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Method for preparing cellulose ether through homogeneous reaction

A technology of cellulose ether and cellulose, which is applied in the field of homogeneous reaction to prepare cellulose ether, can solve the problems of harsh conditions for dissolving cellulose, complicated dissolving process, and accompanying pollution, and achieves wide application, improved degree of substitution, and high product quality. Enhanced effect

Inactive Publication Date: 2016-04-06
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The object of the present invention is to provide a method for preparing cellulose ether in homogeneous phase, which overcomes the disadvantages of complicated cellulose dissolution process, harsh conditions for dissolving cellulose, high cost and accompanying pollution in the prior art. Provides a cellulose homogeneous reaction method, so that the prepared cellulose ether has better uniformity, and this method is simple and fast, with mild conditions, and no pollution to the environment, easy to recycle, and environmentally friendly

Method used

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  • Method for preparing cellulose ether through homogeneous reaction
  • Method for preparing cellulose ether through homogeneous reaction

Examples

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Effect test

Embodiment 1

[0038] At 80°C, take 2.00g of cellulose with a degree of polymerization of 800 and an α-cellulose content of 99wt% and 70.00g of NMMO with a water content of 10wt% and mix evenly, add 0.20g of antioxidant propyl gallate and stir evenly for about 60min Dissolve the cellulose to obtain a 4% cellulose solution; add 6.00 g of 50% NaOH solution to the cellulose solution for alkalization reaction, the reaction time is 90 minutes to obtain alkali cellulose; add 3.54 g of chloroacetic acid at 50 ° C, Make the ratio of alkali to chloroacetic acid 2:1, mix and dissolve, react at normal pressure for 120 minutes, add 70% ethanol aqueous solution, wash and filter 3 times, and dry at 60°C to obtain sodium carboxymethylcellulose. The carboxymethyl cellulose has a degree of substitution of 1.3 and has good water solubility and viscosity.

Embodiment 2

[0040]At 80°C, take 2.00g of cellulose with a degree of polymerization of 500 and an α-cellulose content of 98wt% and 70.00g of NMMO with a water content of 10wt% and mix evenly, add 0.20g of antioxidant propyl gallate and stir evenly for about 60min Dissolve the cellulose to obtain a 4% cellulose solution; add 6.00g of 50% NaOH solution to the cellulose solution for alkalization reaction, and the reaction time is 120min to obtain alkali cellulose; add 2.86g of propylene oxide and heat up to 60°C React at low temperature for 180 minutes, add 85-95°C hot water for separation and purification, and dry at 60°C to obtain hydroxypropyl cellulose. The hydroxypropyl cellulose has a degree of substitution of 2.5 and has good water solubility and viscosity.

Embodiment 3

[0042] At 80°C, take 2.00g of cellulose with a degree of polymerization of 2000 and an α-cellulose content of 99wt% and 80.00g of NMMO with a water content of 10wt% and mix evenly, add 0.20g of antioxidant propyl gallate and stir evenly for about 60min Dissolve cellulose to obtain a 2.4% cellulose solution; add 40% NaOH solution 7.50g to the cellulose solution, add 3.19g ethyl chloride and raise the temperature to 110°C for 240min, add water to separate and purify and dry at 60°C Ethyl cellulose is obtained. The hydroxypropyl cellulose has a degree of substitution of 2.3 and has good oil solubility and viscosity.

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Abstract

The invention discloses a method for preparing cellulose ether through a homogeneous reaction. The method comprises the following steps: dissolving cellulose in an aqueous solution (the water content of 5-17wt%) of N-methylmorpholine oxide, adding an alkali solution, fully carrying out an alkalization reaction to obtain alkali cellulose, adding an etherifying agent to the above obtained system, carrying out an etherifying reaction, neutralizing the obtained reaction product, washing the neutralized product, and drying the washed product to obtain the cellulose ether product. Compared with present industrial cellulose ether preparation methods, the method disclosed in the invention has the advantages of great improvement of the homogeneity of cellulose ether, guaranteeing of the stable quality of the product, and reaction time shortening.

Description

technical field [0001] The invention relates to a method for preparing cellulose ether by homogeneous reaction, and the preparation of cellulose ether through an NMMO dissolution system has better uniformity. Background technique [0002] Cellulose is the most abundant natural polymer on the earth. It is derived from trees, plant straw, cotton and other agricultural by-products. It is a low-cost renewable resource. Derivative products of cellulose through physical and chemical modification have been widely used in chemical industry, medicine, environmental protection, building materials, petrochemical and other fields. Traditional cellulose esterification, etherification, and graft copolymerization are all carried out in a heterogeneous system. Under heterogeneous conditions, the reaction contact is insufficient, and the mass transfer and heat transfer are not uniform, resulting in a low degree of substitution and uniformity of the product, that is, the quality of the produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B11/06C08B11/08C08B11/10C08B1/08
Inventor 张涛张勇唐盛伟
Owner SICHUAN UNIV