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Carbon-based solid acid catalyst and preparation method thereof

A carbon-based solid acid and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve high cost, long solvothermal reaction time, solid The preparation method of acid catalyst is complex and other problems, to achieve the effect of easy recovery, good stability and high catalytic activity

Inactive Publication Date: 2014-04-02
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And the preparation method of the solid acid catalyst is complicated, the cost is high, and the solvothermal reaction time is long

Method used

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  • Carbon-based solid acid catalyst and preparation method thereof
  • Carbon-based solid acid catalyst and preparation method thereof
  • Carbon-based solid acid catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Accurately weigh 8 g of medium-temperature asphalt and 2 g of chlorosulfonated polyethylene, mix them uniformly, put them into a tube furnace, and carbonize at 500°C for 12 h under the protection of nitrogen to obtain a black solid product, which is ground and passed through 200 meshes after cooling. screen.

[0031] The obtained carbonized product was sulfonated with sulfur trioxide at 100°C for 6 h, cooled to room temperature under nitrogen protection, filtered and washed with boiling water until no Cl was detected in the eluate. - , SO 4 2- , and dry at a certain temperature to obtain a carbon-based solid acid catalyst.

[0032] The density of sulfonic acid groups detected by analysis is 4.22mmol / g, and the chlorine content is 2.23mg / g. In a reactor with a condensing reflux device, put an appropriate amount of carbon-based solid acid catalyst, add absolute ethanol and glacial acetic acid (volume ratio is about 10:1), and react in a heating device with a constant-s...

Embodiment 2

[0035] Accurately weigh 5 g of cellulose and 5 g of PVC, mix them uniformly, put them into a quartz tube, place them in a vertical tube furnace, and carbonize them at 450 °C for 8 h under the protection of nitrogen to obtain a black solid product. Pass through a 200-mesh sieve after grinding. The resulting carbonized product and oleum were sulfonated at 150°C for 6 h under the condition of a mass volume ratio of 1 g: 20 ml under nitrogen protection. After cooling to room temperature, they were filtered and washed with boiling water until no trace was detected in the eluate. Out Cl - , SO 4 2- , and dry at a certain temperature to obtain a carbon-based solid acid catalyst. The density of sulfonic acid groups detected by analysis is 1.615mmol / g, and the chlorine content is 4.81mg / g. After accurately weighing 0.2 g of catalyst and 0.1 g of conventionally pretreated cellulose, 10 ml of distilled water was added and hydrolyzed at 150 °C for 6 h. The yield of reducing sugar in t...

Embodiment 3

[0038] Accurately weigh 6 g of lignin and 4 g of chlorinated polyvinyl chloride, mix them evenly, put them into a quartz tube, place them in a vertical tube furnace, and carbonize them at 400 °C for 8 h under the protection of nitrogen to obtain a black solid product , After cooling, it is ground and passed through a 200-mesh sieve. Sulfonate the obtained carbonized product and fuming concentrated sulfuric acid at 140°C under nitrogen protection for 5h at a mass volume ratio of 1 g: 20 ml. After cooling to room temperature, filter and wash with boiling water until no trace is detected in the eluate. Out Cl - , SO 4 2- , and dry at a certain temperature to obtain a carbon-based solid acid catalyst. The density of sulfonic acid groups detected by analysis is 1.215mmol / g, and the chlorine content is 5.78mg / g. After accurately weighing 0.2 g of catalyst and 0.1 g of cellulose and mixing them, 10 ml of distilled water was added and hydrolyzed at 160 °C for 5 h. The yield of red...

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Abstract

The invention discloses a carbon-based solid acid catalyst and a preparation method thereof. The preparation method comprises the following steps: proportionally mixing carbon-containing raw materials and a chlorine-containing organic high-molecular compound, and carbonizing a mixture to obtain a black solid product; cooling and grinding the black solid product, and adding a sulfonating agent to perform sulfonating; performing cooling, filtering, washing and drying to obtain a black granular material, wherein the sulfonic group density of the black granular material is 0.1 to 5mmol / g, the chlorine content of the black granular material is 0.2 to 70mg / g, and the molar ratio of C to H to O is 1:(0.05-1.3):(0.1-1). The black granular material comprises a carbon framework and active sites, wherein aromatic carbon layer sheets which are in bridge bond connection so as to form a basic unit; the active sites are connected to the carbon layer sheets and comprise -Cl, -SO3H, -OH and -COOH. The carbon-based solid acid catalyst prepared by using the method is stable in structure, high in acidity, low in cost, good in catalytic effect, easy to recycle and wide in application prospect.

Description

technical field [0001] The invention relates to a carbon-based catalyst and a preparation method thereof, in particular to a chlorine-functionalized carbon-based solid acid catalyst and a preparation method thereof. Background technique [0002] As an important chemical catalyst, liquid acids such as sulfuric acid, phosphoric acid, and hydrochloric acid are widely used in various fields of the chemical industry. They have the advantages of strong acidity, low price, and high catalytic activity, but they also have disadvantages that cannot be ignored, such as liquid Acid pollutes the environment greatly, the catalyst is not easy to separate from the reaction system, and is highly corrosive to equipment. Under the background that people pay more and more attention to their living environment and advocate "green chemistry", liquid acid catalysts are gradually replaced by solid acid catalysts. [0003] Carbon-based solid acid catalyst is a new type of solid acid catalyst, which...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J27/10
Inventor 申曙光秦海峰蔡蓓李焕梅王春艳王艳梅
Owner TAIYUAN UNIV OF TECH
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