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Method for preparing biomass polylol by using ultrasonic waves and application thereof

A biomass polyol and ultrasonic technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of incomplete liquefaction reaction, troublesome operation, low yield, etc., and achieve the reduction of liquefaction yield , fast liquefaction rate and high output

Inactive Publication Date: 2014-04-02
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The shortcomings of the existing research mainly lie in: (1) The time required for the liquefaction reaction is long: there are a large number of three-dimensional ordered crystal structures in the cellulose molecules in the plant biomass, and there are strong hydrogen atoms between and within the molecules. bond, so the cellulose component in plant biomass is difficult to be liquefied, and generally requires a longer reaction time or a higher catalyst dosage to completely liquefy the cellulose; however, under longer reaction time or higher catalyst When the dosage is low, the lignin and hemicellulose decomposition products that have been dissolved in the solvent are easy to condense again into insoluble condensates; (2) additional heating equipment is required: general liquefaction reactions require oil baths or other heating equipment to liquefy The mixture is heated to 150-180°C; (3) the operation is cumbersome, for example, the corn stalks in CN101186560B need to be added several times; (4) the most important thing is that sometimes the liquefaction reaction is not thorough enough, resulting in a low yield, when the yield is the highest in CN101186560B (Example 6) Only polyols containing 46.6% corn stalk degradation products were obtained

Method used

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  • Method for preparing biomass polylol by using ultrasonic waves and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 80g of ethylene glycol, 20g of glycerol and 3g of p-toluenesulfonic acid into a three-necked flask equipped with a condenser tube, stir it mechanically to make it evenly mixed, add 20g of poplar wood powder (100 mesh) under stirring, and then Place in an ultrasonic cell pulverizer with an ultrasonic power of 850W and an ultrasonic frequency of 20kHz. After ultrasonication for 10 minutes, the three-neck flask was placed in a mixed solution of ice and water to cool and terminate the reaction. The yield of the obtained liquefied product (i.e. biomass polyol) was 90.7% by mass, the viscosity was 550-1100 mPa·S, and the hydroxyl value was 440- 680mgKOH / g (the determination of yield and hydroxyl value is according to the literature (Zhang Hairong, Ji Hongguo, Shi Jinzhi, etc. Research on the organic sulfonic acid catalyzed thermochemical liquefaction of eucalyptus powder. Forestry Chemistry and Industry, 2010, 30 (6): 35- 39) to carry out, the measurement of viscosity is ...

Embodiment 2

[0027] Add 80g of ethylene glycol, 20g of glycerol and 3g of sulfuric acid into a three-necked flask equipped with a condenser, first use mechanical stirring to make it evenly mixed, add 20g of bagasse (60 mesh) under stirring, and then place it in an ultrasonic In the cell pulverizer, the ultrasonic power is 750W, and the ultrasonic frequency is 30kHz; after ultrasonic 60min, the three-neck flask is placed in the ice-water mixture to cool and terminate the reaction, and the yield of the obtained liquefied product (i.e. biomass polyol) is 97.7%, and the viscosity is 435~1000mPa·S, hydroxyl value 320~460mg KOH / g.

Embodiment 3

[0029] Add 100g of phenol and 3g of p-toluenesulfonic acid into a three-necked flask equipped with a condenser, first use mechanical stirring to make it evenly mixed, add 20g of bamboo powder (80 mesh) under stirring, and then place it in an ultrasonic cell pulverizer In the process, the ultrasonic power is 1500W, and the ultrasonic frequency is 20kHz; after ultrasonication for 40min, the three-necked flask is placed in a mixture of ice and water to cool and terminate the reaction. ·S.

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Abstract

The invention discloses a method for preparing biomass polylol by using ultrasonic waves and application thereof. The method comprises the followings steps of: uniformly mixing 100 parts by mass of organic solvent, 1-6 parts by mass of catalyst and 15-40 parts by mass of plant raw material; and reacting under the action of ultrasonic waves of which the power is 650-2500W and the frequency is 15-30 kHz for 10-16 minutes to obtain biomass polylol. Compared with the conventional liquefying method, the method has the advantages of high liquefying rate, short time, no need of additional heating, easiness for operating, full liquefaction, high yield and difficulty in undergoing a condensation reaction on xylogen and a hemicellulose decomposed product. Due to the adoption of the method, plant biomass can be rapidly liquefied, plant substances can be decomposed, and the biomass polylol with large market potential is obtained.

Description

technical field [0001] The invention relates to a method for preparing biomass polyols, in particular to a method and application for preparing biomass polyols by using ultrasonic waves. Background technique [0002] Polyurethane material is one of the most important polymer materials, widely used in various fields of national defense industry and national economy. The polyols and isocyanates required for the synthesis of polyurethane materials generally come from petrochemical products. With the increasing depletion of fossil resources and the increasing environmental pollution caused by the waste of products, it is becoming more and more important to replace fossil resources with renewable resources. more and more attention from all over the world. Since plant raw materials (plant biomass) are inexhaustible and inexhaustible green resources with large reserves and rich sources, the utilization of plant biomass can effectively alleviate people's dependence on fossil resour...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/18C07C29/00
Inventor 廖兵张海荣庞浩王斌刘海露计红果石锦志
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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