ethanol and stir for 1 hour to obtain solution A; 0.654g of organosilicon source 3-mercaptopropyltrimethoxysilane (3.3mmol) and 1.396g of inorganic Silicon source TEOS (6.7mmol) was hydrolyzed under the condition of 1.0g (0.2mol / L) hydrochloric acid for 30 minutes; mixed the two solutions to obtain solution B, added 1.0g soluble resole phenolic resin (2.5mmol), stirred at 40°C for 2 Hours. Then spread the mixed solution evenly in a petri dish, and place it at room temperature for 7 hours to volatilize the organic solvent; finally transfer it to an oven at 100°C, and after 24 hours, reflux the product in a solution of 48wt% sulfuric acid for 48 hours to remove surface activity. agent; oxidized in 30wt% hydrogen peroxide for 24 hours, and acidified in 1mol / / L sulfuric acid solution for 2 hours to prepare a sulfonic acid functionalized ordered mesoporous polymer-silicon oxide composite material. The obtained ...

Embodiment 3

[0047] At 40°C, dissolve 1.0g F127 (0.08mmol) in 10.00g absolute ethanol and stir for 1 hour to obtain solution A; 0.982g organosilicon source 3-mercaptopropyltrimethoxysilane (5mmol) and 1.040g inorganic Silicon source TEOS (5mmol) was hydrolyzed under the condition of 1.0g (0.2mol / L) hydrochloric acid for 30 minutes; mixed the two solutions to obtain solution B, added 1.0g soluble resole phenolic resin (2.5mmol), and stirred at 40°C for 2 Hour. Then spread the mixed solution evenly in a petri dish, and place it at room temperature for 7 hours to volatilize the organic solvent; finally transfer it to an oven at 100°C, and after 24 hours, reflux the product in a solution of 48wt% sulfuric acid for 48 hours to remove surface activity. agent; oxidized in 30wt% hydrogen peroxide for 24 hours, and acidified in 1mol / L sulfuric acid solution for 2 hours to prepare a sulfonic acid functionalized ordered mesoporous polymer-silicon oxide composite material. The obtained material has a...

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Abstract

The invention discloses a sulfonic acid-functionalized ordered mesoporous polymer-silicon oxide composite material and a synthetic method thereof. An ordered mesoporous polymer-silicon oxide composite material catalyst with high sulfonic acid group content is synthesized. The synthetic method comprises the following steps of: preparing a sulfydryl-functionalized ordered mesoporous polymer-silicon oxide composite material by taking phenolic resin as a carbon source, taking 3-mercaptopropyltrimethoxysilane as an organic functional group source, taking ethyl orthosilicate as an inorganic silicon source and taking a triblock copolymer as a template with a polybasic co-assembling method; and oxidizing sulfydryl to obtain the sulfonic acid-functionalized ordered mesoporous polymer-silicon oxide composite material. The high acid content of the ordered mesoporous sulfonic acid-functionalized material is (0.9-4.6mmol / g), the specific surface area is 200-500m<2> / g, the hole volume is 0.3-1.0cm<3> / g, and the pore diameter is 4-10 nanometers. The method is easy to operate, and is low in cost. The composite material can be used for catalyzing the reaction of cyclohexanone and propylene glycol to generate ketal, and the yield is up to 91 percent. The composite material can be used for catalyzing a reaction for generating acetal with butanediol, and the yield can be up to 82 percent. The composite material has a considerable application prospect in industrial catalysis.

Description

technical field [0001] The invention relates to the field of materials, and is a novel sulfonic acid functionalized ordered mesoporous polymer-silicon oxide composite material and a synthesis method thereof. Background technique [0002] Acid catalysts are widely used in organic synthesis and fine chemical production. Traditional liquid acid catalysts such as sulfuric acid and phosphoric acid are commonly used in industry. Liquid acid catalysts have many disadvantages, such as corrosive equipment, polluting the environment, not conducive to separation and recovery, and difficult to reuse. Therefore, it is of great significance to invent new catalysts to replace traditional liquid acid catalysts. Replacing traditional liquid acid catalysts with non-toxic and harmless solid acid catalysts can effectively solve the above problems, and the development of solid acid catalysts has attracted widespread attention. [0003] There are still many problems in the existing solid acid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J35/10C07D317/72C07D321/06
Inventor 万颖汪微庄鑫
Owner SHANGHAI NORMAL UNIVERSITY