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Preparation method of sulfonated cellulose

A technology of cellulose and dialdehyde cellulose, which is applied in the field of sulfonated cellulose preparation, can solve the problems of lower yield, large consumption of deionized water, time-consuming and labor-consuming, etc.

Active Publication Date: 2020-12-29
GUANGDONG IND TECHN COLLEGE
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional separation methods such as dialysis, usually using a dialysis membrane (such as 5000Da or 14000Da), will easily cause the loss of low molecular weight sulfonated cellulose, reduce the yield, and consume a large amount of deionized water, which is time-consuming and labor-intensive
Centrifugation will remove part of the dissolved sulfonated cellulose along with the supernatant, resulting in low yield and high energy consumption
The ion exchange method relies on electrostatic interaction to remove only the charged ions in the reactants, and the ion exchange resin is expensive

Method used

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  • Preparation method of sulfonated cellulose
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  • Preparation method of sulfonated cellulose

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preparation example Construction

[0030] A method for preparing sulfonated cellulose, the preparation method comprising the step of preparing sulfonated cellulose through an addition reaction between dialdehyde cellulose and a sulfonating agent, wherein the reaction medium of the addition reaction contains ethanol.

[0031] At present, in most cases, when preparing sulfonated cellulose through the addition reaction of dialdehyde cellulose and sulfonating agent, the selected reaction medium is water. However, the inventors have found that when water is used as the reaction medium, if the aldehyde group content of dialdehyde cellulose is low, the correspondingly prepared sulfonated cellulose does not have high hydrophilicity. At this time, the obtained sulfonated cellulose can be compared It is easily separated from the reaction system by conventional separation methods (such as filtration, etc.), and it is also relatively easy to purify for subsequent use. However, if the aldehyde group content of dialdehyde ce...

Embodiment 1

[0056] This example provides a method for preparing sulfonated cellulose, the preparation process is shown in figure 1 , including the following steps:

[0057] Step 1, preparation of dialdehyde cellulose.

[0058] (1) Weigh 4g microcrystalline cellulose into a 250ml Erlenmeyer flask, add 200ml distilled water, 5.28g NaIO 4 (molar ratio NaIO 4 :AGU=1:1) and 3.364g sodium chloride (molar ratio NaCl:AGU=7:3), and cover the Erlenmeyer flask with aluminum foil to prevent photocatalytic decomposition of periodate.

[0059] (2) Stir the reaction at 50° C. in a water bath for 3 hours.

[0060] (3) After the reaction is over, add 3ml of ethylene glycol and continue the reaction for 10 minutes.

[0061] (4) Filtrate and wash with deionized water for several times until the conductivity is less than 50 μS / cm, wash with ethanol twice, and then vacuum-dry to prepare absolute-dry dialdehyde cellulose.

[0062] Step 2, preparation of sulfonated cellulose.

[0063] Pipette 70ml of etha...

Embodiment 2

[0088] This embodiment is a modification of embodiment 1. Compared with embodiment 1, the only difference is that the ratio (volume ratio) of ethanol to water in step 2 is 10:0. Specifically, the steps of this embodiment include:

[0089] Step 1, preparation of dialdehyde cellulose.

[0090] (1) Weigh 4g microcrystalline cellulose into a 250ml Erlenmeyer flask, add 200ml distilled water and 5.28g NaIO 4 (molar ratio NaIO 4 :AGU=1:1) and 3.364g sodium chloride (molar ratio NaCl:AGU=7:3), and cover the Erlenmeyer flask with aluminum foil to prevent photocatalytic decomposition of periodate.

[0091] (2) Stir the reaction at 50° C. in a water bath for 3 hours.

[0092] (3) After the reaction is over, add 3ml of ethylene glycol and continue the reaction for 10 minutes.

[0093] (4) Filtrate and wash with deionized water for several times until the conductivity is less than 50 μS / cm, wash with ethanol twice, and then vacuum-dry to prepare absolute-dry dialdehyde cellulose.

...

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Abstract

The present invention relates to a sulfonated cellulose preparation method, which comprises that dialdehyde cellulose and a sulfonating agent are subjected to an addition reaction to prepare sulfonated cellulose, wherein the reaction medium of the addition reaction contains ethanol. According to the invention, a reaction medium containing ethyl alcohol is used for an addition reaction of dialdehyde cellulose and a sulfonating agent, so that the sulfonated cellulose can be easily separated from a reaction system even if the highly hydrophilic sulfonated cellulose is prepared from the dialdehydecellulose with the high aldehyde group content; and the yield of sulfonated cellulose is high by adopting the reaction medium containing ethanol.

Description

technical field [0001] The invention relates to the technical field of cellulose modification, in particular to a preparation method of sulfonated cellulose. Background technique [0002] Cellulose is oxidized by periodate to produce dialdehyde cellulose, which has active aldehyde groups, and can be modified to produce carboxylated cellulose, diol cellulose, ammoniated cellulose and sulfonated cellulose. The sulfonated cellulose is prepared by the addition reaction of bisulfite and dialdehyde cellulose, and after sulfonation, sulfonic acid groups are introduced into the 2- and 3-position carbons of the cellulose glucose unit. The reaction formula of continuous sodium periodate oxidation and sodium bisulfite sulfonation of cellulose is shown in the following formula: [0003] [0004] Sulfonated cellulose prepared by continuous sodium periodate oxidation and bisulfite sulfonation. The characteristics of sulfonated cellulose include: (1) The sulfonic acid group has strong ...

Claims

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Application Information

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IPC IPC(8): C08B15/00
CPCC08B15/00
Inventor 王宝玉李荣骆雪萍林嘉定
Owner GUANGDONG IND TECHN COLLEGE
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