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Preparation method of hemicellulose phenyl carbonate

A technology of phenyl carbonate and hemicellulose, which is applied in the field of preparation of hemicellulose phenyl carbonate, can solve the problems of the yield of hemicellulose easily degradable products, the low degree of product substitution, the generation of by-products, etc. High yield, single product and controllable degree of substitution

Inactive Publication Date: 2018-06-29
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the complexity and diversity of the hemicellulose structure, the modification process of hemicellulose has high energy consumption, large pollution, generation of by-products, low degree of product substitution, easy degradation of hemicellulose, and low product yield. problems, there is a certain distance from industrial applications in terms of performance or cost

Method used

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  • Preparation method of hemicellulose phenyl carbonate
  • Preparation method of hemicellulose phenyl carbonate
  • Preparation method of hemicellulose phenyl carbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Weigh 9g of 1-allyl-3-methylimidazole chloride in a 50mL three-neck flask, dissolve in an oil bath at 80°C, add 1g of xylan, stir magnetically for 2 hours until completely dissolved; cool the above xylan / ionic liquid to At room temperature, add 10 mL of pyridine, stir at room temperature for 0.5 h; slowly add 5.81 mL of phenyl chloroformate, and react at room temperature for 1 h; After washing 5 times, vacuum drying at 40°C for 24 hours, xylan phenyl carbonate was obtained with a yield of 78.4% and a degree of substitution of 2.0. The reaction scheme was as follows:

[0036]

[0037] Identification of xylan phenyl carbonate: the FT-IR spectrograms of xylan and xylan phenyl carbonate in this embodiment are respectively as follows figure 1 In a, b shown, by figure 1 It can be known from the b in 1770cm -1 The C=O stretching vibration peak in the ester bond appears at 3070cm -1 and 832cm -1 are the C-H stretching and bending vibration peaks on the benzene ring respe...

Embodiment 2

[0043] Weigh 9g of 1-allyl-3-methylimidazole chloride into a 50mL three-neck flask, dissolve in an oil bath at 80°C, add 1g of xylan, stir magnetically for 2 hours until completely dissolved; cool the above xylan / ionic liquid to At room temperature, add 10mL of pyridine, stir at room temperature for 0.5h; slowly add 0.83mL of phenyl chloroformate, and react at room temperature for 1h; after the reaction, use methanol to precipitate, collect the precipitate and continue to use methanol to wash 5 times, and vacuum dry at 40°C for 24h , to obtain xylan phenyl carbonate with a yield of 71.9% and a degree of substitution of 0.2. The FT-IR spectrogram of xylan and xylan phenyl carbonate in the present embodiment is as Figure 5 shown.

Embodiment 3

[0045] Weigh 9g of 1-allyl-3-methylimidazole chloride into a 50mL three-neck flask, dissolve in an oil bath at 80°C, add 1g of xylan, stir magnetically for 2 hours until completely dissolved; cool the above xylan / ionic liquid to At room temperature, add 10mL of pyridine, stir at room temperature for 0.5h; slowly add 3.32mL of phenyl chloroformate, and react at room temperature for 1h; after the reaction, use methanol to precipitate, collect the precipitate and continue to use methanol to wash 5 times, and vacuum dry at 40°C for 24h , to obtain xylan phenyl carbonate with a yield of 76.2% and a degree of substitution of 1.6. The FT-IR spectrogram of xylan and xylan phenyl carbonate in the present embodiment is as Figure 6 shown.

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Abstract

The invention discloses a preparation method of hemicellulose phenyl carbonate, and belongs to the field of biomass material modification. The method comprises the following steps: firstly, dissolvinghemicellulose in ionic liquid, and adding pyridine; then, reacting with phenyl chloroformate to obtain a hemicellulose phenyl carbonate crude product; precipitating, washing and centrifuging the crude product with an organic solvent to obtain a final product. The preparation method of the hemicellulose phenyl carbonate disclosed by the invention has the advantages of high economical efficiency, high efficiency, simple preparation process, no side reactions, high yield of product and controllable degree of substitution, and can meet the needs of different substitution degrees of hemicellulosephenyl carbonate in different application scenes. Compared with hemicellulose, the hemicellulose phenyl carbonate has significantly higher solubility, thermal stability and the like; moreover, as a structurally-controllable active intermediate, the hemicellulose phenyl carbonate can further realize various modifications of hemicellulose through nucleophilic substitution, and has a certain application value in the field of biomass high-value conversion.

Description

technical field [0001] The invention belongs to the field of biomass material modification, in particular to a preparation method of hemicellulose phenyl carbonate. Background technique [0002] With the relative depletion of petrochemical raw material reserves and the decreasing forest area in the world, there has been an upsurge in the research, development and utilization of biomass renewable resources in the world, aiming to obtain alternative non-renewable resources from renewable resources such as agricultural and forestry wastes. new materials and new energy sources. Hemicellulose is an abundant biomass resource in nature, second only to cellulose. Different from the single structural composition of cellulose, hemicellulose is a general term for a class of heteropolysaccharides containing branched chain structures. The sugar groups that make up hemicellulose mainly include xylose, mannose, galactose, glucose, arabinose, etc. The composition and structure of complex ...

Claims

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Application Information

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IPC IPC(8): C08B37/14
CPCC08B37/00
Inventor 王小慧葛文娇孙润仓
Owner SOUTH CHINA UNIV OF TECH
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