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Preparation method of composite carbon base solid acid catalyst

A technology of solid acid catalyst and composite carbon, which is applied in the preparation of organic compounds, preparation of carboxylic acid esters, chemical instruments and methods, etc., can solve the problems of expensive raw material sources, underdeveloped pore size, and difficulty in regulation, and achieve mechanical strength and stability High catalytic activity, improved acidity, and low raw material cost

Inactive Publication Date: 2012-08-01
NINGXIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the materials obtained by these methods are limited by the source of the carbon source matrix, or the source of the raw material is expensive, or the mechanical strength is poor due to the serious powderization of the product; Underdeveloped and difficult to control, acidity is not very ideal and the acidic sites on the surface are easily lost in the liquid phase reaction

Method used

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  • Preparation method of composite carbon base solid acid catalyst
  • Preparation method of composite carbon base solid acid catalyst
  • Preparation method of composite carbon base solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Preparation of composite resin:

[0019] At room temperature, take 4g of sucrose with a particle size of about 190μm, add it to a beaker filled with 40g of sodium humate solution with a mass concentration of 10%, and stir it magnetically for about 30 minutes. , a thermometer, a reflux condensing tube, and a three-necked flask of a water separator, then add 2.3ml of formalin as a crosslinking agent and 2.2g of p-toluenesulfonic acid as a catalyst; 2 Stir and heat to reflux. When the heating temperature reaches 80°C, keep the temperature constant for 12 hours; then vacuum dehydrate at 0.08MPa and dry for 4 hours to obtain a black block composite resin;

[0020] (2) carbonization

[0021] Grind the above-mentioned massive composite resin to about 200 meshes, and place it in a carbonization furnace under N 2 Under protection, after carbonization at 450°C for 8h, cool to room temperature;

[0022] (3) Washing, suction filtration and drying:

[0023] Add the above-men...

Embodiment 2-7

[0027] On the basis of the process step of above-mentioned embodiment 1, change carbohydrate, cross-linking agent, catalyst and process technology condition, specifically see the following table:

[0028]

[0029] In the above examples, the acidity (mmol / g) of the obtained sulfonated solid acid is between 1.52-1.86.

Embodiment 8-12

[0031] On the basis of the process steps of any of the above-mentioned embodiments, change the process conditions described in the table below in the sulfonation reaction step, the results are shown in the table below:

[0032]

[0033] In the above-mentioned embodiments, the drying time and temperature are determined at 110-120° C. for 2-6 hours according to the specific conditions of the materials, and the purpose is to dry the materials.

[0034] The composite carbon-based solid acid catalyst obtained in the above examples was used in the catalytic esterification reaction and the catalytic condensation reaction respectively, and the process is shown in the following examples.

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Abstract

The invention relates to preparation of a catalyst, in particular to a preparation method of a composite carbon base solid acid catalyst. The preparation method comprises the following processing steps of: preparing composite resin; carbonizing; washing with water; performing suction filtration; drying; and performing sulfonation reaction. The technical scheme provided by the invention has the characteristics that: 1, the raw materials have wide sources and are readily available; according to the preparation method, a renewable biomass base is used as a raw material, i.e., carbohydrate is used as the raw material, so that the raw materials are low in cost and have wide sources; 2, after the biomass base is modified by using a cross-linking agent, carbonized resin is formed after carbonization, so that a multi-condensed-ring carbon nuclear structure matrix is more favorably formed than direct carbonation of biomass, and meanwhile, the mechanical strength and the stability of the carbonized resin are higher than those in the prior art; and 3, the carbonized resin has low probability of forming easily soluble small molecular compound in a sulfonation process, so that more sulfonic acid groups can be linked; and thus, the reusability, the catalytic activity and the acidity of the composite carbon base solid acid catalyst are greatly improved.

Description

Technical field [0001] The invention relates to the preparation of a catalyst, in particular to the preparation method of a composite carbon-based solid acid catalyst. Background technique [0002] Solid acid catalyst is an inevitable choice to achieve green chemical industry. At present, the solid acid catalysts reported at home and abroad mainly include styrene sulfonic acid resin, polytetrafluoroethylene sulfonic acid resin and solid carbon sulfonic acid catalyst. Styrene sulfonic acid resin has the disadvantage of poor heat resistance, which limits its scope of application; although polytetrafluoroethylene sulfonic acid resin has high thermal stability, its expensive price limits its application in chemical processes. limit. [0003] In recent years, the preparation and application of solid carbon sulfonic acid catalysts have attracted the attention of academic circles. People have developed a variety of solid carbons obtained from polycyclic aromatic hydrocarbons, sug...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C69/24C07C67/08
Inventor 刘万毅李冰陈静梁世娇孙媛胡奇林
Owner NINGXIA UNIVERSITY
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