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Cellulose levulinate and method for preparing mixed ester with same

A technology of levulinic acid ester and levulinic acid ester, which is applied in the field of compound synthesis, can solve the problems of uncontrollable reaction products, complex product purification energy, difficult to control yield, etc., and achieve efficient, controllable and good transesterification process. The effect of reactivity and mild reaction

Inactive Publication Date: 2019-01-04
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of synthesizing cellulose levulinate and its mixed esters under this condition, the use of catalysts will cause side reactions, the yield is difficult to control, and the product purification performance is relatively complicated.
And using levulinic acid as an esterification reagent, the reaction product is uncontrollable

Method used

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  • Cellulose levulinate and method for preparing mixed ester with same
  • Cellulose levulinate and method for preparing mixed ester with same
  • Cellulose levulinate and method for preparing mixed ester with same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Proceed as follows:

[0064] 1) Mix cellulose, organic base and organic solvent, in a certain CO 2 The pressure is 0.1-10.0MPa, the temperature is 30°C-100°C, and the reaction is 0.1-12 hours to obtain a cellulose solution;

[0065] 2) adding levulinate or angelica lactone to the cellulose solution, and reacting at 30-150° C. for 0.1-48 hours to obtain a cellulose levulinate solution;

[0066] 3) Add C1-C4 lower aliphatic alcohol or ethyl acetate or water to the cellulose levulinate solution, and then filter the reaction mixture containing lower aliphatic alcohol or ethyl acetate or water to obtain a filtered solid; filter The obtained solid mixture is washed, purified and dried with C1-C4 lower aliphatic alcohol or ethyl acetate to obtain cellulose levulinate;

[0067] 4) adding an acylating agent to the cellulose levulinic acid ester solution, and continuing to react at 30-100° C. for 0.5-12 hours to obtain a cellulose levulinic acid mixed ester solution;

[0068] ...

Embodiment 2

[0071] According to the steps of Example 1, 0.5 g of different types of cellulose were weighed, respectively mixed with 1.406 g of 1,8-diazabicyclo[5.4.0]-7-undecene (DBU) and dimethyl methylene Add 7.86g of sulfone (DMSO) into the reactor, cover the reactor, and charge and discharge CO 2 Cycle three times, remove the air, and finally in 0.5Mpa CO 2 Atmosphere, 50° C., stirring for 3 hours to obtain a homogeneous cellulose solution (wt%=5%). Take 10 g of the above solution and add it to a two-neck bottle, and add 2.494 ml (such as formula 2-1) α-angelica lactone dropwise under mechanical stirring at 120°C (the ratio of the molar number of α-angelica lactone to the original -OH on the cellulose 3:1) reaction for 0.5h, the reaction was completed to obtain a dark brown homogeneous solution, using 100mL of isopropanol as an anti-solvent to precipitate a solid product, washed and filtered 3 times, and freeze-dried to obtain the product. The products made from different celluloses...

Embodiment 3

[0077] According to the steps of Example 1, take microcrystalline cellulose 0.5g, take organic base 1,8-diazabicyclo[5.4.0]-7-undecene (DBU), triethylamine (TEA) or 1,5-diazabicyclo[4.3.0]non-5-ene (DBN), take organic solvent dimethylsulfoxide (DMSO), N,N-dimethylformamide (DMF) or N-formaldehyde Pyrrolidone (NMP), one of the microcrystalline cellulose, one of the organic base and one of the organic solvent was mixed and added to the inside of the reaction kettle, the reaction kettle was covered, and the CO 2 Cycle three times, remove the air, and finally in 0.5Mpa CO 2 Atmosphere, 50°C, stirring for 3 hours to obtain a homogeneous cellulose solution. Take 10g of the above solution and put it into a two-neck bottle, add 2.494ml of α-angelica lactone dropwise under mechanical stirring at 120°C (the molar ratio of α-angelica lactone to the original -OH on the cellulose is 3:1) and react for 0.5h , the reaction was completed to obtain a dark brown homogeneous solution, using 10...

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Abstract

The invention discloses cellulose levulinate and a method for preparing mixed ester with the same. Hybrid reaction is carried out on celluloses, organic alkali and organic solvents to obtain cellulosesolution; levulinic acid base ester or angelica lactone is added into the cellulose solution, and reaction is carried out to obtain cellulose levulinate solution; anti-solvents are added into the cellulose levulinate solution, and then filtering, washing purification and drying are carried out to obtain the cellulose levulinate. The method includes dissolving the cellulose levulinate; adding acylation reagents; then adding C1-C4 low fatty alcohol, ethyl acetate or water; carrying out filtering, purification and drying to obtain the cellulose levulinic acid mixed ester. The cellulose levulinate and the method have the advantages that levulinic acid functional areas with active carboxyl are constructed on cellulose molecular chains in an in-situ manner, cellulose derivatives with novel structures, adjustable properties and levulinic acid structures are prepared, accordingly, the celluloses can be structurally specifically derived, and the cellulose levulinate and the method have important significance in high-valued utilization of the celluloses.

Description

technical field [0001] The invention relates to a preparation method of cellulose levulinate and mixed esters thereof, belonging to the field of compound synthesis. Background technique [0002] With the severe energy and environmental problems brought about by the increasing consumption of fossil energy, biomass resources have attracted people's attention and attention. Biomass resources, especially lignocellulose, are one of the most abundant and cheapest renewable resources on earth. The components of lignocellulose are cellulose, hemicellulose and lignin, among which cellulose is the most abundant. Cellulose is an inexhaustible renewable biomass resource, and it has the characteristics of complete biodegradation, easy modification, and good biocompatibility [A.J.Ragauskas, et al.Science (New York , N.Y.), 2006, 311, 484-489.]. Therefore, high-value utilization of cellulose-based materials is very important. Based on the background of the increasingly serious problems...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B3/16
CPCC08B3/16
Inventor 谢海波裴敏
Owner GUIZHOU UNIV
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