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A kind of preparation method of halloysite nanotube-sulfonic acid group-cr (iii) ion acidic composite catalyst

A technology of halloysite nanotubes and composite catalysts, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve problems such as insoluble cellulose, achieve high recovery rate, good selectivity, strong The effect of catalytic efficiency

Inactive Publication Date: 2015-10-28
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, cellulose cannot be dissolved in common solvents, such as water, ethyl acetate, acetonitrile and ether, etc.

Method used

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  • A kind of preparation method of halloysite nanotube-sulfonic acid group-cr (iii) ion acidic composite catalyst
  • A kind of preparation method of halloysite nanotube-sulfonic acid group-cr (iii) ion acidic composite catalyst
  • A kind of preparation method of halloysite nanotube-sulfonic acid group-cr (iii) ion acidic composite catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A preparation method of halloysite nanotube-sulfonic acid group-Cr (III) ion acidic composite catalyst is characterized in that it is carried out according to the following steps:

[0032] 1. Catalyst Synthesis

[0033] (1) Synthesis of thiolated halloysite nanotubes:

[0034]0.8 g of the treated halloysite nanotubes were added to a three-necked flask containing 40 mL of toluene, and then 7.5 mL of silane coupling agent 3-(mercaptopropyl)trimethoxysilane was added to the whole system, and after mixing The system was heated to reflux at 110 °C for 24 h. The obtained product was filtered and washed 3 times with toluene to remove residual 3-(mercaptopropyl)trimethoxysilane, and the filtered solid was vacuum-dried at 70 °C.

[0035] (2) Synthesis of sulfonated halloysite nanotubes:

[0036] Add 0.43 g of thiol-modified halloysite nanotubes into a three-necked flask, then add 7.8 mL of 30% hydrogen peroxide, 9.5 mL of distilled water, and 8.6 mL of methanol into the sys...

Embodiment 2

[0052] A preparation method of halloysite nanotube-sulfonic acid group-Cr (III) ion acidic composite catalyst is characterized in that it is carried out according to the following steps:

[0053] 1. Catalyst Synthesis

[0054] (1) Synthesis of thiolated halloysite nanotubes:

[0055] 1.2 g of the treated halloysite nanotubes were added to a three-necked flask containing 40 mL of toluene, and then 8.5 mL of silane coupling agent 3-(mercaptopropyl)trimethoxysilane was added to the whole system, and after mixing, The system was heated to reflux at 110 °C for 24 h, the obtained product was filtered and washed 5 times with toluene to remove residual 3-(mercaptopropyl)trimethoxysilane, and the filtered solid was vacuum-dried at 80 °C.

[0056] (2) Synthesis of sulfonated halloysite nanotubes:

[0057] Add 0.57 g of mercapto-modified halloysite into a three-necked flask, then add 12.2 mL of 30% hydrogen peroxide, 10.5 mL of distilled water, and 11.4 mL of methanol into the system, ...

Embodiment 3

[0067] A preparation method of halloysite nanotube-sulfonic acid group-Cr (III) ion acidic composite catalyst is characterized in that it is carried out according to the following steps:

[0068] 1. Catalyst Synthesis

[0069] (1) Synthesis of thiolated halloysite nanotubes:

[0070] 1.0 g of the treated halloysite nanotubes were added to a three-necked flask containing 40 mL of toluene, and then 8.0 mL of silane coupling agent 3-(mercaptopropyl)trimethoxysilane was added to the whole system, and after mixing The system was heated to reflux at 110 °C for 24 h, and the obtained product was filtered and washed with toluene four times to remove residual 3-(mercaptopropyl)trimethoxysilane, and the filtered solid was vacuum-dried at 75 °C.

[0071] (2) Synthesis of sulfonated halloysite nanotubes:

[0072] Add 0.50 g of mercapto-modified halloysite into a three-necked flask, then add 10.0 mL of 30% hydrogen peroxide, 10.0 mL of distilled water, and 10.0 mL of methanol into the s...

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Abstract

The invention relates to a preparation method for a halloysite nanotube-sulfonic acid group-Cr(III) ion acid composite catalyst, which belongs to the technical field of environmental functional material preparation. Firstly, obtaining activated HNTs (halloysite nanotubes) via high temperature and acid treatment; secondly, dissolving HNTs with methylbenzene and 3-(mercaptopropyl) trimethoxysilane, grafting hydrosulphonyl on the surfaces of the HNTs, and obtaining HNTs-SH; thirdly, performing oxidation by using hydrogen peroxide with the concentration of 30 percent and methanol, and obtaining HNTs-SO3H via vacuum drying; fourthly, adding a CrCl3 solution, sequentially performing ultrasonic dispersion and dipping at the room temperature through the whole night; lastly, obtaining a composite acid catalyst HNTs-SO3H-Cr(III) via filtration and vacuum drying. The halloysite nanotube-sulfonic acid group-Cr(III) ion acid composite catalyst has large specific surface areas and relatively large bore diameters, and facilitates the adsorption and degradation of cellulose; a relatively strong acidity condition facilitates shortening reaction time and increasing product output; the preparation method has the advantages of high heterogeneous catalysis recovery rate, decrease in reaction cost and reduction of equipment loss.

Description

technical field [0001] The invention relates to a method for preparing an acidic composite catalyst by grafting a modified clay carrier on the surface, in particular to a method for preparing a halloysite nanotube-sulfonic acid group-Cr(III) ion acidic composite catalyst, which belongs to the preparation of environmental functional materials technology field. Background technique [0002] Cellulose is a biomass material composed of b-1,4-glucoside unit glucose, which has the advantage of being renewable, and catalytically derivatizes small molecules that can be converted into biofuels, such as glucose, 5-hydroxymethylfurfural (5 -HMF) and ethanol biomass energy, etc. Cellulose degradation product—5-hydroxymethylfurfural (5-HMF) is mainly produced by dehydration of glucose or fructose. The molecule contains a furan ring, an aldehyde group and a hydroxymethyl group. Its chemical properties are relatively active and can be oxidized , hydrogenation and condensation reactions t...

Claims

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Application Information

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IPC IPC(8): B01J27/02C07D307/46
Inventor 潘建明张云雷甘梦颖欧红香殷毅杰
Owner JIANGSU UNIV
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