Method for producing cellulose ester acetate by using plant cellulose

A technology of cellulose acetate and plant cellulose, applied in the field of preparation of cellulose acetate, can solve the problem of high cost of raw materials, and achieve the effects of improving reaction rate, expanding application scope and abundant raw material sources

Inactive Publication Date: 2007-05-09
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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The method solves the problem of high raw material co...
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Abstract

This invention relates to a method for preparing cellulose ester acetate from plant cellulose in ionic liquid. The method comprises: (1) utilizing plant cellulose as the raw material; (2) dissolving plant cellulose in ionic liquid; (3) adding acylation agent into the ionic liquid, performing homogeneous acetylation on plant cellulose, washing the intermediate with water and drying; (4) separating and purifying dried intermediate to obtain cellulose ester acetate. This invention provides a method for homogeneously preparing cellulose ester acetate in clean solvent (ionic liquid) by using low quality plant cellulose as the raw material. The method solves the problem of high cost faced by the present methods.

Application Domain

Bulk chemical production

Technology Topic

SolventIon +7

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  • Method for producing cellulose ester acetate by using plant cellulose
  • Method for producing cellulose ester acetate by using plant cellulose
  • Method for producing cellulose ester acetate by using plant cellulose

Examples

  • Experimental program(9)

Example Embodiment

[0030] Example 1
[0031] Weigh about 0.6 g of corn ear husk cellulose and 59.4 g of ionic liquid 1-allyl-3-methylimidazole chloride (AMIMCl), put them into a round bottom flask, heat it to 80°C in an oil bath, seal and stir strongly mechanically. 2h. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 1% (mass fraction). At the same time, acetic anhydride (about 1.05ml) was added to the solution so that the molar ratio of acetic anhydride to the cellulose glucose unit was 3:1, and the reaction was carried out for 1 hour. After the reaction is completed, the product is repeatedly washed with water and placed in a vacuum drying cabinet, dried at 60°C for 24 hours; at the same time, the water in the washing liquid is removed by rotary evaporation to realize the recovery of the ionic liquid.
[0032] Weigh 0.1 g of the intermediate product, dissolve it in 3 ml of a dichloromethane-methanol mixed solvent (volume ratio of 9:1), dissolve it at room temperature for 2 hours, and then filter with suction to obtain a clear and transparent filtrate. After the filtrate is settled in n-hexane and filtered, the filter residue is collected, and the filter residue is cellulose acetate. The cellulose acetate was placed in a vacuum oven at 60°C for drying.

Example Embodiment

[0033] Example 2
[0034] Weigh about 0.6 g of corn stalk cellulose and 9.6 g of ionic liquid 1-ethyl-3-methylimidazole acetate (EMIMAc), put them into a round bottom flask, heat the oil bath to 60°C, seal and stir vigorously for 4 hours. . A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 4% (mass fraction). The temperature of the oil bath was raised to 90° C., and acetic anhydride (about 1.58 ml) was added to the solution at the same time, so that the molar ratio of acetic anhydride to cellulose glucose unit was 4.5:1, and the reaction was carried out for 8 hours.
[0035] Ionic liquid recovery and product separation were the same as in Example 1.

Example Embodiment

[0036] Example 3
[0037] Weigh about 0.6 g of peanut shell cellulose and 9.6 g of ionic liquid 1-butyl-3-methylimidazole chloride (BMIMCl), put them into a round-bottomed flask, heat the oil bath to 90° C., seal and stir vigorously for 6 hours. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 4% (mass fraction). The temperature of the oil bath was raised to 120°C, and acetic anhydride (about 2.45 ml) was added to the solution at the same time, so that the molar ratio of acetic anhydride to the cellulose glucose unit was 7:1, and the reaction was carried out for 12 hours.
[0038] Weigh 0.1 g of the intermediate product, dissolve it in 5 ml of a dichloromethane-methanol mixed solvent (volume ratio of 9:1), dissolve it at room temperature for 4 hours, and then filter with suction to obtain a clear and transparent filtrate. After the filtrate is settled in n-hexane and filtered, the filter residue is collected, and the filter residue is cellulose acetate. The cellulose acetate was placed in a vacuum oven at 60°C for drying.

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