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Method for grafting polycaprolactone onto hemicellulose in polar aprotic solvent system

A polar aprotic and hemicellulose technology, which is applied in the field of high-value utilization of biomass, can solve the problems of variable structure, solubility and reactivity changes, complex hemicellulose composition, etc., and achieve strong solubility and improved The effect of processability

Inactive Publication Date: 2014-03-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the research on grafting polycaprolactone to polymer compounds such as cellulose and starch has been reported. Compared with these uniform polymer compounds, hemicellulose has complex composition, variable structure, and different solubility and reactivity with different structures. And change, so far there is no report about hemicellulose grafted polycaprolactone

Method used

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  • Method for grafting polycaprolactone onto hemicellulose in polar aprotic solvent system
  • Method for grafting polycaprolactone onto hemicellulose in polar aprotic solvent system
  • Method for grafting polycaprolactone onto hemicellulose in polar aprotic solvent system

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Embodiment 1

[0024] The hemicellulose grafted polycaprolactone of the present embodiment is in DMSO / LiCl, and its specific process is as follows:

[0025] Step 1. Hemicellulose (xylan content 85%) was vacuum dried at 50°C for 12h; the hemicellulose was dispersed in DMSO / LiCl (LiCl mass percentage 6%) and stirred at 80°C under nitrogen protection 2h, obtain hemicellulose solution;

[0026] Step 2. Slowly add caprolactone monomer dropwise according to the ratio of caprolactone monomer to hemicellulose mass ratio of 18:1, and react at 100°C for 24h;

[0027] Step 3. After the reaction solution is cooled to room temperature, add ethanol to precipitate (150ml*3 times), filter and add 150ml of dichloromethane to the precipitate, stir magnetically for 72h, filter, and dry under reduced pressure at 50°C and vacuum degree of 0.1MPa for 48h , to obtain the final product hemicellulose grafted polycaprolactone.

[0028] Infrared and hydrogen spectra of unmodified hemicellulose and hemicellulose graf...

Embodiment 2

[0036] The hemicellulose grafted polycaprolactone of the present embodiment is in DMAc / LiCl, and its specific process is as follows:

[0037] Step 1. Hemicellulose (55% xylan content) was vacuum-dried at 50°C for 12 hours; the hemicellulose was dispersed in DMAc / LiCl (0.1% LiCl by mass), stirred at 150°C under nitrogen protection 24h, obtain hemicellulose solution;

[0038] Step 2. Slowly add caprolactone monomer dropwise according to the ratio of caprolactone monomer to hemicellulose mass ratio of 52:1, and react at 30°C for 0.5h;

[0039] Step 3. After the reaction liquid is cooled to room temperature, add ethanol to precipitate (150ml*3 times), filter and add 150ml of dichloromethane to the precipitate, magnetically stir for 72h, filter, and freeze-dry at -40°C for 36h to obtain the final product Hemicellulose grafted polycaprolactone. The infrared spectrum of the prepared hemicellulose grafted polycaprolactone and figure 1 Similarly, the hydrogen spectrum is similar to ...

Embodiment 3

[0041] The hemicellulose grafted polycaprolactone of the present embodiment is in DMF / LiCl, and its specific process is as follows:

[0042] Step 1. Hemicellulose (65% xylan content) was vacuum-dried at 50°C for 12 hours; the hemicellulose was dispersed in DMF / LiCl (15% LiCl by mass), stirred at 30°C under nitrogen protection 0.1h, obtain hemicellulose solution;

[0043] Step 2. Slowly add caprolactone monomer dropwise according to the ratio of caprolactone monomer to hemicellulose mass ratio of 0.5:1, and react at 150° C. for 16 hours;

[0044] Step 3. After the reaction solution is cooled to room temperature, add ethanol to precipitate (150ml*3 times), filter and add 150ml of dichloromethane to the precipitate, stir magnetically for 72h, filter, and dry under reduced pressure at 20°C and vacuum 0.1MPa for 48h , to obtain the final product hemicellulose grafted polycaprolactone.

[0045] The infrared spectrum of the prepared hemicellulose grafted polycaprolactone and figure ...

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Abstract

The invention discloses a method for grafting polycaprolactone onto hemicellulose in a polar aprotic solvent system. The method comprises the following steps: firstly dissolving hemicellulose in a polar aprotic solvent under nitrogen protection to obtain a hemicellulose liquid; then carrying out mixed reaction between a caprolactone monomer and the hemicellulose liquid under nitrogen protection according to a mass ratio of the caprolactone monomer to hemicellulose being (0.5:1)-(52:1) and controlling the reaction temperature to be 30-150 DEG C and the reaction time to be 0.5-50 hours; and pouring a reaction liquid into precipitating agents to be precipitated, filtering the liquid and washing and drying the precipitate, thus obtaining the end product. The method has the beneficial effects that the method is simple to operate and is efficient; the prepared hemicellulose derivative is soluble in water; the processability of hemicellulose is improved; and technical support is provided for producing industrial new materials with the hemicellulose raw material.

Description

technical field [0001] The invention relates to the application of hemicellulose, in particular to a method for grafting polycaprolactone to hemicellulose in a polar aprotic solvent, and belongs to the field of high-value utilization of biomass. Background technique [0002] Hemicellulose is one of the main components of agricultural and forestry biomass, and its content is second only to cellulose. It has the advantages of cheap and easy to obtain, abundant sources, renewable and biodegradable. Due to the disadvantages of complex structure, low degree of polymerization, and poor film-forming properties, hemicellulose resources have not been effectively developed and utilized. With the increasing shortage of non-renewable resources such as petrochemicals and the emphasis on environmental pollution in various countries, how to effectively utilize hemicellulose is a research hotspot in the efficient utilization of agricultural and forestry biomass resources. Due to the poor s...

Claims

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Application Information

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IPC IPC(8): C08G63/08C08G63/81C08B37/14
Inventor 刘传富张雪琴孙润仓陈铭杰陈超羿
Owner SOUTH CHINA UNIV OF TECH
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