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Method for preparing cellulose carbamate through liquid-solid-phase reaction

A carbamate and cellulose technology, applied in the field of liquid-solid phase reaction to prepare cellulose carbamate, can solve problems such as difficulty in large-scale industrial production, high pressure, etc., achieve low solvent toxicity, improve reactivity, and prepare Ease of the process

Inactive Publication Date: 2014-08-13
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, supercritical conditions require high pressure (≥8Mpa), which brings certain difficulties to large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] According to the ratio of cotton pulp and urea mass ratio of 1:3, the mass ratio of cellulose pulp and solvent is 1:10 ratio, take a certain amount of cotton pulp, urea, DMF, add to the reaction with reflux condenser Then, the temperature was raised to 150°C, and the esterification reaction was maintained for 15 hours. After the reactor dropped to normal temperature, the product was taken out, washed, and dried to obtain cellulose carbamate.

Embodiment 2

[0018] According to the mass ratio of wood pulp and urea 1: 4, the mass ratio of cellulose pulp and solvent is 1: 20, weigh a certain amount of wood pulp, urea, DMAc, and add it to the reaction reaction with reflux condenser. Then, the temperature was raised to 155°C, and the esterification reaction was maintained for 20 hours. After the reactor dropped to normal temperature, the product was taken out, washed, and dried to obtain cellulose carbamate.

Embodiment 3

[0020] According to the ratio of bamboo pulp and urea mass ratio 1:6, the mass ratio of cellulose pulp and solvent is 1:15 ratio, take a certain amount of bamboo pulp, urea, DMF, add the reaction reaction with reflux condenser Then, the temperature was raised to 145°C, and the esterification reaction was maintained for 18 hours. After the reactor dropped to normal temperature, the product was taken out, washed, and dried to obtain cellulose carbamate.

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PUM

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Abstract

The invention discloses a method for preparing cellulose carbamate through a liquid-solid-phase reaction. The method comprises the following step: performing esterification reaction on cellulose pulp or activated cellulose pulp and urea as raw materials in a high-boiling-point nonprotonic strong-polarity solvent such as dimethyl formamide (DMF), dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO) or N-methylpyrrolidone (NMP) to synthesize cellulose carbamate. In the process of preparing cellulose carbamate by adopting a liquid-solid-phase method, the used solvent is low in toxicity and easy to recover; the preparation process is simple and convenient, environment-friendly, safe, and controllable; prepared cellulose carbamate can be dissolved in a NaOH solution to form a stable solution and can be used for preparing regenerated cellulose fibers, membranes and the like.

Description

technical field [0001] The invention relates to a method for preparing cellulose carbamate by liquid-solid phase reaction. Background technique [0002] With the development of society and economy, petroleum resources, which are non-renewable, will face depletion. Research and development of materials with natural polymers as raw materials has become a hot spot in polymer science research. Cellulose is a renewable, biocompatible and biodegradable resource, and has become a very active branch of chemistry with cross-penetration of various disciplines. In addition to being used in traditional industries such as plastics, textiles, and paper, cellulose chemically modified products have also been widely developed in the fields of food industry, daily chemical industry, pharmaceutical industry, construction industry, oil field industry, biological industry, and membrane separation technology. and apply. Cellulose carbamate (CC) is a product of the esterification reaction of ce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/06
Inventor 尹翠玉岳军
Owner TIANJIN POLYTECHNIC UNIV
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