Cellulose solution, cellulose dissolution method and regenerated cellulose

A cellulose solution and cellulose technology, applied in the field of regenerated cellulose, can solve the problems of limited industrial utilization process, complexity, and huge influence of ionic liquid solubility.

Inactive Publication Date: 2014-04-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] 1) The solubility of ionic liquids is greatly affected by moisture, and the water must be vacuumed before use, which is a high-energy-consuming process;
[0023] 2) Ionic liquids are expensive, difficult and complicated to recover and purify;
[0024] 3) Bio-based materials are prepared by dissolving biomass polymers in ionic liquids, and ionic liquids have some residues. Due to the biological toxicity of ionic liquids, their industrial utilization is limited
[0025] 4) The ionic liquid cellulose or biomass polymer solution has a high viscosity and does not use industrial processes for treatment
However, there are no patents and literature reports for the dissolving and processing of cellulose by this type of solvent

Method used

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  • Cellulose solution, cellulose dissolution method and regenerated cellulose
  • Cellulose solution, cellulose dissolution method and regenerated cellulose
  • Cellulose solution, cellulose dissolution method and regenerated cellulose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0189] described in this patent can be used with CO 2 One or two or more compounds that form switch-type reversible ionic compounds, we press the chemical equivalent tetramethylguanidine (TMG) and ethylene glycol in DMSO, in CO 2 The formation of switch-type reversible ionic compounds in the atmosphere is illustrated. This type of CO 2 The formation of switch-type reversible ionic compounds is the key to the ability of the mixed system described in the present invention to dissolve cellulose. We validated [TMGH] by NMR techniques 2 2+ [O 2 COCH 2 CH 2 OCO 2 ] 2- Formation. For specific test results, see Figure 1 , Figure II .

Embodiment 2

[0191] The dissolving system described in the present invention, its dissolving capacity can be adjusted by CO 2 The structure of the switch-type ionic compound, the dissolution temperature and the dissolution time are adjusted. When the total mass of the solution is set to 20.0 g, it will be compatible with CO 2 One or two or more compounds that form reversible ionic compounds and DMSO are added to the reactor at a certain molar ratio, a certain amount of microcrystalline cellulose is added to the mixed system, the reactor is covered and closed, and 2MPa CO 2 Gas, under stirring, heated to a certain temperature, dissolved for 12 hours, released to obtain a cellulose solution. The experimental results are summarized in the following table:

[0192]

[0193]

[0194]

[0195] From the table, we found that the system composed of strong organic base guanidine compounds and squint compounds and alcohol compounds, such as methanol, ethanol, ethylene glycol, and glycerin,...

Embodiment 3

[0197] The patent described by using organic solvents with good swelling effect on cellulose and CO 2 switch-type ionic compound mixture, although this type of solvent is for CO 2 It is not necessary for the switch-type ionic compound to dissolve cellulose, but the use of this type of solvent can greatly accelerate the dissolution rate and solubility, and at the same time reduce the viscosity of the obtained cellulose solution, thereby greatly improving its subsequent processing and use.

[0198] Mix tetramethylguanidine (0.036 moles, 4.14 grams), ethylene glycol (0.018 moles, 1.14 grams), a certain amount of organic solvent and 1.6 grams of microcrystalline cellulose, add to the reaction kettle, cover and seal the reaction kettle, and pass into P at a certain pressure CO2 =2MPa gas, under stirring, heat the system to 80°C, dissolve for 10 hours, and obtain a cellulose solution. The experimental results are summarized as follows:

[0199]

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Abstract

The invention relates to a method for dissolving cellulose in a CO2 switchable ionic compound or a mixed system composed of a CO2 switchable ionic compound and an organic solvent. Various anti-solvents are added into the system, or a gas is introduced into the system or heating is conducted to destroy the structure of a CO2 switchable solvent. The dissolved cellulose regenerates in various physical structure forms. By adjusting the CO2 pressure, and selecting organic amine or alcohol of cations and anions able to compose a CO2 switchable ionic compound or the structure of an assistant organic solvent, the solubility of cellulose and various properties of the solution can be controlled.

Description

technical field [0001] The invention belongs to the field of cellulose processing and application, and in particular relates to a cellulose solution, a method for dissolving cellulose and regenerated cellulose. Background technique [0002] Provenance, technical status, existing problems [0003] While the chemical industry meets our growing material and cultural needs, it also has a serious impact on our environment due to its excessive dependence on petroleum resources. At the same time, with the depletion of petroleum resources, the efficient use of biorenewable resources, as a "carbon neutral" resource, has gained a lot of attention. The use of biomass resources to prepare green materials and high value-added chemicals through chemical catalysis and biotransformation methods has been a hot spot in scientific research so far. [0004] Cellulose is one of the most widely distributed and abundant natural biomass resources in nature, and its renewable and biodegradable cha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/09C08L1/02C08B16/00
Inventor 谢海波赵宗保
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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