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Method for preparing hydroxyethyl cellulose

A technology of hydroxyethyl cellulose and cellulose, applied in the field of preparation of cellulose fibers, can solve the problems of narrow processing window, high energy consumption of solvent recovery, expensive solvent and the like, achieves simple production control, and is beneficial to industrialization promotion and manufacturing low cost effect

Inactive Publication Date: 2010-10-20
DONGHUA UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Since the 1970s, there has been a wet spinning process that uses N-methylmorpholine-N-oxide (NMMO) as a solvent to directly dissolve cellulose at home and abroad. The problem with this solution is: the fiber The dissolution temperature of the element is too high, the processing window is narrow, the solvent is expensive, and the energy consumption of solvent recovery is high
In 1998, the German Zimmer company published the patent DE19635473 of the CC process, which replaced CS with urea 2 React with cellulose to generate cellulose carbamate intermediate to avoid CS in viscose process 2 and H 2 The emission of toxic gases such as S, but this process has not been effectively promoted due to the reaction control problem of cellulose carbamate

Method used

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  • Method for preparing hydroxyethyl cellulose
  • Method for preparing hydroxyethyl cellulose
  • Method for preparing hydroxyethyl cellulose

Examples

Experimental program
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Effect test

preparation Embodiment 2

[0030] In this example, except that the mass of ethylene oxide added to the reactor is 44g, the remaining reaction conditions are exactly the same as those of the above-mentioned low molar substitution HEC preparation example 1, and the obtained HEC was obtained by using 1 H NMR ( figure 2 ) The measured molar substitution is 0.49.

Embodiment 1

[0032] First 101g NaOH is dissolved in 1659g water, and this solution is precooled to-5 ℃, then weighs the product 440g of the low molar substitution HEC preparation example 2 (which contains HEC 132g, NaOH 74.8g, water 233.2g, HEC The molar substitution is 0.49), and it was added into the pre-cooled NaOH aqueous solution while stirring. After the HEC powder swells into a transparent state, increase the stirring speed and continue stirring for 1 hour before stopping the dissolution process. Obtained 2200 g of spinning dope with HEC mass percentage concentration of 6.0%, wherein NaOH content was 8%. Since there are many air bubbles in the spinning stock solution, the spinning is performed after vacuum defoaming. The spinneret hole diameter that adopts during spinning is 0.1mm, and hole number is 6 holes, and coagulation bath temperature is 45 ℃, and washing, drawing bath temperature are 45 ℃, and the spinning speed of the first drawing roll is 7m / min, The draw ratio was 1.3 t...

Embodiment 2

[0034] Firstly, 75g NaOH was dissolved in 1531g water, and the solution was precooled to -5°C. Then weigh 594g of the product of the low molar substitution HEC preparation example 2 (containing 178.2g of HEC, 101g of NaOH, 314.8g of water, and the molar substitution of HEC is 0.49), and add it into the precooled NaOH aqueous solution. After the HEC powder swells into a transparent state, increase the stirring speed and continue stirring for 1 hour before stopping the dissolution process. A spinning dope with a concentration of 8.1% by mass of HEC was obtained, wherein the content of NaOH was 8%. Since there are many air bubbles in the spinning stock solution, the spinning is performed after vacuum defoaming. The diameter of the spinneret holes used in spinning is 0.08mm, and the number of holes is 50 holes. The temperature of the coagulation bath was 45°C, the temperature of the washing and drawing bath was 50°C, the spinning speed of the first drafting roll was 7m / min, and ...

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Abstract

The invention relates to a method for preparing hydroxyethyl cellulose. The method comprises the following steps of: (1) reacting alkali cellulose containing 30 weight percent of cellulose which serves as a raw material with ethylene oxide at the temperature of 25 DEG C in vacuum so as to obtain hydroxyethyl cellulose HEC with low molar substitution degree; (2) dissolving the HEC in aqueous solution of NaOH at the temperature of -5 DEG C to prepare 5 to 12 mass percent hydroxyethyl cellulose spinning solution; and (3) forming the prepared spinning solution by adopting a wet spinning method. The method has the advantages of environmental-friendly and low energy-consumption raw materials, simplicity, continuous manufacturing, contribution to industrial popularization and capability of spinning novel hydroxyethyl cellulose with high mechanical performance.

Description

technical field [0001] The invention belongs to the field of preparation of cellulose fibers, in particular to a preparation method of hydroxyethyl cellulose fibers Background technique [0002] Cellulose fiber has excellent moisture absorption and air permeability, meets the physiological requirements of human skin, and also has the advantages of soft hand feeling, easy dyeing, antistatic, etc. Therefore, the annual demand for cellulose fiber in the world has remained at 250 in recent years. More than 10,000 tons. In fact, the source of cellulose is very rich, and it is produced by CO in nature. 2 and H 2 O is produced through the photosynthesis of plants, and after being discarded, it can participate in the big cycle of nature and be decomposed into CO again 2 and H 2 O is then reabsorbed by plants. Due to various difficulties in the melting and solution processing of cellulose, the development and utilization rate of cellulose is still very low, and most of the cellu...

Claims

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Application Information

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IPC IPC(8): D01F2/28D01D1/02D01D5/06C08B11/08
Inventor 王夏琴李冬梅胡祖明周兴平张敬芳李雪峰
Owner DONGHUA UNIV
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