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Preparation method of nanometer carbon-based solid acid

A technology of carbon-based solid acid and solid acid, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of high preparation cost, large-scale production and application of bound solid acid catalysts, and product application range Narrow problems, to achieve the effect of mild reaction conditions, energy saving, easy large-scale production, simple and feasible process

Inactive Publication Date: 2010-03-17
青岛生物能源与过程研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Based on the existing literature and patent reports, the existing solid acid catalysts still have the problems of high preparation cost and narrow product application range, which directly restricts the large-scale production and application of solid acid catalysts in chemical production

Method used

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  • Preparation method of nanometer carbon-based solid acid
  • Preparation method of nanometer carbon-based solid acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Take 4g of glucose, dissolve it in 40ml of water and stir until it becomes clear, add it to the reaction kettle and keep it warm for 10h at 175°C, take out the reaction kettle, filter and wash it, and dry it in an oven at 80°C for 12h to obtain a brown-red powder solid. Put the carbon material into a reaction kettle or a three-necked flask to react with concentrated sulfuric acid at 150°C for 15 hours, filter and wash the reactant with 100ml of boiling water to obtain a black powder solid acid. Take 0.2g of the above-mentioned solid acid and add it to a 100ml three-neck flask, then add 58.3ml of absolute ethanol, 5.7ml of acetic acid, and react in an oil bath at 70°C for 6h, the conversion rate of acetic acid is 60%, and the rate of ethyl acetate formation is 0.67mmol / min / g.

Embodiment 2

[0045] Take 4g of glucose, dissolve it in 40ml of water and stir until it becomes clear, add it to the reaction kettle and keep it warm for 10h at 175°C, take out the reaction kettle, filter and wash it, and dry it in an oven at 80°C for 12h to obtain a brown-red powder solid. Put the carbon material into a reaction kettle or a three-necked flask to react with 20% oleum at 120°C for 15 hours, filter and wash the reactant with 100ml of boiling water to obtain a black powder solid acid. Take 0.2g of the above-mentioned solid acid and add it to a 100ml three-neck flask, then add 58.3ml of absolute ethanol, 5.7ml of acetic acid, and react in an oil bath at 70°C for 3h, the conversion rate of acetic acid is 83%, and the rate of ethyl acetate generation is 2.10mmol / min / g.

Embodiment 3

[0047] Get 0.1g of the solid acid gained in Example 2, join in the 100ml three-necked flask, then add dehydrated ethanol 58.3ml, acetic acid 5.7ml, oil bath 70 ℃ of reaction 4h, acetic acid conversion rate is 73%, ethyl acetate generation rate is 3.13 mmol / min / g.

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Abstract

The invention relates to a preparation method of a nanometer carbon-based solid acid which adopts biomass as carbon source to prepare carbon precursor under the hydrothermal condition and performs sulfonation reaction to obtain the carbon-based solid acid. The method comprises the following steps: 1) adding biomass in water, stirring evenly to perform a reaction, standing at 120-200 DEG C to prepare a carbon material; 2) filtrating and washing the carbon material obtained in the step 1, drying at 25-120 DEG C to obtain the dried carbon material; 3) taking the dried carbon material obtained inthe step 2 to perform sulfonation reaction at 25-180 DEG C in the presence of sulfonating agent and obtain a carbon-based solid acid catalyst; and 4) washing the carbon-based solid acid catalyst withhot water and drying at 25-120 DEG C. The method of the invention can reduce the production cost of the solid acid and improve product performance. The prepared nanometer carbon-based solid acid can be applied to the reactions such as esterification, hydrolysis, hydration and the like.

Description

technical field [0001] The invention belongs to the preparation technology of green and energy-saving chemical materials, and specifically relates to a method for preparing nano-carbon-based solid acids by using biomass monosaccharides, starch, and cellulose as raw materials. The prepared nano-carbon-based solid acids can be applied to esterification, hydrolysis, hydration and other reactions. Background technique [0002] In recent years, with the increasingly prominent energy issues and environmental issues, human awareness of energy conservation and environmental protection has been increasing. At present, pollution in the chemical industry has become an urgent problem to be solved. People hope to realize energy-saving and green atomic economy, realize zero emission of pollution, use non-toxic and harmless raw materials, and produce environmentally friendly products. [0003] In the chemical industry, protonic acids (such as sulfuric acid, hydrochloric acid, phosphoric a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C69/14C07C67/08C13K1/06
Inventor 姜义军牟新东
Owner 青岛生物能源与过程研究所
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