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Dissolution and processing of cellulose using ionic liquids

A technology for dissolving cellulose and ionic liquid, applied in the field of dissolving cellulose, which can solve the problems of being unacceptable and having no practical value.

Inactive Publication Date: 2008-01-30
UNIVERSITY OF ALABAMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the degree of secrecy with which the molten salt system was described at the time, the discovery appeared to be a novelty with no practical value
When people did not understand ionic liquids and realized the application and value of ionic liquids as a class of solvents, this original work was not accepted by people

Method used

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  • Dissolution and processing of cellulose using ionic liquids
  • Dissolution and processing of cellulose using ionic liquids
  • Dissolution and processing of cellulose using ionic liquids

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0097] Example 1: Cellulose dissolution

[0098] We found that the best ionic liquid used to dissolve the exemplary test material, that is, regenerated fibrous cellulose is [C 4 mim]Cl. In the general method, fibrous cellulose (0.2g) is placed in a glass vial to melt [C 4 mim]Cl(2g), and heated in a household microwave oven with a 3×5 second heating pulse. After each heating pulse, remove the vial and vortex to mix the contents, and then put it back in the microwave. Obtain an optically transparent viscous solution of cellulose in ionic liquid.

[0099] In this way, solutions of cellulose dissolved in ionic liquids at different concentrations can be prepared. The viscosity of the solution increases with the increase of the cellulose concentration. When the cellulose concentration reaches 25% by weight, a transparent solution can still be obtained. When the cellulose concentration is higher, an opaque viscous gel is formed. For cellulose in [C 4 The actual solubility limit in mim]...

Embodiment 2

[0102] Example 2: Dissolution of cellulose in 1,3-dialkylimidazolium salt and anions and cations Functional relationship

[0103] Compared with conventional solvents, cellulose is easier to dissolve in ionic liquids at high concentrations. Screen ionic liquids with different cations as their chloride salts. These salts include [C 6mim]Cl and [C 8 mim]Cl. It is found that as the length of the cationic alkyl chain increases, the solubility of cellulose in the imidazolium-based ionic liquid decreases.

[0104] Screen various anions, from small hydrogen bond acceptors (Cl - ) To large non-coordinating anions (tetrafluoroborate and hexafluorophosphate) as (C 4 mim] + salt. Anions include Cl, Br, thiocyanate, perchlorate, hexafluorophosphate and tetrafluoroborate. These results are shown in Table 1 below.

[0105] We found that ionic liquids containing strong hydrogen bond acceptors (halogens and pseudohalogens) can achieve good dissolution effects. It is known that all these anions ...

Embodiment 3

[0114] Example 3: Cellulose regeneration

[0115] We found that the cellulose can be precipitated from the ionic liquid by adding water. This incompatibility is the basis for the following regeneration method.

[0116] By adding a known amount of water to the ionic liquid, and then using microwave heating for the dissolution process to determine the water that can still maintain the solvent properties of the ionic liquid in [C 4 mim] Concentration in Cl. When the moisture content of the ionic liquid is greater than about 1% by weight (about 0.5 mole fraction of H 2 O), the solvent properties are significantly weakened, and we found that the fibrous cellulose is no longer soluble.

[0117] When the high concentration of cellulose (more than 10% by weight) is dissolved in [C 4 In mim]Cl, a solution with optical anisotropy between the cross-polarizing filter and the birefringence is obtained. The formation of cellulose liquid crystal solutions can be applied to the production of new...

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Abstract

Cellulose is dissolved in an ionic liquid without derivatization, and is regenerated in a range of structural forms without requiring the use of harmful or volatile organic solvents. Cellulose solubility and the solution properties can be controlled by the selection of the ionic liquid constituents, with small cations and halide or pseudohalide anions favoring solution.

Description

Background technique [0001] Cellulose is the most abundant bio-renewable material, and various products derived from cellulose have been used in all cultural fields from the most primitive society to the highly developed modern technological society. In addition to the use of unmodified cellulose-containing materials (such as wood, cotton), modern cellulose technology also requires the use of various modern chemical industrial processes to extract and process cellulose from the original source, making the obtained cellulose change quite small . [0002] As a raw material, cellulose and its various derivatives can replace many chemicals. For example, cellulose can be used to replace petroleum raw materials to prepare various polymers used in paints, plastics and other formulation materials. Cellophane is prepared by dissolving the viscose intermediate and then regenerating it. The chemical dissolution is usually accompanied by derivatization (such as ester formation or ether format...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L1/02C08B1/00C08B16/00C05G5/00C08J3/09C08J3/28C08L1/06C12N11/12D01F2/02
CPCC08L1/06C12N11/12C08J2301/02C08J3/28C08J3/096C08B1/003D01F2/02Y10T428/31772Y10T428/31971C08J11/08Y02W30/62
Inventor R·P·斯瓦特罗斯基R·D·罗杰斯J·D·霍尔布雷
Owner UNIVERSITY OF ALABAMA
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