Preparation method and application of solid acid catalyst

A solid acid catalyst and solid technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as unfavorable large-scale preparation, environmental protection, and inability to meet industrial production

Inactive Publication Date: 2012-12-12
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

James Dumesic, a professor at the University of Wisconsin-Madison in the United States, reported the synthesis process of HMF. Under the condition of 180°C, acid-catalyzed dehydration reaction was used to obtain HMF, and DMSO was used to suppress side reactions. Using this process, fructose was used as raw material to prepare 5-HMF. Reaching more than 85%, but the process conditions are harsh, the reaction temperature is high, and there is a problem of separation between the product and DMSO that cannot be solved, which is not conducive to large-scale preparation
Later research work (Zhao H, Holladay J E, Zhang Z, et al. Science, 2007, 316, 1597) found that in ionic liquid, CrCl 2 It can effectively convert fructose and glucose into HMF, but the Cr catalyst pollutes the environment and is not environmentally friendly
[0004] In short, the current HMF production process still has certain defects, which cannot meet the needs of industrial production.

Method used

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  • Preparation method and application of solid acid catalyst

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preparation example Construction

[0049] The present invention also provides a method for preparing 5-hydroxymethylfurfural, the method comprising the steps of: mixing the ionic liquid, carbohydrates and the solid acid catalyst obtained by the preparation method provided by the present invention at 100-130°C ( Preferably, 105-115°C) is reacted for 1-10 hours to obtain 5-hydroxymethylfurfural; preferably, the carbohydrate is selected from glucose or fructose; the mass percentage of the carbohydrate and the ionic liquid solvent is 8-12% ; The mass percentage of the solid acid catalyst and the ionic liquid solvent is 3-7%.

[0050] The above-mentioned features mentioned in the present invention, or the features mentioned in the embodiments can be combined arbitrarily. All the features disclosed in the specification of this case can be used in combination with any combination, and each feature disclosed in the specification can be replaced by any alternative feature that can provide the same, equivalent or similar...

Embodiment 1

[0063] Preparation of Ionic Liquids and Solid Acid Catalysts

[0064] Ionic liquid 1-methyl-3-ethylimidazole bromide ([C 2 MIM]Br) was prepared by the following method: put 0.5mol of N-methylimidazole, 0.75mol of ethyl bromide and 80ml of ethyl acetate into a 250ml round bottom flask, and reflux at 80°C for 24h in an oil bath. After the reaction, the upper ethyl acetate layer was removed, and the lower oily liquid was washed repeatedly with ethyl acetate (80ml×4). After removing the upper layer of ethyl acetate, the oily liquid in the lower layer was placed in a vacuum oven, and dried in vacuum at 80°C for 12 hours to obtain [C 2 MIM] Br.

[0065] Ionic liquid 1-methyl-3-butylimidazole bromide ([C 4 MIM]Br) was prepared by the following method: put 0.5mol of N-methylimidazole, 0.75mol of 1-bromobutane and 80ml of ethyl acetate into a 250ml round bottom flask, and reflux at 80°C for 24h in an oil bath. After the reaction, the upper ethyl acetate layer was removed, and the l...

Embodiment 2

[0076] Preparation of 5-Hydroxymethylfurfural

[0077] Add 1.0g ionic liquid [C 2 MIM] Br, 100 mg glucose and 50 mg solid acid catalyst Sn-MCM-41 (50). Then the reaction tube was placed in an oil bath containing electromagnetic stirring, and reacted at 110°C for 6 hours, the conversion rate of glucose was 99%, and the yield of 5-HMF was 51%.

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Abstract

The invention discloses a preparation method and application of a solid acid catalyst. The preparation method of the solid acid catalyst comprises the following steps: (1) mixing a silicon source, an alkali source, a metallic compound and a template, and carrying out hydrothermal reaction to obtain a reaction product 1; (2) filtering the reaction product 1 to obtain a solid, and drying at 60-120 DEG C for 12-36 hours to obtain a reaction product 2; and (3) calcining the reaction product 2 at 500-600 DEG C for 3-10 hours to obtain the solid acid catalyst. The silicon source is selected from hydrophilic nano silicon oxide, sodium silicate and tetraethyl orthosilicate; the alkali source is selected from tetramethylammonium hydroxide, alkali metal hydroxide and ammonia water; the metallic compound is selected from tin tetrachloride, zirconium sulfate, sodium silicate, chromic nitrate, nickel nitrate and tetrabutyl titanate; and the template is cetyl trimethyl ammonium bromide. The solid acid catalyst disclosed by the invention can be used for preparing 5-hydroxymethylfurfural.

Description

technical field [0001] The invention relates to the field of mesoporous molecular sieve catalysts, in particular to a preparation method and application of a solid acid catalyst. Background technique [0002] 5-Hydroxymethylfurfural (or 5-Hydroxymethyl-2-furfuraldehyde, 5-HMF for short) is an important furyl compound. Because of its relatively active properties, it can be used as an intermediate for many chemicals. It is an important platform compound. It can be oxidized to obtain 2,5-diformylfuran, which can be used as a drug intermediate or polymer precursor and antibacterial agent; it can be catalyzed and oxidized to obtain an important platform compound 2,5-furandicarboxylic acid, which can be further transformed into other various compound; it can be catalytically reduced to obtain 2,5-dimethylfuran (DMF), a liquid fuel with a higher octane number and higher boiling point than ethanol; it can also be hydrolyzed to obtain the platform compound levulinic acid and the che...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03C07D307/46
Inventor 傅尧陈蒙远田玉奎邓晋罗冬芬郭庆祥
Owner UNIV OF SCI & TECH OF CHINA
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