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A kind of preparation method of cellulose long-chain fatty acid ester or long-short-chain mixed ester

A technology of cellulose ester and fatty acid anhydride, applied in the chemical field, can solve the problems of unstable trifluoroacetate, adverse effects on product performance and surrounding environment, etc., to save reaction time, excellent solubility, and reduce pollution Effect

Active Publication Date: 2019-01-01
NANTONG CELLULOSE FIBERS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the trifluoroacetate of cellulose is relatively unstable, and it will gradually decompose in the later stage of the process or during the use of the product, which will easily bring adverse effects on the performance of the product and the surrounding environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] (1) Put 3 g of cellulose-grade hardwood pulp and 120 g of trifluoroacetic acid (the mass ratio of trifluoroacetic acid to cellulose pulp is 40:1) after drying at 105°C for 2 hours into a three-necked bottle with mechanical stirring , stirred and infiltrated in an ice bath for 3 hours;

[0060] (2) Then add 15g of long-chain anhydride caprylic anhydride (the mass ratio of long-chain fatty acid anhydride to cellulose pulp is 5:1) to a transparent state, and keep the reaction at 60°C for 5 hours;

[0061] (3) Add 30 g of acetic acid to complete the reaction, transfer to a rotary evaporator at 65° C. for 1 hour, and recover trifluoroacetic acid; finally, the resulting product is precipitated in an acetic acid / water mixed solvent, washed with water, and dried to obtain 11.3 g of white powder.

[0062] The product is cellulose octanoate, and the degree of substitution (DS) measured by 1H-NMR is 1.91. The product is insoluble in 91% / 9% dichloromethane / methanol, acetone, dimet...

Embodiment 2

[0064] (1) Put 3 g of cellulose softwood pulp and 120 g of trifluoroacetic acid (the mass ratio of trifluoroacetic acid to cellulose pulp is 40:1) after drying at 105°C for 2 hours into a three-necked bottle with mechanical stirring, Stir and infiltrate in an ice bath for 3 hours;

[0065] (2) Then add 15g of capric anhydride (the mass ratio of long-chain fatty acid anhydride to cellulose pulp is 5:1) to a transparent state, and keep the reaction at 60°C for 5 hours;

[0066] (3) Add 30g of acetic acid to complete the reaction, transfer to a rotary evaporator and treat at 65°C for 1 hour, and recover trifluoroacetic acid; finally, the product obtained is precipitated in a mixed solvent of acetic acid / water, washed with water, and dried to obtain 12.7g of light yellow powder shaped product.

[0067] The product is cellulose caprate, and the degree of substitution (DS) measured by 1H-NMR is 2.08. The product is not soluble in 91% / 9% dichloromethane / methanol, acetone, dimethyl ...

Embodiment 3

[0069] (1) Put 3 g of cellulose-grade cotton pulp and 120 g of trifluoroacetic acid (the mass ratio of trifluoroacetic acid to cellulose pulp is 40:1) after drying at 105°C for 2 hours into a three-necked bottle with mechanical stirring , stirred and infiltrated in an ice bath for 3 hours;

[0070] (2) Then add a mixed solution of 0.74g octanoic anhydride and 6.66g acetic anhydride (the mass ratio of long-chain fatty acid anhydride to cellulose pulp is 1:4.05, the mass ratio of short-chain anhydride to long-chain fatty acid anhydride is 9:1, and the mass ratio of short-chain fatty acid anhydride to long-chain fatty acid anhydride is 9:1. The mass ratio of acid anhydride to cellulose pulp is 2.22) to a transparent state, and the reaction is kept at 50°C for 3 hours;

[0071] (3) After finishing the reaction, the obtained product was precipitated in an acetic acid / water mixed solvent, washed with water, and dried to obtain 5.7 g of a white powdery product.

[0072] The product ...

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Abstract

The invention belongs to the technical field of chemistry and relates to a preparation method of cellulose ester. The preparation method comprises the following steps: 1, placing cellulose pulp and trifluoroacetic acid into a reactor; 2, adding fatty acid anhydride into the reactor of step 1, and conducting reaction till a transparent state is reached; 3, conducting precipitation, washing and drying on an obtained product in acetic acid / water mixed solvent. According to the preparation method, trifluoroacetic acid is adopted as solvent and a catalyst, and one-step method synthesis of cellulose aliphatic ester is conducted under a homogeneous reaction system, so that an acylation reaction can be conducted under a mild condition, cellulose is not prone to being oxidized and degraded, the substitution degree is high, and the controllablility is achieved. Meanwhile, due to the fact that trifluoroacetic acid is low in boiling point, recovery is easy to conduct. Through continuous improvement of the recovery technology, reaction cost can be reduced, and industrial production is facilitated. Prepared cellulose long-chain and short-chain mixed acid ester has stable physicochemical properties, and moulding formation can be achieved without plasticizer.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and relates to a method for preparing cellulose esters, in particular to a method for preparing cellulose long-chain fatty acid esters or long- and short-chain mixed acid esters. Background technique [0002] As the most abundant natural polymer material in the world, cellulose is widely used in industrial production, such as film, fiber, etc. , sheets and coatings [1,2]. Cellulose derivatives generally include cellulose esters, ethers, and viscose fibers. Among the cellulose esters, only C2-C4 organic acid cellulose esters, such as cellulose acetate, cellulose acetate propionate and cellulose acetate butyrate, have been used in industrial applications. Cellulose acetate, acetate propionate, and acetate butyrate can all be used as molding compounds. However, plasticizers such as phthalates, triacetin and citric acid esters must be added during processing. Cellulose acetate should usually ad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B3/12C08B3/16C08B3/02
Inventor 陈昀曹建华王林富顾海兵李鹏辉张丽
Owner NANTONG CELLULOSE FIBERS CO LTD