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A method for preparing cellulose and lignin with high-boiling alcohol as a solvent and atmospheric pressure ultrasonic assisted preparation

A high-boiling alcohol and ultrasonic technology, applied in the field of crop waste resource utilization, can solve problems such as high safety requirements, high volatility, and solvent recovery problems that have not been completely resolved, achieving high purity, reducing secondary precipitation, and realizing The effect of cleaning full utilization

Inactive Publication Date: 2016-05-11
徐州市布瑞林新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the characteristics of low molecular weight organic solvents such as low boiling point, high volatility and flammability, high pressure is generated in the pulping process, which requires high safety requirements for pulping equipment and process operations, and the problem of solvent recovery has not yet been completely solved. Therefore, low-boiling point organic solvent pulping represented by ethanol has not yet entered industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The first step: pretreatment of raw materials

[0042] Bagasse is dried, cut into small pieces, crushed, sieved with a 70-80 mesh sieve, select the part that passes through the sieve, put it in a 250ml beaker, add deionized water, heat at a constant temperature of 80°C, and assist ultrasonic treatment After 30 minutes, centrifuge again, collect the lower precipitate, and dry at 60°C for 24 hours for later use.

[0043] Step 2: Separation of Cellulose

[0044] Weigh 8g of processed bagasse powder, put it in a three-necked flask, add 96ml of 1,4-butanediol aqueous solution with a volume ratio of 80% according to the solid-to-liquid ratio (mass of raw material: volume of solvent) of 1:12 , 0.5mlH 2 SO 4 , 9mlHAc, heated to reflux at 135°C for 4.5h and assisted ultrasonic treatment for 2.5h at the same time, the ultrasonic power is 120W; then cooled to 100°C, hot filtration to separate the filter residue and filtrate.

[0045] The filter residue was soaked in 56ml of 85...

Embodiment 2

[0051] The first step: pretreatment of raw materials

[0052] After the reeds are dried, cut them into small pieces, crush them, and sieve them with a 70-80-mesh sieve, select the part that passes through the sieve, put them in a 250ml beaker, add deionized water, heat at a constant temperature of 80°C, and assisted ultrasonic treatment for 30 minutes , and centrifuged again, the lower precipitate was collected, and dried at 60° C. for 24 hours for later use.

[0053] Step 2: Separation of Cellulose

[0054] Weigh 8g of the treated reed powder and place it in a three-necked flask, add 80ml of 1,3-butanediol aqueous solution with a volume ratio of 80% according to the solid-to-liquid ratio (mass of raw material: volume of solvent) of 1:10, 0.5mlH 2 SO 4 , 8mlHAc, heated to reflux at 140°C for 4h and assisted ultrasonic treatment for 2.5h at the same time, the ultrasonic power was 120W; then cooled to 100°C, hot filtration to separate the filter residue and filtrate.

[0055...

Embodiment 3

[0061] The first step: pretreatment of raw materials

[0062] After the straw is dried, cut it into small pieces, crush it, and sieve it with a 70-80 mesh sieve, select the part that passes through the sieve, put it in a 250ml beaker, add deionized water, heat at a constant temperature of 80°C, and assisted ultrasonic treatment for 30 minutes , and centrifuged again, the lower precipitate was collected, and dried at 60° C. for 24 hours for later use.

[0063] Step 2: Separation of Cellulose

[0064] Weigh 8g of the treated rice straw powder, put it in a three-necked flask, add 88ml of 1,4-butanediol aqueous solution with a volume ratio of 75% according to the solid-to-liquid ratio (mass of raw material: volume of solvent) of 1:11, 0.5mlH 2 SO 4 , 9mlHAc, heated to reflux at 135°C for 4.5h and assisted ultrasonic treatment for 2.5h at the same time, the ultrasonic power is 120W; then cooled to 100°C, hot filtration to separate the filter residue and filtrate.

[0065] The f...

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Abstract

The invention discloses a normal pressure ultrasonic-assisted method for preparing cellulose and lignin by using high boiling alcohol as a solvent. The method comprises the following steps: firstly treating plant raw materials to obtain plant raw material powder; adding the powder into a high boiling alcohol water solution with volume fraction of A, then adding a composite catalyst formed by H2SO4 and HAc, carrying out normal pressure boiling reflux for 3.5-5 hours under ultrasonic assistance and filtering the solution to obtain filtrate and filter residues; soaking the filter residues into a high boiling alcohol water solution with volume fraction of B for at least one time, washing the filter residues obtained through filtration by water for at least one time and then centrifugally separating, drying and grinding the filter residues to obtain the cellulose; mixing the filtrate generated through filtration each time, adding alkaline liquor into the filtrate to adjust the filtrate to be neutral, carrying out standing and suction filtration on the obtained filter residues and then washing and drying the filter residues, thus obtaining the lignin, wherein the volume fraction B is more than the volume fraction A. With the assistance of the composite catalyst and ultrasonic, the cellulose and the lignin are obtained by using crop wastes as the raw materials and carrying out separation under mild conditions.

Description

technical field [0001] The invention relates to the field of utilization of crop waste resources, in particular to a method for assisting the preparation of cellulose and lignin by using high-boiling alcohol as a solvent under normal pressure ultrasonic waves. Background technique [0002] As a huge green resource, cellulose has attracted the attention of many scientists due to its renewability, biocompatibility, degradability and derivatization. [0003] As we all know, cellulose, lignin and hemicellulose constitute the main components of the plant skeleton, among which cellulose and lignin are valuable non-petroleum resources that can be provided by nature, and exist in a large amount in various wood raw materials and non-wood raw materials. Widely used in various industries to improve people's livelihood. Since the 1990s, with people's further understanding of environmental protection and oil resource crisis, the development and utilization of cellulose and lignin have a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D21C5/00C08H7/00
Inventor 李文江童庆王学武
Owner 徐州市布瑞林新材料有限公司