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Synthetic method of propyne cellulose

A synthesis method and cellulose technology, applied in the synthesis field of propyne cellulose, can solve the problems of cumbersome process and complicated reaction, and achieve the effects of uniform reaction, simple operation and high degree of product substitution

Inactive Publication Date: 2012-08-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(2) The synthesis of propyne cellulose has not been reported in China, but Sun Fu reported it in his doctoral thesis "Synergy ATRP, click chemistry and supercritical carbon dioxide technology to prepare composite materials based on hydrogel and polyaniline (2010)" Preparation method of alkynylated nylon fiber
From the above synthesis method, whether it is to introduce propyne group into cellulose or activated nylon fiber, the prior art is synthesized through a two-step method, the process is cumbersome, the reaction is complicated, and it is a heterogeneous reaction.

Method used

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  • Synthetic method of propyne cellulose

Examples

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Embodiment 1

[0033] A kind of synthetic method of propyne cellulose of the present embodiment comprises the following steps:

[0034] (1) Wetting: add α-cellulose to N,N-dimethylacetamide to moisten for 2 hours, and the temperature of moistening is 80°C; the mass of α-cellulose and N,N-dimethylacetamide The volume ratio is 1:200, and the unit is g / ml;

[0035] (2) Dissolution: Add LiCl to the solution obtained in step (1), continue to stir for 2 hours, completely dissolve α-cellulose, and maintain the temperature at 80°C; the mass-volume ratio of LiCl to N,N-dimethylacetamide 1:25~1:10, the unit is g / ml;

[0036] (3) Reaction:

[0037] (3-1) Lower the solution obtained in step (2) to room temperature, add NaH, and stir for 10 min; wherein the molar ratio of NaH to anhydroglucose units in α-cellulose is 1:1;

[0038] (3-2) Add chloropropyne at the following ratio: the molar ratio of anhydroglucose unit in chloropropyne to α-cellulose is 3:1, and stir at room temperature for 24 hours; the...

Embodiment 2

[0046] A kind of synthetic method of propyne cellulose of the present embodiment comprises the following steps:

[0047] (1) Moisturizing: add microcrystalline cellulose to N,N-dimethylformamide to moisten for 4 hours, and the temperature of embellishment is 120°C; the mass of microcrystalline cellulose and N,N-dimethylformamide The volume ratio is 1:20, and the unit is g / ml;

[0048] (2) Dissolution: Add LiCl to the solution obtained in step (1), continue to stir for 4 hours, completely dissolve the microcrystalline cellulose, and maintain the temperature at 120°C; the mass-volume ratio of LiCl to N,N-dimethylformamide 1:10, the unit is g / ml;

[0049] (3) Reaction:

[0050] (3-1) Cool the solution obtained in step (2) to room temperature, add LiOH, and stir for 30 minutes; wherein the molar ratio of LiOH to anhydroglucose units in microcrystalline cellulose is 1:1-6:1.

[0051] (3-2) First add propyne bromide according to the following ratio: the molar ratio of propyne bro...

Embodiment 3

[0058] A kind of synthetic method of propyne cellulose of the present embodiment comprises the following steps:

[0059] (1) Wetting: add pulp and paper to N,N-dimethylacetamide to moisten for 3 hours, and the temperature of moistening is 100°C; wherein the mass volume ratio of pulp and paper to N,N-dimethylacetamide is 1: 100, the unit is g / ml;

[0060] (2) Dissolving: add LiCl to the solution obtained in step (1), continue stirring for 3 hours, completely dissolve the pulp and paper, and maintain the temperature at 100°C; wherein the mass volume ratio of LiCl to N,N-dimethylacetamide is 1 : 18, the unit is g / ml;

[0061] (3) Reaction:

[0062] (3-1) Cool the solution obtained in step (2) to room temperature, add KOH, and stir for 20 minutes; wherein the molar ratio of KOH to anhydroglucose units in pulp and paper is 3:1.

[0063] (3-2) Add chloropropyne in the following ratio: the molar ratio of chloropropyne to the anhydroglucose unit in the pulp and paper is 9:1, and st...

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Abstract

The invention discloses a synthetic method of propyne cellulose. The method comprises the following steps of: (1) wetness-swelling: adding cellulose into N,N-dimethyl acetamide or N,N-dimethyl formamide for swelling; (2) dissolving: adding LiCl into a solution obtained in the step (1), continuously stirring, and fully dissolving cellulose; (3) reacting: cooling a solution obtained in the step (2) to the room temperature, and adding a catalyst and halogenated propyne for reacting; (4) precipitating: adding a solution obtained in the step (3) into a water-ethanol mixed solution for precipitating a reaction product; (5) purifying: washing a precipitate obtained in the step (4) with ethanol and water in sequence; and (6) drying. Compared with the prior art, the method has the advantages of one-step homogeneous reaction, easiness, high synthesizing efficiency and uniform reaction.

Description

technical field [0001] The invention relates to the field of cellulose synthesis, in particular to a method for synthesizing propyne cellulose. Background technique [0002] Cellulose is a polymer glucan formed by D-glucose connected by β-1,4 glycosidic bonds. It is the main component of plant cell walls, and it is also the most widely distributed and most abundant polysaccharide in nature. In biomass cell walls, cellulose generally accounts for 40-50%, hemicellulose accounts for 10-30%, and lignin accounts for 20-30%. my country's agricultural and forestry biomass content is more than 18 billion tons, and the annual output of crop straw, forest stubble and wood processing residues is 700-1000 million tons, which can produce 300-400 million tons of cellulose, and its resource advantages are obvious. Products produced from cellulose, an abundant renewable natural polymer and its derivatives, such as pulp paper, viscose fiber, rayon, fuel ethanol, and ester derivatives such a...

Claims

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Application Information

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IPC IPC(8): C08B11/00
Inventor 彭湃曹学飞孙润仓
Owner SOUTH CHINA UNIV OF TECH
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