Preparation method for mesoporous carbon-based solid acid catalyst and application of mesoporous carbon-based solid acid catalyst

A solid acid catalyst and mesoporous carbon technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, fatty acid esterification, etc., can solve problems such as difficult product purification, improper waste liquid treatment, and difficulty in continuous production. High catalytic esterification and acid reduction activity, suitable strength and uniform pore size distribution

Active Publication Date: 2014-04-02
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, concentrated sulfuric acid is the catalyst widely used in industry for acid reduction treatment through esterification. Its acid reduction effect is the most significant, but there are many problems as follows, including difficulty in product purification, corrosion of equipment by concentrated sulfuric acid catalyst, improper treatment of waste liquid, easy to cause environmental pollution, Difficulty in continuous production, etc.

Method used

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  • Preparation method for mesoporous carbon-based solid acid catalyst and application of mesoporous carbon-based solid acid catalyst
  • Preparation method for mesoporous carbon-based solid acid catalyst and application of mesoporous carbon-based solid acid catalyst
  • Preparation method for mesoporous carbon-based solid acid catalyst and application of mesoporous carbon-based solid acid catalyst

Examples

Experimental program
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Embodiment 1

[0034] Example 1. Weigh 1.6g of glucose, 0.16g of concentrated sulfuric acid and 30mL of distilled water, mix and stir to obtain a clear solution, and use supercritical carbon dioxide as a solvent to introduce it into 1g of mesoporous silica SBA-15 casting powder , wherein the mass fraction of carbon dioxide in the mixed solution is 80%, which is maintained for 2 hours. Then the mixture was dried at 100° C. for 6 hours, and then heated to 160° C. for pre-carbonization for 6 hours to obtain a carbon-silicon composite. Then put it in a tube furnace, raise the temperature to 900°C at 1°C / min under a nitrogen atmosphere, and roast for 5 hours, mix the obtained solid with 5g 2mol / L sodium hydroxide solution, and stir at room temperature for 24 hours to remove SiO, after filtering and washing, vacuum drying at 100° C. for 6 hours to obtain the mesoporous carbon material. Take 1 g of mesoporous carbon material and 20 mL of concentrated sulfuric acid, put them into a polytetrafluoroe...

Embodiment 2

[0035] Embodiment 2. Weigh 1.0g sucrose, 0.18g phosphoric acid and 30mL distilled water, mix and stir to obtain a clear solution, and use supercritical carbon dioxide as a solvent to import it into 1g of mesoporous silica MCM-48 casting powder, Wherein the mass fraction of carbon dioxide accounting for the mixture is 60%, which is maintained for 4 hours. Then the mixture was dried at 100° C. for 6 hours, and then heated to 160° C. for pre-carbonization for 6 hours to obtain a carbon-silicon composite. Then put it in a tube furnace, raise the temperature to 800°C at 5°C / min under a nitrogen atmosphere, and carbonize it for 8 hours. SiO, after filtering and washing, vacuum drying at 100° C. for 6 hours to obtain the mesoporous carbon material. Take 1 g of mesoporous carbon material and 20 mL of p-toluenesulfonic acid, put them into a polytetrafluoroethylene-lined reactor, keep at 180 °C for 10 hours, and cool to room temperature naturally. After filtering, washing with distill...

Embodiment 3

[0036] Embodiment 3. Take by weighing 2.0g glycerin, 0.12g hydrochloric acid and 30mL distilled water, mix and stir to obtain clear solution, and with supercritical carbon dioxide as solvent, it is imported in 1g mesoporous silica KIT-6 mold powder, Wherein the mass fraction of carbon dioxide accounting for the mixed liquid is 40%, which is maintained for 8 hours. Then the mixture was dried at 100° C. for 6 hours, and then heated to 160° C. for pre-carbonization for 6 hours to obtain a carbon-silicon composite. Then put it in a tube furnace, heat up to 700°C at 10°C / min under a nitrogen atmosphere, and carbonize it for 10 hours. The resulting solid is mixed with 20mL of hydrofluoric acid solution and stirred at room temperature for 24 hours to remove the mesoporous silica. , after filtering and washing, vacuum drying at 100° C. for 6 hours to obtain the mesoporous carbon material. Take 1 g of mesoporous carbon material and 20 mL of phosphoric acid, put them into a polytetrafl...

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Abstract

The invention relates to a preparation method for a mesoporous carbon-based solid acid catalyst and application of the mesoporous carbon-based solid acid catalyst. Under an acidic condition, saccharides or oligomerization phenolic aldehyde serving as a carbon source is dissolved through supercritical carbon dioxide serving as a solvent to perform pouring filling on a silicon dioxide template according to the special property of supercritical fluid; under inert atmosphere, the silicon dioxide template is carbonized at high temperature to obtain a carbon-silicon composite; a silicon dioxide casting is removed through a strong acid or strong alkaline solution; then the mesoporous carbon-based solid acid catalyst is obtained through acid modification. The mesoporous carbon-based solid acid catalyst prepared by the preparation method disclosed by the invention has a regularly ordered mesoporous duct structure with proper intensity, is larger in specific surface area and the pore volume and is higher in acid density. The catalyst is used for catalyzing the esterification acid reduction reaction of biological diesel raw materials; after the reaction, the oil acid value is reduced to be smaller than 2 mgKOH / g, and excellent solid acid catalysis performance is achieved.

Description

technical field [0001] The invention relates to the field of preparation and application of catalytic materials, in particular to the preparation of a mesoporous carbon-based solid acid catalyst and its application in catalyzing the acid reduction reaction of biodiesel raw material oil. Background technique [0002] Facing the global food shortage and the shortage of arable land, especially in my country with a large population and little land, the traditional way of producing biofuels from edible crop resources has encountered a bottleneck. This means that the development of green energy in the future must be based on cheap and easy-to-obtain non-edible raw materials that do not compete with others for food or land. In recent years, the use of non-edible oils with high acid value, such as jatropha fruit oil and waste cooking oil, to prepare biodiesel has become a hotspot of extensive research. [0003] The key to the preparation of biodiesel from oil with high acid value i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/02B01J31/02B01J27/16B01J27/24C11C3/04C10L1/02
CPCY02E50/13Y02E50/10
Inventor 姜浩锡李桂明王凌涛董秀芹张敏华
Owner TIANJIN UNIV
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