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A method for degrading lignocellulose based on molybdenum polyoxometalates

A polyoxometalate, lignocellulose technology, applied in chemical instruments and methods, sugar production, sugar production and other directions, can solve problems such as poor cellulose degradation effect, achieve good cellulose degradation effect and simple method , the effect of high catalyst activity

Active Publication Date: 2018-06-29
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, it has been reported in the literature that phosphotungstic heteropolyacid and phosphomolybdenum heteropolyacid are used as catalysts to degrade cellulose in an aqueous system, but when these catalysts catalyze the degradation reaction of cellulose, the cellulose degradation effect is poor.

Method used

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  • A method for degrading lignocellulose based on molybdenum polyoxometalates
  • A method for degrading lignocellulose based on molybdenum polyoxometalates
  • A method for degrading lignocellulose based on molybdenum polyoxometalates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 1-hexyl-3-methylimidazole molybdate ([Hmim] 4 Mo 8 O 26 ) Catalytic degradation of microcrystalline cellulose

[0029] (一)1-hexyl-3-methylimidazole molybdate ([Hmim] 4 Mo 8 O 26 ) Preparation

[0030] [Hmim] 4 Mo 8 O 26 The structural formula is as follows:

[0031]

[0032] The preparation method is as follows:

[0033] 1) Add a certain amount of acetonitrile solvent to N-methylimidazole and bromo-n-hexane in a molar ratio of 1:1.2. 2 Under protection, react at 35-40°C for 1h, then heat to 70°C and reflux for 12h to obtain the reaction intermediate product [Hmim]Br. Add a mixture of acetonitrile and ethyl acetate with a volume ratio of 1:2 to recrystallize it. The crystals are washed with n-hexane for 2 to 3 times, and the pure intermediate [Hmim]Br is obtained by distillation and drying.

[0034] 2) Pass a certain amount of diluted [Hmim]Br aqueous solution through a cation resin exchange column for ion exchange, and the Br - Exchange for OH - ion. Collect the eff...

Embodiment 2

[0038] Example 2 1,2-Dimethyl-3-hexyl imidazole molybdate ([DHmim] 4 Mo 8 O 26 ) Catalytic degradation of microcrystalline cellulose

[0039] (1) 1,2-Dimethyl-3-hexylimidazole molybdate ([DHmim] 4 Mo 8 O 26 ) Preparation

[0040] [DHmim] 4 Mo 8 O 26 The structural formula is as follows:

[0041]

[0042] The preparation method is as follows:

[0043] 1) Add 1,2-dimethylimidazole and bromo-n-hexane into a certain amount of acetonitrile solvent at a molar ratio of 1:1.2, 2 Under protection, react at 35-40℃ for 1h, then heat to 70℃ and reflux for 12h to obtain the reaction intermediate product [DHmim]Br. Add a mixture of acetonitrile and ethyl acetate with a volume ratio of 1:2 to recrystallize it. The crystals are washed with n-hexane for 2 to 3 times, and the pure intermediate [DHmim]Br is obtained by distillation and drying.

[0044] 2) Pass a certain amount of diluted [DHmim]Br aqueous solution through a cation resin exchange column for ion exchange, and the Br - Exchange for OH - i...

Embodiment 3

[0048] Example 3 1-Hexylpyridine molybdate ([Hpy] 4 Mo 8 O 26 ) Catalytic degradation of microcrystalline cellulose

[0049] (1) 1-Hexyl pyridine molybdate ([Hpy] 4 Mo 8 O 26 ) Preparation

[0050] [Hpy] 4 Mo 8 O 26 The structural formula is as follows:

[0051]

[0052] The preparation method is as follows:

[0053] 1) Add pyridine and bromo-n-hexane into a certain amount of acetonitrile solvent at a molar ratio of 1:1.2. 2 Under protection, react at 35-40°C for 1h, then heat to 70°C and reflux for 12h to obtain the reaction intermediate product [Hpy]Br. Add a mixture of acetonitrile and ethyl acetate with a volume ratio of 1:2 to recrystallize it. The crystals are washed with n-hexane for 2 to 3 times, and the pure intermediate [Hpy]Br is obtained by distillation and drying.

[0054] 2) Pass a certain amount of diluted [Hpy]Br aqueous solution through a cation resin exchange column for ion exchange. - Exchange for OH - ion. Collect the effluent solution in batches and use AgNO 3 -...

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Abstract

The invention relates to a method for degrading lignocellulose based on molybdenum polyoxometallate. The adopted technical scheme is that cellulose is dissolved into ionic liquid, and molybdenum polyoxometallate of which the anions are Mo8O26<4-> is used as a catalyst to conduct degradation. The degradation reaction temperature is 120-170 DEG C, and the reaction time is 10-60 min. Water is added after the reaction is finished so as to dilute and filter the reacting liquid. The method not only is less in catalyst dosage and higher in TRS and glucose yield, but also is easy to recycle and has no pollution to environment.

Description

Technical field [0001] The invention belongs to the field of cellulose degradation methods, and specifically relates to a lignocellulose catalytic degradation method based on molybdenum polyoxometalate ionic liquid. Background technique [0002] With the continuous advancement of industrialization and urbanization, energy consumption continues to increase. The geological disasters and environmental problems caused by the excessive exploitation and utilization of fossil energy have threatened the survival and development of mankind. Therefore, due to environmental pressure and the limitation of fossil energy, people have to find a renewable resource that can replace fossil energy. my country is rich in agricultural and forestry resources, and the use of cellulose-rich straw, straw and other agricultural and forestry wastes to produce energy materials or chemicals has gradually become a research focus in recent years. Cellulose is the main component of lignocellulose, which can b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/18C13K1/00
CPCB01J27/188B01J31/0239B01J31/0244C13K1/00
Inventor 王景芸周明东王唯黎袁玉国付霓虹
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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