Photoresponse ionic liquid capable of dissolving cellulose as well as preparation method and application thereof

A technology for dissolving cellulose and ionic liquids, which is applied in the field of light-responsive ionic liquids and their preparation, can solve the problems of limited operating temperature of ionic liquids, complex methods of recovering ionic liquids, and difficulty in recycling and reusing ionic liquids, etc., to achieve Effect of good photoisomerization performance

Active Publication Date: 2020-11-24
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this patent is that the preparation method is simple, the reaction conditions are mild, and the operation is convenient; the disadvantage is that the recovery and reuse of the ionic liquid is not easy
[0007] There are certain defects in the preparation and recovery of ionic liquids for soluble cellulose in the prior art: there is a problem of energy consumption in the use of vacuum distillation during recovery, and the use of temperature variability to recover the reversible phase tra...

Method used

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  • Photoresponse ionic liquid capable of dissolving cellulose as well as preparation method and application thereof
  • Photoresponse ionic liquid capable of dissolving cellulose as well as preparation method and application thereof
  • Photoresponse ionic liquid capable of dissolving cellulose as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0064] A method for preparing a cellulose-soluble photoresponsive ionic liquid, comprising the steps of:

[0065] (1) Add 2.0 g of KOH, 0.297 g of KI catalyst, 4.00 ml of 1,3-dichloropropane and 10 ml of acetone into a 100 ml three-neck flask under nitrogen protection. Turn on the oil bath for magnetic stirring and heating, set the temperature to 60°C, and the stirring rate to 180r / min. The temperature of the reaction vessel was maintained at 60-65° C., the stirring rate was constant, and the reflux phenomenon was waited for.

[0066] (2) After a stable reflux occurs, weigh 2.1g of 4-hydroxyazobenzene and dissolve it in 20ml of acetone, and slowly add it dropwise for 1 hour. After the dropwise addition, maintain the current temperature and rotation speed to react for 24 hours.

[0067] (3) After the reaction is completed, the solution is filtered while it is hot, and the filter residue is washed with acetone to obtain a washing solution. The collected filtrate and washing so...

Embodiment 2

[0078] A method for preparing a cellulose-soluble photoresponsive ionic liquid, comprising the steps of:

[0079] (1) Add 1.889g of KOH, 0.287g of KI catalyst, 4.00ml of 1,3-dichloropropane and 10ml of acetone into a 100ml three-neck flask under nitrogen protection. Turn on the oil bath for magnetic stirring and heating, set the temperature at 65°C, and the stirring rate at 190r / min. The temperature of the reaction vessel was maintained at 60-67° C., the stirring rate was constant, and the reflux phenomenon was waited for.

[0080] (2) After a stable reflux occurs, weigh 2.517g of 4-hydroxyazobenzene and dissolve it in 18ml of acetone, and slowly add it dropwise for 1 hour. After the dropwise addition, maintain the current temperature and rotation speed to react for 24 hours.

[0081] (3) After the reaction is completed, the solution is filtered while it is hot, and the filter residue is washed with acetone to obtain a washing solution. The collected filtrate and washing sol...

Embodiment 3

[0089] A method for preparing a cellulose-soluble photoresponsive ionic liquid, comprising the steps of:

[0090] (1) Add 1.903g of KOH, 0.201g of KI catalyst, 4.5ml of 1,3-dichloropropane and 12ml of acetone into a 100ml three-neck flask under nitrogen protection. Turn on the oil bath for magnetic stirring and heating, set the temperature at 62°C, and the stirring rate at 185r / min. The temperature of the reaction vessel was maintained at 60-65° C., the stirring rate was constant, and the reflux phenomenon was waited for.

[0091] (2) After a stable reflux occurs, weigh 2.713g of 4-hydroxyazobenzene and dissolve it in 20ml of acetone, and slowly add it dropwise for 1 hour. After the dropwise addition, maintain the current temperature and rotation speed to react for 24 hours.

[0092] (3) After the reaction is completed, the solution is filtered while it is hot, and the filter residue is washed with acetone to obtain a washing solution. The collected filtrate and washing solu...

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Abstract

The invention belongs to the technical field of ionic liquids, and particularly relates to a photoresponse ionic liquid capable of dissolving cellulose as well as a preparation method and applicationthereof. The preparation method comprises the following steps: under the protection of nitrogen, stirring and refluxing 1,3-dichloropropane, acetone, KOH and KI to obtain a mixed solution; dissolving4-hydroxyazobenzene into acetone, adding a dissolved solution into the mixed solution, and continuing stirring for reaction; adding petroleum ether, performing standing, cooling, precipitating and filtering, and collecting and drying filter residues to obtain 1-chloro-3-(4-oxyazobenzene) propane; and carrying out reflux reaction on 1-chloro-3-(4-oxyazobenzene) propane, 1-methyl-1H-imidazole and ethanol under the protection of the nitrogen to obtain the photoresponse ionic liquid capable of dissolving cellulose. The photoresponsive ionic liquid prepared by the method has photoisomerization andcan dissolve cellulose, and the hydrophilicity and hydrophobicity of the photoresponsive ionic liquid are regulated and controlled by light so as to realize effective separation of the ionic liquid and water, so that the ionic liquid is easy to recycle.

Description

technical field [0001] The invention belongs to the technical field of ionic liquids, and in particular relates to a photoresponsive ionic liquid capable of dissolving cellulose, a preparation method and application thereof. Background technique [0002] The dissolution of cellulose has always been a difficult problem in cellulose processing, conversion and utilization. As a new type of green solvent, ionic liquids have shown a broad range in cellulose dissolution due to their advantages such as low volatility, good thermal stability, and good solubility. application prospects. Ionic liquids have good solubility to cellulose, and have great potential application value in the regeneration and sustainable development of biomass energy. However, the price of ionic liquids is relatively high and there are certain pollution problems when they are lost to the environment. Therefore, It is necessary to efficiently recycle and reuse them. [0003] The existing ionic liquid recover...

Claims

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Application Information

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IPC IPC(8): C07D233/60C08J3/09C08L1/04
CPCC07D233/60C08J3/096C08J2301/02
Inventor 王晶薛静程宇萌黄昊飞谢雨航宋暖张晶晶李玉超左村村
Owner SHANDONG UNIV OF TECH
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