Dissolution regeneration and stable dispersion system of monomolecular cellulose

A technology of dissolution regeneration and dispersion system, which is applied in the preparation of sulfonate and organic chemistry, etc. It can solve the problems of cellulose molecular macromolecular chain damage, high dissolution temperature, and long temperature for dissolving cellulose.

Active Publication Date: 2021-08-20
青岛量子元基环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the ionic liquid cations used in the dissolution of cellulose published in patents are imidazoles. Although there are nitrogen-rich triazole and tetrazole-type energetic ionic liquids, the cations of the ionic liquids are all monovalent charges, and the charge density is low. Dissolving High temperature and long time can damage the macromolecular chains of cellulose molecules
The ionic liquid with dual-nuclear structure announced by Chinese patent CN111057007A has two positive monovalent imidazole rings, but there are hydrocarbon chain links between the two positive monovalent imidazole rings, so that the charge density is very dispersed and remains stable when dissolving cellulose. It is equivalent to an ionic liquid with a monovalent charge of the ...

Method used

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  • Dissolution regeneration and stable dispersion system of monomolecular cellulose
  • Dissolution regeneration and stable dispersion system of monomolecular cellulose
  • Dissolution regeneration and stable dispersion system of monomolecular cellulose

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Synthesis of novel adenine ionic liquids:

[0026] Add 0.8mol of adenine to a 500mL single-necked round bottom flask, and then add 200mL of methanol and 2.4mol of tert-butoxycarbonic anhydride Boc 2 O was heated to reflux in a constant temperature oil bath at 45°C and stirred for 1 h. Then 2.45mol of 1-chloropropane was added, heated to reflux and stirred in a constant temperature oil bath at 40°C for 25h. After the reaction was completed, the solvent methanol was removed by heating and rotary evaporation. Add 2mL of 1mol / L HCl / dioxane, heat and stir in a constant temperature oil bath at 60°C for 1h to remove Boc, and remove HCl / dioxane and isobutene and CO produced by Boc by rotary evaporation under reduced pressure. 2 . Add 1.5g NaHCO 3 The remaining HCl was removed. The white solid in the lower layer was washed three times with ethyl propionate, then rotary evaporated under reduced pressure at 40°C, and then placed in a vacuum oven for 9 hours at 60°C to obtain ...

Embodiment 2

[0037] Ionic liquid recovery:

[0038] When preparing regenerated monomolecular cellulose, the mixed solution of ionic liquid and water was obtained. Firstly, it was subjected to vacuum rotary evaporation at 90°C, and then the aqueous solution of ionic liquid was frozen into a solid state in a refrigerator, and then put into a freeze dryer. Freeze-dry at ℃ for 24 hours, and remove the final remaining small amount of distilled water. Wait for the temperature to slowly rise to room temperature in a desiccator to obtain a pure ionic liquid.

[0039] Application of monomolecular cellulose as water retaining agent:

[0040] Prepare 775.0g of gypsum powder, add 0.80g of monomolecular cellulose, and then add 240.3g of water and stir evenly to make mortar. After adding gypsum mortar to the Buchner funnel with a mass of 847.0g, the total mass is 1208.5g, and the total mass of the funnel after suction filtration is 1200.0g. The calculated water retention rate of monomolecular cellulo...

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Abstract

The invention relates to a dissolution regeneration and stable dispersion system of monomolecular cellulose. In order to separate and obtain monomolecular chain cellulose and large-scale application of the monomolecular cellulose, adenine cations of prepared high-charge nitrogen-rich adenine trifluoromethanesulfonic acid ionic liquid [Aden] (CF3SO3) 3 have three positive charges, one adenine cation [Aden] < 3 + > can be simultaneously complexed with three O atoms on three hydroxyl groups of cellulose molecules, and a-NH2 group and a-NH-group of the adenine cation [Aden] < 3 + > and an anion CF3SO3- simultaneously form a new hydrogen bond network with H atoms on the hydroxyl groups of the cellulose molecules; the high-charge nitrogen-rich adenine ionic liquid [Aden] (CF3SO3) 3 can dissolve cellulose within a short time in a low temperature range including room temperature. According to a prepared polyethylene glycol lauric acid histidine ester dispersion stabilizer, the cellulose molecules are uniformly dispersed without hydrogen bond aggregation when being separated out from the ionic liquid, and after the cellulose is centrifugally separated, single cellulose molecules still exist stably under the dispersion effect of the polyethylene glycol lauric acid histidine ester dispersion stabilizer.

Description

technical field [0001] The invention relates to a high-charge-density ionic liquid for dissolving and regenerating unimolecular cellulose and its preparation, as well as a dispersion stabilizer for unimolecular cellulose separation and its preparation, in particular to a dissolving, regenerating and regenerating unimolecular cellulose Stable dispersion system. Background technique [0002] Cellulose is the most abundant renewable natural polymer on earth, with up to 90% cellulose in cotton. However, the strong hydrogen bonding between and within the cellulose molecules, as well as the complex aggregate structure and high crystallinity of cellulose molecules limit the wide application of cellulose. Therefore, researchers have developed solvents for dissolving cellulose, including organic solvent systems, aqueous solvent systems, and ionic liquids. Organic solvent systems include paraformaldehyde / dimethylsulfoxide (PF / DMSO) system, dinitrogen tetroxide / dimethylformamide (N ...

Claims

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Application Information

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IPC IPC(8): C08J3/09C08L1/02C08L71/02C08L1/28C07D473/34C07C309/06C07C303/32
CPCC08J3/096C07D473/34C07C309/06C07C303/32C08J2301/02C08J2471/02C08J2301/28Y02P20/54
Inventor 刘元会张云波谢蕾徐振民高于斐
Owner 青岛量子元基环保科技有限公司
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