Novel solid acid catalyst preparation method

A solid acid catalyst, a new type of technology, applied in catalyst activation/preparation, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problems of non-reusable catalyst, long carbonization and sulfonation time, long reaction time, etc. The effect of easy separation, easy recovery and simple preparation method

Inactive Publication Date: 2008-08-27
HUAQIAO UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional biodiesel production process uses liquid acid and alkali as catalysts, and there are mainly the following problems: a. A large amount of liquid acid added is easy to cause coking; b. After the reaction is completed, a large amount of alkali needs to be added to neutralize sulfuric acid; c. The residue after vacuum distillation There are a lot of coke and impure glycerin, which is difficult to recycle; d. It will produce a lot of acidic or high-salt wastewater; e. The catalyst cannot be reused, and the cost is high
However, most solid acid catalysts generally have the problems of difficult preparation, low activity, long reaction time, and easy deactivation.
Sulfonated amorphous carbon is a promising solid acid catalyst, but it needs to be heated under the isolation of oxygen during the preparation process. As described in the patent 200610036699.2, the preparation of the catalyst in the patent application needs to be carried out under oxygen-free conditions. And the carbonization and sulfonation time is longer, it should be 10~30h

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Weigh 40.0g of glucose and 40.0g of sucrose respectively, add 250ml of porous glass balls, burn at 300°C for 30 minutes, stir to disperse the glass balls evenly, continue burning for 180 minutes to obtain a tan solid, wash until the eluate is clear After drying, add 500ml of concentrated sulfuric acid (>96%) to it, react at 160°C for 5h, and cool to room temperature. Slowly add the sulfonated and cooled particles into 1000ml of distilled water, stir, and stand still to obtain a black solid precipitate, then wash it repeatedly with distilled water at 80°C until the eluate is neutral, and finally remove the washed black solid precipitate Put the thing in oven and dry, promptly obtain the solid acid catalyst of the present invention.

[0013] Application effect: put 40.00g of methanol, 25.00g of oleic acid and 5g of the solid acid catalyst prepared by the method of this example into a three-necked flask, connect the stirrer, reflux at 80°C, react for 6 hours, and the conve...

Embodiment 2

[0015] Weigh 40.0g glucose and 40.0g sucrose respectively, add 300ml porous glass balls, burn at 380°C for 10 minutes, stir to disperse the glass balls evenly, continue burning for 120 minutes to obtain a tan solid, wash until the eluate is clear After drying, add 500ml of concentrated sulfuric acid (>96%) to it, react at 120°C for 4h, and cool to room temperature. Slowly add the sulfonated and cooled particles into 1000ml of distilled water, stir, and stand still to obtain a black solid precipitate, then wash it repeatedly with distilled water at 80°C until the eluate is neutral, and finally remove the washed black solid precipitate Put the thing in oven and dry, promptly obtain the solid acid catalyst of the present invention.

[0016] Application effect: put 40.00g of methanol, 25.00g of oleic acid and 5g of the solid acid catalyst prepared by the method of this example into a three-necked flask, connect the stirrer, reflux at 80°C, react for 6 hours, and the conversion rat...

Embodiment 3

[0018] Weigh 40.0g glucose and 40.0g sucrose respectively, add 400ml porous glass balls, burn at 350°C for 20 minutes, stir to disperse the glass balls evenly, continue burning for 150 minutes to obtain a tan solid, wash until the eluate is clear After drying, add 800ml of concentrated sulfuric acid (>96%) to it, react at 160°C for 3h, and cool to room temperature. Slowly add the sulfonated and cooled particles into 1000ml of distilled water, stir, and stand still to obtain a black solid precipitate, then wash it repeatedly with 85°C distilled water until the eluate is neutral, and finally remove the washed black solid precipitate Put the thing in oven and dry, promptly obtain the solid acid catalyst of the present invention.

[0019] Application effect: put 40.00g of methanol, 25.00g of oleic acid and 5g of the solid acid catalyst prepared by the method of this example into a three-necked flask, connect the stirrer, reflux at 80°C, react for 6 hours, and the conversion rate c...

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PUM

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Abstract

The invention discloses a method for preparing a novel solid acid catalyst. The method adopts porous high temperature-resistance media as carriers and includes adding soluble sugar or starch solution; evaporating to dryness for a plurality of times; igniting; washing in water; drying; reacting with concentrated sulfuric acid; washing until a neutral condition with hot water; filtering; and drying to obtain the novel solid acid catalyst. The obtained solid acid catalyst is linked with sulfonic groups and loaded on the porous high temperature-resistance medium based on hydrophobic amorphous carbon structure prepared by calcining different glycosyl groups, and has the advantages of porosity, large specific surface area, even particle size and easy separation and filling into a tubular reactor. The catalyst has an activity higher than the conventional solid acid catalyst which can be reutilized and easily recovered and is an excellent catalyst for preparing biodiesel oil from waste edible oil such as trench oil and acidification oil.

Description

technical field [0001] The invention relates to a preparation method of a solid acid catalyst, in particular to a preparation method of a loaded solid acid catalyst capable of simultaneously catalyzing esterification and transesterification reactions. Background technique [0002] Biodiesel is a kind of biomass energy. Compared with petrochemical diesel, it does not contain sulfur and aromatics, has high cetane number, can be biodegraded, and is less harmful to the environment. It has a high flash point and is very safe for storage, use, and transportation, so it has become one of the most popular alternative energy sources for petroleum. [0003] The traditional biodiesel production process uses liquid acid and alkali as catalysts, and there are mainly the following problems: a. A large amount of liquid acid added is easy to cause coking; b. After the reaction is completed, a large amount of alkali needs to be added to neutralize sulfuric acid; c. The residue after vacuum d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053B01J37/025C07C67/08C07C67/03
CPCY02E50/13Y02E50/10
Inventor 陈国黄世丰方柏山
Owner HUAQIAO UNIVERSITY
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