Method for separating straw acetylized component and preparing straw cellulose acetate

A technology of cellulose acetate and acetylation, applied in the field of utilization of straw waste resources, to achieve the effects of increasing reactivity, saving resources, and improving utilization

Inactive Publication Date: 2008-03-12
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] One of the purposes of the present invention is to develop a component separation method for the special structure of straw, which is a multi-component lignocellulosic raw material, so that the straw can be fully utilized to obtain val

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: 3 g of steam-exploded corn stalks after drying, then add equal volumes of glacial acetic acid and acetic anhydride, liquid-solid ratio 12: 1 (weight ratio), add sulfuric acid 0.03 g, add in the flask after fully mixing, in Stir at 50°C for 30min, then raise the temperature to 120°C, keep it warm for 2h, and cool to room temperature after the reaction;

[0031] Pour it into a centrifuge tube, centrifuge at 10000r / min for 10min, then separate the supernatant from the precipitate, the supernatant is the acetylated product;

[0032] Discard the precipitate; wash the supernatant with water, precipitate occurs after washing, then suction filter, wash with water until neutral, pulverize, boil, dry, and weigh the obtained acetylated product;

[0033] Then the washed supernatant precipitate is refluxed with acetone for 2 hours, the insoluble in acetone is cellulose triacetate, and the soluble in acetone is cellulose diacetate, acetylated lignin and acetylated hemic...

Embodiment 2

[0041] Embodiment 2: 3 g of steam-exploded corn stalks after drying, then add equal volumes of glacial acetic acid, acetic anhydride, liquid-solid ratio 12: 1 (weight ratio), sulfuric acid 0.11 g, add in the flask after fully mixing, at 50 ℃ Stir for 30 minutes, then heat up to 120°C, keep warm for 2 hours, and cool to room temperature after the reaction is complete;

[0042] Pour it into a centrifuge tube, centrifuge at 8000r / min for 20min, then separate the supernatant from the precipitate, the supernatant is the acetylated product;

[0043]Discard the precipitate; wash the supernatant with water, precipitate occurs after washing, then suction filter, wash with water until neutral, pulverize, boil, dry, and weigh the obtained acetylated product;

[0044] Then the washed supernatant precipitate was refluxed with acetone for 0.5h, the insoluble in acetone was cellulose triacetate, and the soluble in acetone was acetylated lignin and acetylated hemicellulose. Most of the aceto...

Embodiment 3

[0052] Example 3: 3 g of steam-exploded corn stalks after drying, then add equal volumes of glacial acetic acid, acetic anhydride, liquid-solid ratio 12: 1 (weight ratio), sulfuric acid 0.22 g, add in the flask after fully mixing, at 50 ℃ Stir for 30 minutes, then heat up to 120°C, keep warm for 2 hours, cool to room temperature after the reaction, pour it into a centrifuge tube, and centrifuge at 9000r / min for 15 minutes, then separate the supernatant from the precipitate, the supernatant is the acetylated product, discard the precipitate; wash the supernatant with water, precipitate occurs after washing, then suction filter, wash with water until neutral, pulverize, boil, dry, and weigh. Then the washed supernatant was refluxed with acetone for 1 hour, the insoluble in acetone was cellulose triacetate, and the soluble in acetone was acetylated lignin and acetylated hemicellulose. Most of the acetone was distilled off, and substances soluble in acetone after adding water prec...

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Abstract

The present invention relates to the separation of straw acetyl cellulose and a preparation method for acetate: cold acetic acid and acetic acid which are of the same volume are added into the steamed straw; the steamed straw is acetylated with under a sulfuric acid condition to generate acetic acid fibrin, acetylation half-fibrin and acetylation lignin liquid; the liquid is placed in a centrifuge for centrifugal treatment; sypernatant and deposit are obtained; the deposit is disposed and the sypernatant is reserved; after that the sypernatant is cleaned by water to produce deposit which is then filtered; The deposit is washed to neutral and is boiled and dried; acetylation products of acetic acid fibrin, acetylation lignin and acetylation half-fibrin are generated; the acetylation products are extracted by solvent; twain-acetic acid fibrin, acetylated half-fibrin and lignin dissolve in the solvent and the remained that does not dissolve in the solvent is tri-acetic acid fibrin. The present invention overcomes the shortcoming of the traditional separation method in terms of environmental pollution. The acetic acid fibrin obtained through the method can be used in industry. The acetylated lignin is improved and becomes more stable. The group separation of straw can be realized through the method.

Description

technical field [0001] The invention belongs to the field of utilization of straw waste resources, and in particular relates to a method for separating acetylated components of straw and preparing cellulose acetate from straw, that is, firstly subjecting plant straw to steam explosion pretreatment, then directly acetylating, and then performing straw component Separation and preparation of cellulose acetate, acetylated lignin, etc., enabling high-value utilization of straw resources. Background technique [0002] my country is rich in straw resources, with an annual output of more than 700 million tons. However, due to the many components and complex structure of this renewable resource, it has not been economically and rationally developed and utilized for a long time. Some current straw utilization technologies have problems such as unstable product quality, low utilization rate of raw materials, and environmental pollution. On the one hand, in recent years, with the cha...

Claims

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Application Information

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IPC IPC(8): C08B3/06D21B1/36D21C5/00
Inventor 陈洪章张建兴
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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