羧甲基纤维素钠的制备及表征
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摘要
羧甲基纤维素钠(简称CMC)是以精制短棉为原料而合成的一种阴离子型高分子化合物。分子量6400(±1000),具有优良的水溶性与成膜性,广泛应用于石油、日化、轻工、食品、医药等工业中,被誉为“工业的味精”。1989年4月化工部曾将CMC-Na 列为“新领域精细化工‘八五’规划产品”。
CMC-Na生产发展到今天,合成方法主要有两种,一种是水煤直接法(喷碱法),另一种是采用有机溶媒体的溶媒法,由于后者具有用碱量少,醚化时间短,醚化剂利用率高等特点,因此目前已被广泛采用。然而目前国内使用的CMC-Na普遍存在着合格率较低,成本大幅度上升,新产品开发缓慢等问题。
衡量CMC-Na质量的主要指标是取代度(DS)和粘度,一般来说,DS不同,则CMC-Na 的性质也不同;取代度增大,溶液的透明度及稳定性也越好。据报道,CMC-Na取代度在0.7-1.2时透明度较好,其水溶液粘度在pH为6-9时最大,为保证其质量,除选择醚化剂外,还必须考虑影响取代度和粘度的一些因素,例如碱与醚化剂之间的用量关系、醚化时间、体系含水量、温度、pH值、溶液浓度等。
本文目的旨在降低成本,提高质量,通过从几大因素——碱化温度、醚化温度、碱化时间、醚化时间、碱的浓度、醚化剂配比分别合成,并检验各种产品的性能,进而得出合成CMC-Na的最佳工艺条件。
关键词:溶媒法;粘度;醚化剂;最佳工艺条件
Abstract
Sodium carboxymethyl cellulose (CMC)is an anionic polymer compound composed by refine short cotton, whose molecular weight is 6400(±1000), highly water-soluble and good film-forming property. It is widely used in the industries of petroleum, daily chemicals, light industry, food and pharmaceuticals, which is renowned as the “Aginomoto of Industries”. The Ministry of Chemical Industry ranked CMC-Na as the project product in fine chemical industry of the “Eighth Five-year Plan”.
So far, two synthetic methods of CMC-Na have been developed, one of which is direct compounding of coal and water (Alkali Spraying) and the other is organic solvent. The lower alkali charge, shorter etherification process and high-efficient utilization of etherifying agent, the latter method is adopted widely. But lower quality, increasing production cost and slow development of new product are the common problems resided in the domestic CMC-Na.
The main indexes to assess the quality of CMC-Na are degree of substitution (DS) and viscosity. Generally, DS determines the property of CMC-Na; the more the degree of substitution, the better the transparency and stability of the solution. It is said the transparency of CMC-Na is higher when the DS is in 0.7-1.2, and the viscosity is at the highest when pH is 6-9. To ensure the quality, apart from etherifying agent, the factors affecting the DS and viscosity shall also be taken into account, such as the relationship between alkali and the amount of etherifying agent, how long etherification lasts, content of water in the system, temperature, pH and concentration of solution.This thesis aims to seek ways to reduce the production cost and improve the quality of CMC-Na. The common factors, such as temperature of alkalization and etherification, time for alkalization and etherification, concentration of alkaline and ration of etherifying agent are respectively used to synthesize CMC-Na in order to find out the best processing conditions for synthesis of CMC-Na.
Key word:organic solvent ;viscosity ;etherifying agent ;the best processing conditions for synthesis