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Preparation method of highly cross-linked macroporous/mesoporous solid acid catalyst

A solid acid catalyst, high cross-linking technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the mechanical properties of low surface area and macroporous polymers Poor problems, to achieve the effect of high yield

Inactive Publication Date: 2015-01-07
JIANGSU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, macroporous polymers synthesized only with surfactants have the disadvantages of poor mechanical properties and low surface area

Method used

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  • Preparation method of highly cross-linked macroporous/mesoporous solid acid catalyst
  • Preparation method of highly cross-linked macroporous/mesoporous solid acid catalyst
  • Preparation method of highly cross-linked macroporous/mesoporous solid acid catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0033] A preparation method of highly cross-linked macroporous / mesoporous solid acid catalyst: its steps include the following steps:

[0034] (1) Synthesis of hydrophobic silica particles

[0035] Add 5.8mL tetraethyl orthosilicate (TEOS) to 85mL CH 3 CH 2 OH and 9mL H 2 O aqueous solution, then add 3mL of 22% NH 3 ·H 2 O, stirred at 800rpm / min at 30°C for 1-1.5 hours, centrifuged at 8000-10000rpm at high speed, and dried in a vacuum oven at 80°C for 3-4 hours to obtain hydrophilic silica particles. Prepare 0.9g of silica particles, 140mL of toluene, 8mL of water and 3.2mL of γ-methacryloxypropyltrimethoxysilane (KH-570), mix them at 40°C for 20-24 hours, and centrifuge at a high speed , and dried in a vacuum oven at 60-80° C. for 3-4 hours to obtain hydrophobic silicon dioxide particles.

[0036] (2) Preparation of polymers based on water-in-oil Pickering high internal phase emulsion polymerization and highly cross-linked macroporous / mesoporous solid acid catalysts

...

Embodiment 2

[0051] A preparation method and application of a highly cross-linked macroporous / mesoporous solid acid catalyst, characterized in that it is carried out according to the following steps:

[0052] (1) Synthesis of hydrophobic silica particles

[0053] Add 6mL tetraethyl orthosilicate (TEOS) to 90mL CH 3 CH 2 OH and 11 mL H 2 O aqueous solution, then add 3.14mL of 25% NH 3 ·H 2 O, stirred at 30°C at 600rpm / min for 1-1.5 hours, centrifuged at high speed, and dried in a vacuum oven at 60-80°C for 3 hours to obtain hydrophilic silica particles. Prepared 1g of silica particles, 150mL of toluene, 15mL of water and 3.5mL of γ-methacryloxypropyltrimethoxysilane (KH-570), mixed at 40°C for 20-24 hours, after high-speed centrifugation, Dry in a vacuum oven at 60° C. for 3 to 4 hours to obtain hydrophobic silicon dioxide particles.

[0054] (2) Preparation of polymers based on water-in-oil Pickering high internal phase emulsion polymerization and highly cross-linked macroporous / meso...

Embodiment 3

[0061] A preparation method and application of a highly cross-linked macroporous / mesoporous solid acid catalyst, characterized in that it is carried out according to the following steps:

[0062] (1) Synthesis of hydrophobic silica particles

[0063] Add 5.9mL tetraethyl orthosilicate (TEOS) to 88mL CH 3 CH 2 OH and 10mL H 2 O aqueous solution, then add 3.12mL of 22-25% NH 3 ·H 2 O, stirred at 600-800rpm / min at 30°C for 1-1.5 hours, centrifuged at a high speed, and dried in a vacuum oven at 70°C for 3-4 hours to obtain hydrophilic silica particles. The prepared 0.95g di Mix silica particles, 145mL toluene, 12mL water and 3.4mL γ-methacryloxypropyltrimethoxysilane (KH-570), stir at 40°C for 20-24 hours, centrifuge at 60-80 °C in a vacuum oven for 3 to 4 hours to obtain hydrophobic silicon dioxide particles.

[0064] (2) Preparation of polymers based on water-in-oil Pickering high internal phase emulsion polymerization and highly cross-linked macroporous / mesoporous solid a...

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Abstract

The invention discloses a preparation method of a highly cross-linked macroporous / mesoporous solid acid catalyst. The preparation method comprises the following steps: synthetizing hydrophobic silicon dioxide particles; mixing the hydrophobic silicon dioxide particles, divinylbenzene (DVB), span80 and 2,2'-azobis(2-methylpropionitrile) (AIBN) in a certain ratio to form oil phase; and dissolving potassium persulfate, potassium sulfate and sodium p-styrenesulfonate (SS) in deionized water to form water phase, adding the water phase to the oil phase to form Pickering high internal phase emulsion, and performing polymerization, high crosslinking and sulfonation on the Pickering high internal phase emulsion to obtain the highly cross-linked macroporous / mesoporous solid acid catalyst. HC-PDVB-SS-SO3H produced by the preparation method can be easily and quickly separated from a reacted mixture, has remarkable acid catalytic effect and high repeatability, and can be converted to 5-hydroxymethylfurfural by catalytic cellulose in one step, and high yield can be achieved.

Description

technical field [0001] The invention belongs to the technical field of preparation of environmentally friendly functional materials, and in particular relates to a preparation method of a highly cross-linked macroporous / mesoporous solid acid catalyst. Background technique [0002] Although coal, natural gas, oil, and other non-renewable fossil resources supply most energy and chemicals today, it is unlikely that these fossil resources will meet the growing needs of humanity in the coming decades. At the same time, consumers and governments are increasingly concerned about environmental issues and environmental protection, and are paying more attention to renewable energy and products. With the development of conversion technologies, abundant biomass resources have the potential to occupy a major position as raw materials, especially renewable carbon fuels and chemicals. Among them, the platform chemical 5-hydroxymethylfurfural plays an important role in biomass energy becau...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/30C07D307/46
Inventor 彭银仙高和平曾俊徐庆涛
Owner JIANGSU UNIV OF SCI & TECH
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