Load type perrhenate ionic liquid based cellulose degradation method

A technology of cellulose degradation and ionic liquid, which is applied in chemical instruments and methods, sugar production, sugar production, etc., can solve the problems of catalyst cost increase, unfavorable catalyst recovery and reuse, etc., and achieve high catalyst activity and chemical The effect of stable properties and simple processing methods

Active Publication Date: 2017-10-20
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, perrhenate can be dissolved in the solvent ionic liquid together with cellulose, which is not conducive to the recovery and reuse of the catalyst, which greatly increases the cost of the catalyst.

Method used

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  • Load type perrhenate ionic liquid based cellulose degradation method
  • Load type perrhenate ionic liquid based cellulose degradation method
  • Load type perrhenate ionic liquid based cellulose degradation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 Catalytic degradation of microcrystalline cellulose by supported N-methylimidazolium perrhenate ionic liquid

[0026] The structural formula of the loaded N-methylimidazolium perrhenate ionic liquid is shown in the following formula:

[0027]

[0028] Weigh 0.1g of microcrystalline cellulose and 2.0g of 1-allyl-3-methylimidazolium chloride ionic liquid in a 10mL reaction flask, stir well, dissolve at 100°C for 10min, add 0.05g of loaded N- Methylimidazolium perrhenate ionic liquid and 70 μL of water were heated at 150° C. for 30 minutes. After the reaction, the reaction solution was diluted with water and filtered, and the filtrate was settled to 100mL. The TRS was measured by the DNS method, and the reaction product was analyzed by high performance liquid chromatography. The TRS was 78.5.9%, and the glucose yield was 39.3%. %.

Embodiment 2

[0029] Example 2 Catalytic degradation of microcrystalline cellulose by supported 1-(3-sulfonic acid)propyl-3-methylimidazolium perrhenate ionic liquid

[0030] (1) Supported 1-(3-sulfonic acid) propyl-3-methylimidazolium perrhenate ionic liquid

[0031] The structural formula is as follows:

[0032]

[0033] The preparation method is as follows:

[0034]Add 2.0g MCM-41 molecular sieve and 1.0g chloropropyltriethoxysilane to 25mL toluene, stir at 60°C for 12h, add 1.0g imidazole, continue stirring for 12h, filter and dry to obtain intermediate A; A and 1.0g of 1,3-propane sultone were placed in 25mL of toluene, refluxed at 70°C for 24h, cooled, filtered, washed with ether, and dried in vacuum at 50°C for 8h to obtain the ionic liquid intermediate B; in 25mL of toluene Add ionic liquid intermediate B and 5mL 37% concentrated hydrochloric acid to the mixture, react at 70°C for 12h, after the reaction is complete, filter to obtain intermediate C; add intermediate C and 0.5g ...

Embodiment 3

[0038] Example 3 Catalytic degradation of microcrystalline cellulose by supported 1-(α-carboxylic acid)methyl-3-methylimidazolium perrhenate ionic liquid

[0039] (1) Supported 1-(α-carboxylic acid)methyl-3-methylimidazolium perrhenate ionic liquid

[0040] The structural formula is as follows:

[0041]

[0042] The preparation method is as follows:

[0043] Add 2.0g MCM-41 molecular sieve and 1.0g chloropropyltriethoxysilane to 25mL toluene, stir at 60°C for 12h, add 1.0g imidazole, continue stirring for 12h, filter and dry to obtain intermediate A; A and 1.0 g of ethyl chloroacetate were placed in 25 mL of toluene, refluxed at 70 ° C for 24 h, cooled, filtered, washed with ether, and dried in vacuum at 50 ° C for 8 h to obtain ionic liquid intermediate B; ionic liquid was added to 25 mL of toluene Intermediate B and 5 mL of 37% concentrated hydrochloric acid were reacted at 70°C for 12 hours. After the reaction was complete, filtered to obtain Intermediate C; Intermedia...

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Abstract

The invention relates to a load type perrhenate ionic liquid based cellulose degradation method. According to the technical scheme, the method is characterized in that cellulose is dissolved in an ionic liquid solvent, and load type perrhenate ionic liquid in which ReO4<-> is used as negative ion is used as a catalyst for degrading; the degrading reaction is carried out for 10-60min at the temperature of 120-170 DEG C; and water is added to dilute reaction liquid after the reaction is finished, and then the dilute is filtered and separated. The method is simple; the catalyst is green, environment-friendly and easily recovered; the cellulose degrading effect is good.

Description

technical field [0001] The invention belongs to the field of cellulose degradation methods, in particular to a cellulose degradation method based on loaded perrhenate ionic liquid. Background technique [0002] China is a big energy consumer, and it is difficult to achieve sustainable social and economic development solely relying on fossil energy. Biomass is widely distributed on the earth, and it is the only renewable energy that can be produced materially to form a huge industry like coal, oil and natural gas. my country is a large agricultural country with abundant agricultural and forestry biomass resources such as straw. Developing biomass energy and improving my country's energy structure is not only the need for low-carbon and environmentally friendly development, but also a necessary guarantee for future energy supply. [0003] Cellulose is an important component of lignocellulose, and various platform compounds can be generated after degradation. Strong acids su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C13K1/02B01J31/02
CPCB01J31/0284B01J31/0295C13K1/02
Inventor 王景芸门楠白雪周明东
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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