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Solvent recovery method in cellulosic fiber preparation with ionic liquid as solvent

A cellulose fiber and ionic liquid technology, applied in the direction of concentrating waste liquid, etc., can solve the problems of difficulty in carrying out, high energy consumption for recovery, and achieve the effects of low cost, simple recovery process and reduced production cost.

Inactive Publication Date: 2009-08-12
CHTC HELON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent 200510108024.X discloses a method of recovering hydrophobic and hydrophilic ionic liquids by extraction, and some methods of recovering ionic liquids by distillation, but the above recovery methods are only suitable for the production and use of cellulose fibers When the water content in the ionic liquid is low, the recovery of the ionic liquid is carried out. In the case of a high water content in the ionic liquid after cellulose fiber production and use, the recovery of the ionic liquid by the above method requires high energy consumption and is not easy to carry out.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Use [BMIM]Cl with a mass content of 100% as a solvent to prepare a spinning solution with a mass content of cotton pulp of 8% for wet spinning, use water as a coagulant, and after spinning for a period of time, take out 10000g of it from the coagulation water bath and the temperature is 93 °C solution containing [BMIM]Cl, after chemical titration, it is known that this 10000g solution contains 2.7g of ionic liquid [BMIM]Cl;

[0021] Filter 10000g of the solution to remove solid particulate impurities;

[0022] After filtration, the temperature of the liquid dropped to 75°C, and a reverse osmosis membrane with a pore size of 20 nanometers was used to perform three-stage membrane concentration, and the quality of the solution containing the ionic liquid was 115 g;

[0023] Under the condition of 300 Pa, 125° C. was distilled under reduced pressure for 2 hours to finally obtain 22.5 g of an ionic liquid-containing solution with a water mass content of 0.8%, and the recover...

Embodiment 2

[0025] Using the ionic liquid mixture of [BMIM]Cl and [AMIM]Cl with a molar ratio of 8:2 as a solvent, prepare a spinning solution with a mass content of wood pulp of 5% for wet spinning, use water as a coagulant, and spin for one stage After a period of time, take out 10000g of the solution containing [BMIM]Cl and [AMIM]Cl at a temperature of 90°C from the water bath. After chemical titration, it is known that the 10000g solution contains ionic liquid [BMIM]Cl30.7g;

[0026] Filter 10000g of the solution through 80 bleached poplins with one layer of filter material to remove solid particulate impurities therein;

[0027] After filtering through bleached poplin, the temperature of the solution dropped to 70°C, and a reverse osmosis membrane with a pore size of 16 nanometers was used for the first-stage membrane concentration, and the mass of the solution containing the ionic liquid was 118g;

[0028] Under the condition of 70Pa, 106° C. was distilled under reduced pressure for...

Embodiment 3

[0030] Use an ionic liquid with a mass content of 100% [AMIM]Cl as a solvent to prepare a spinning solution with a mass content of 9% of bamboo pulp for wet spinning, use water as a coagulant, and after spinning for a period of time, take out 10000g of bamboo pulp from the water coagulation bath A solution containing [AMIM]Cl at a temperature of 90°C. After chemical titration, it is known that the ionic liquid [BMIM]Cl contained in this 10000g solution is 39.5g;

[0031] 10000g solution is filtered through 80 bleached poplins with 3 layers of filter material to remove solid particulate impurities therein;

[0032] After being filtered by bleached poplin, the temperature of the solution dropped to 65°C, and a membrane with a pore size of 40 nm was used for three-stage membrane concentration, and the mass of the solution containing the ionic liquid was 263 g;

[0033] Under the condition of 800 Pa, 96° C. was distilled under reduced pressure for 5 hours to finally obtain 39.7 g ...

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Abstract

The invention discloses a method for reclaiming solvent in cellulose fiber preparation taking ionic liquid as the solvent, which comprises the following steps: filtering solution containing the ionic liquid to remove solid particle impurities; performing film condensation by a reverse osmosis membrane; and distilling the condensed solution containing the ionic liquid under reduced pressure to make the mass content of water in the solution containing the ionic liquid less than or equal to 2 percent, and obtaining the reclaimed ionic liquid. The method is suitable for reclaiming the solution containing the ionic liquid in wide concentration range, and has low energy consumption and easy implementation.

Description

technical field [0001] The invention relates to a method for purifying and recovering ionic liquid produced during the preparation of cellulose fibers using ionic liquid as a solvent. Background technique [0002] Cellulose is a renewable resource that is ubiquitous in nature. Trees, cotton, rice stalks, corn and other plants and some bacterial secretions contain a lot of cellulose. Cellulose fibers may become a renewable resource to replace petroleum-based fibrous products. At present, the production of cellulose fiber mainly uses sodium hydroxide, acetone, carbon disulfide, etc. as solvents and additives, and the cellulose used needs to be yellowed, aged and matured, and it also involves formaldehyde, sulfite, sodium sulfide, sulfuric acid And chemical reagents such as zinc sulfate, all of the above-mentioned organic reagents are volatile, causing serious pollution to the environment and endangering the health of operators; and inorganic reagents are highly corrosive, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21C11/10
CPCY02P70/10
Inventor 逄奉建刘建华马君志李琳马峰刚姜明亮
Owner CHTC HELON
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