Method for preparing carbonic ester-carbamate mixed ester based on cellulose carbonic ester

A technology of carbamate and carbonate, applied in the field of preparation of mixed ester materials, can solve the problems of cellulose carbonate derivative literature and patent reports, type restrictions, etc.

Inactive Publication Date: 2018-11-20
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The properties of cellulose carbamate derivatives vary with the structure and substitution position of the carbamate, but based on the limitation of the type of isocyanate, the types of cellulose carbamate derivatives are subject to certain restrictions
[0006] The present invention uses cellulose carbonate as raw material, obtains cellulose carbonate solution through dissolution, continues to react with isocyanate reagents, and successfully prepares cellulose derivatives with a

Method used

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  • Method for preparing carbonic ester-carbamate mixed ester based on cellulose carbonic ester
  • Method for preparing carbonic ester-carbamate mixed ester based on cellulose carbonic ester
  • Method for preparing carbonic ester-carbamate mixed ester based on cellulose carbonic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0107] Weigh 1.00 g of cellulose carbonates with different substitution structures in a flask, take 5 mL of dimethyl sulfoxide (DMSO), and heat to dissolve at 50° C. Add 1.165 mL of p-toluene isocyanate and 10 wt % DBU relative to cellulose carbonate as a catalyst, and react at 50° C. for 3 h. After the end, use 100 mL of water for precipitation, wash with suction and filter 3 times, and freeze-dry to obtain the product. The relevant results are shown in the table below:

[0108] Table 1 Reaction of cellulose carbonates with different structures

[0109]

[0110] where DS C1 and DS C2 Respectively represent the degree of substitution of carbonate groups of pure cellulose carbonate and the reacted cellulose carbonate-urethane mixed ester. discover DS C2 The value is generally higher than the DS C1 Large, due to NMR calculation errors.

[0111] This example fully demonstrates that for cellulose carbonates of different structures, cellulose carbonate-urethane mixed este...

Embodiment 2

[0113] Weigh 1.00 g of cellulose hexyl carbonate into a flask, take different volumes of dimethyl sulfoxide (DMSO), and heat to dissolve at different temperatures. Add 1.165mL of p-toluene isocyanate, and catalysts of different types and different mass fractions, and react at 50°C for 3h. After the end, use 100 mL of water for precipitation, wash with suction and filter 3 times, and freeze-dry to obtain the product. The relevant results are shown in the table below:

[0114] Table 2 Study of different cellulose carbonate concentrations, temperatures and organic solvents

[0115]

[0116] a: ratio content of cellulose carbonate to solvent (W / V); b: dissolution temperature of cellulose carbonate; c: dissolution reagent used.

[0117] This example fully demonstrates that for different cellulose carbonate concentrations, as well as dissolution temperature and dissolution reagents, the reaction with isocyanate reagents can be realized, and finally a carbonate-urethane mixed ce...

Embodiment 3

[0119] Based on the fact that ionic liquid is a good solvent with good stability and wide adaptability, it is also a good catalyst for organic reactions. Ionic liquid has both the functions of solvent and catalyst, and a series of researches are carried out on this.

[0120] Weigh 1.00 g of cellulose hexyl carbonate into a flask, take different ionic liquids (Ionic Liquid), and heat to dissolve at different temperatures. Add 1.165mL of p-toluene isocyanate and react at 50°C for 3h. After the end, use 100 mL of water for precipitation, wash with suction and filter 3 times, and freeze-dry to obtain the product. The relevant results are shown in the table below:

[0121] Table 3 Ionic Liquids as Solvents

[0122]

[0123] a: ratio of cellulose carbonate to ionic liquid (W / W); b: dissolution temperature of cellulose carbonate; c: ionic liquids with different structures.

[0124] In conjunction with Example 2, examples fully demonstrate that ionic liquids have good solubility...

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Abstract

The invention discloses a method for preparing carbonic ester-carbamate mixed ester based on cellulose carbonic ester. The method comprises the following steps: 1) by taking cellulose carbonic ester as a raw material; 2) dissolving the cellulose carbonic ester of the step 1) into a solvent at 10-120 DEG C so as to obtain a product A; 3) putting isocyanate and a catalyst into the product A, and carrying out a reaction for 0.1-10 hours at 20-100 DEG C so as to obtain a product B; 4) putting an anti-solvent into the product B, filtering a precipitate substance, washing and purifying precipitate,and drying, thereby obtaining a cellulose carbonic ester-carbamate mixed ester material. The cellulose carbonic ester-carbamate mixed ester material prepared by using the method is of a novel structure, has the specificity of properties of carbonic ester groups and carbamate groups, has instruction significances in achieving structural diversity and high-value utilization of cellulose and in addition is simple in preparation method and convenient to operate, and the solvent can be recycled.

Description

technical field [0001] The invention relates to a method for preparing mixed ester materials, in particular to a method for preparing carbonate-urethane mixed ester based on cellulose carbonate. Background technique [0002] Realizing the efficient utilization of biomass resources will help alleviate the current energy crisis and environmental crisis. Among them, cellulose is the most abundant. As a natural polymer material, its repeating unit is β-1,4 glycosidic bonds, which are insoluble and infusible. In order to effectively utilize it, people have developed a variety of methods to dissolve it, including inorganic strong acid and strong alkali treatment, DMAc / LiCl system, NaOH / urea system, ionic liquid system and other dissolution measures. Among them, it is found that the DMAc / LiCl dissolution system is more efficient (Marson G A, et al. Journal of Applied Polymer Science, 2015, 74(6):1355-1360.), this system is in a strong polar solvent, the Cl of the inorganic salt I...

Claims

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Application Information

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IPC IPC(8): C08G18/64C08G18/71C08G18/73C08G18/75C08G18/76C08G18/77C08G18/78
CPCC08G18/6484C08G18/71C08G18/711C08G18/712C08G18/714C08G18/715C08G18/718C08G18/73C08G18/758C08G18/7614C08G18/7642C08G18/7657C08G18/7671C08G18/7678C08G18/7685C08G18/771C08G18/773C08G18/776C08G18/7893Y02P20/54
Inventor 谢海波蔡龙
Owner GUIZHOU UNIV
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