Mechanical activation and enhancement method for preparing cellulose acetate-butyrate or cellulose acetate-propionate

A technology of cellulose acetate propionate and mechanical activation is applied in the field of preparing cellulose acetate butyrate/cellulose acetate propionate by a mechanical activation strengthening method, which can solve the problems of low availability, high cost, long time consumption, etc. The effect of cost reduction, easy operation and simple process

Active Publication Date: 2014-03-12
福建鸿燕化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to overcome the problems in the preparation method of cellulose acetate butyrate / cellulose acetate propionate that the preparation process takes a long time, the process is complicated and difficult to control, resulting in high cost, and the cellulose has high crystallinity, low accessibility, and difficult chemical reactions , the crude product purification process has strict requirements, the low degree of acylation of the product results in poor physical and chemical properties of the product, and it is difficult to meet the needs of environmental protection and high-quality coatings. A method for preparing cellulose acetate butyrate / propionic acid acetate by mechanical activation and strengthening method is provided. cellulosic method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 Preparation of cellulose acetate butyrate

[0025] The cellulose used in this embodiment is cotton cellulose; the catalyst is sulfuric acid in acids.

[0026] Weigh the reaction materials according to the ratio of cellulose: butyric acid: acetic anhydride: catalyst = 10g: 43g: 250g: 0.1g, put all the reaction materials in a ball mill, and control the ratio of reaction materials to material balls (pile volume) = 100g: 150ml, the material ball is a zirconia ball with a diameter of 6mm, the temperature of the circulating water bath is controlled at 80°C, the stirring speed is controlled at 450r / min, and the acylation reaction is carried out for 3h. After the reaction, the crude product is obtained, and the crude product is separated from the material ball. The crude product was left to stand in 50% ethanol aqueous solution to precipitate a solid, and the precipitated solid was separated, washed with water to neutralize the precipitated solid, and the cellulose ac...

Embodiment 2

[0028] Example 2 Preparation of cellulose acetate butyrate

[0029]The cellulose used in this embodiment is lignocellulose; the catalyst is methanesulfonic acid in acids.

[0030] Weigh the reaction materials according to the ratio of cellulose: butyric acid: acetic anhydride: catalyst = 10g: 66g: 20g: 0.5g, put all the reaction materials in a ball mill, and control the ratio of reaction materials to material balls (pile volume) = 100g: 100ml, the material ball is a zirconia ball with a diameter of 2mm, the temperature of the circulating water bath is controlled at 50°C, the stirring speed is controlled at 100r / min, and the acylation reaction is carried out for 4h. After the reaction, the crude product is obtained, and the crude product is separated from the material ball. The crude product was left to stand in 40% ethanol aqueous solution to precipitate a solid, and the precipitated solid was separated, and washed with water to neutralize the precipitated solid to obtain a ce...

Embodiment 3

[0032] Example 3 Preparation of cellulose acetate butyrate

[0033] The cellulose used in this example is a composition of cotton cellulose and wood cellulose mixed in a weight ratio of 1:1; the catalyst is sodium hydroxide in alkali.

[0034] Weigh the reaction materials according to the ratio of cellulose: butyric acid: acetic anhydride: catalyst = 10g: 95g: 25g: 0.3g, put all the reaction materials in a ball mill, and control the ratio of reaction materials to material balls (pile volume) = 100g: 200ml, the material ball is a zirconia ball with a diameter of 3.5mm, the temperature of the circulating water bath is controlled at 60°C, the stirring speed is controlled at 200r / min, and the acylation reaction is carried out for 1.5h. After the reaction, the crude product is obtained, and the crude product is separated from the material ball , the crude product was left to stand in 60% ethanol aqueous solution to precipitate solids, the precipitated solids were separated, was...

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Abstract

The invention relates to the field of cellulose processing, and in particularly relates to a mechanical activation and enhancement method for preparing cellulose acetate-butyrate or cellulose acetate-propionate. The method comprises the following steps: weighing reactants including cellulose, butyric acid, acetic anhydride and a catalyst in a ratio of 10g:(30-100g):(10-30g):(0.1-0.5g), putting all the reactants into a ball mill, controlling the ratio of the reactants to pellets at 100g:(100-300ml), controlling the temperature of a circulating water bath at 50-80 DEG C, stirring at a low speed to perform an acylation reaction for 1-4 hours to obtain a crude product, separating the crude product and the pellets, standing the crude product in 50% ethanol water to separate out a solid, separating the separated solid, and washing the separated solid with deionized water until the solid is neutral, thereby obtaining a cellulose acetate-butyrate or cellulose acetate-propionate product. Compared with the existing method for producing cellulose acetate-butyrate or cellulose acetate-propionate, the method disclosed by the invention has the characteristics of simple process, high efficiency, no pollution, high product quality and the like.

Description

technical field [0001] The invention relates to a method for acetic acid butyric acid / cellulose acetate propionate, in particular to a method for preparing cellulose acetate butyrate / cellulose acetate propionate by adopting a mechanical activation strengthening method. Background technique [0002] The development of cellulose derivatives has a long history, especially since the 1970s, with the understanding of the limited energy and petroleum materials, and the cellulose material products themselves have the characteristics that other synthetic polymer materials do not have, in the high In the research and utilization of molecular materials, cellulose derivatives are getting more and more attention. Cellulose ester is one of the important cellulose derivatives. [0003] Cellulose acetate butyrate (CAB) is the product of some hydroxyl groups in cellulose esterified by acetic acid and butyrate. In addition to hydroxyl and acetyl groups, CAB molecules also contain butyryl gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B3/18C08B3/16
Inventor 黄爱民黄祖强张燕娟杨梅冯振飞胡华宇覃宇奔覃杏珍沈芳
Owner 福建鸿燕化工有限公司
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