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Method for preparing cellulose acetate propionate or cellulose acetate butyrate

A technology of cellulose acetate propionate and acetic acid butyric acid is applied in the field of homogeneous preparation of cellulose acetate propionate or cellulose acetate butyrate mixed ester, and the effect of simple process is achieved

Inactive Publication Date: 2009-11-18
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method for preparing cellulose acetate propionate or cellulose acetate butyrate by using ionic liquid has not yet been disclosed

Method used

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  • Method for preparing cellulose acetate propionate or cellulose acetate butyrate
  • Method for preparing cellulose acetate propionate or cellulose acetate butyrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034]About 0.6g of cellulose and 59.4g of ionic liquid 1-allyl-3-methylimidazolium chloride (AMIMCl) were weighed, put into a round bottom flask, heated to 60°C in an oil bath, sealed and vigorously mechanically stirred for 1 hour. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 1% (mass percentage). The temperature of the oil bath was raised to 80°C, and at the same time, acetic anhydride (about 1.05ml) and propionic anhydride (about 4.75ml) were added to the solution, so that the molar ratio of acetic anhydride to cellulose glucose units was 3:1, and propionic anhydride and The molar ratio of cellulose to glucose units was 10:1, and the reaction was performed for 1 h. After the reaction is finished, methanol with 3 times the volume of the ionic liquid is added to the reaction mixture to wash the ionic liquid in the reaction mixture, filter the reaction mixture containing methanol, dry and filter the obtained solid...

Embodiment 2

[0036] About 0.6g of cellulose and 9.4g of ionic liquid 1-ethyl-3-methylimidazolium acetate (EMIMAc) were weighed, put into a round bottom flask, heated to 80°C in an oil bath, sealed and vigorously mechanically stirred for 4h. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 6% (mass percentage). Raise the temperature of the oil bath to 100°C, first add acetic anhydride (about 1.74ml) to the solution so that the molar ratio of acetic anhydride to cellulose glucose unit is 5:1; add propionic anhydride (about 3.80ml) after reacting for 1 hour , so that the molar ratio of propionic anhydride to cellulose glucose unit is 8:1, continue to react for 3h. After the reaction, the post-treatment of the reaction mixture and the recovery of the ionic liquid are basically the same as in Example 1, except that ethanol with 5 times the volume of the ionic liquid is added to the reaction mixture. After testing, the acetyl substituti...

Embodiment 3

[0038] About 3g of cellulose and 12g of ionic liquid 1-butyl-3-methylimidazolium chloride (BMIMCl) were weighed, put into a round bottom flask, heated to 100°C in an oil bath, sealed and vigorously mechanically stirred for 10h. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 20% (mass percentage). Raise the temperature of the oil bath to 120°C, first add propionic anhydride (about 14.25ml) to the solution so that the molar ratio of propionic anhydride to cellulose glucose unit is 6:1; after reacting for 2 hours, add acetic anhydride (about 12.25ml ), the molar ratio of acetic anhydride to cellulose glucose unit is 7:1, and the reaction is continued for 5h. After the reaction, the post-treatment of the reaction mixture and the recovery of the ionic liquid are basically the same as in Example 1, except that propanol, which is 7 times the volume of the ionic liquid, is added to the reaction mixture. After testing, the a...

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Abstract

The invention provides a method for preparing cellulose acetate propionate or cellulose acetate butyrate. The method comprises the following steps: a. mixing fibrin and ionic liquid capable of dissolving the fibrin to obtain an ionic liquid solution containing the fibrin; b. adding acetylate and propionyl reagent (1) or acetylate and reagent (2) into the ionic liquid solution containing the fibrin, reacting for 1-24h at 40-120 DEG C, preferably 1-12h, and obtaining reaction mixture; c. adding lower fatty alcohol from C1 to C3 into the reaction mixture and filtering the reaction mixture containing the lower fatty alcohol; and d. drying a solid obtained by filtering to obtain the cellulose acetate propionate or cellulose acetate butyrate. The invention utilizes the ionic liquid as a solvent without any catalyst and has the advantages of simple process and no pollution.

Description

technical field [0001] The invention relates to a method for preparing cellulose acetate propionate or cellulose acetate butyrate, in particular to a method for homogeneously preparing cellulose acetate propionate or cellulose acetate butyrate mixed ester in an ionic liquid. Background technique [0002] Cellulose derivatives are the earliest natural polymer materials developed by humans. Although since the 1950s, with the rise of petrochemical industry, the successful development of various new synthetic polymer materials and large-scale industrial production, the proportion of cellulose derivative plastics and resins in the field of polymer materials has decreased year by year. . However, since the 1970s, considering the limited energy and petroleum resources, and the irreplaceable characteristics of other synthetic polymer materials in cellulose material products, the research and development of natural polymers in the polymer field have been renewed. Pay attention to u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B3/16C08B3/18
Inventor 李会泉曹妍张懿武进张军何嘉松
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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