Cellulose-soluble photoresponsive ionic liquid and its preparation method and application

A technology for dissolving cellulose and ionic liquids, which is applied in the field of light-responsive ionic liquids and their preparations, and can solve the problems of difficult recovery and reuse of ionic liquids, complicated methods for recovering ionic liquids, and limitations in the use temperature of ionic liquids.

Active Publication Date: 2022-04-12
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 transition of ionic liquids has a negative impact on the use temperature of ionic liquids. Limitations, complex methods for recovering ionic liquids, etc.
Therefore, the existing methods cannot meet the needs of efficient recovery and effective reuse of ionic liquids. At present, there is an urgent need for an environmentally friendly new method that is easy to operate, simple in equipment, low in energy consumption, and free from cross-contamination to recover ionic liquids and achieve multiple cycles. Reuse

Method used

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  • Cellulose-soluble photoresponsive ionic liquid and its preparation method and application
  • Cellulose-soluble photoresponsive ionic liquid and its preparation method and application
  • Cellulose-soluble photoresponsive ionic liquid and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] The preparation method of the cellulose-soluble light-responsive ionic liquid comprises the following steps:

[0065] (1) 2.0g KOH, 0.297g KI catalyst, 4.00ml 1,3-dichloropropane and 10ml acetone were added to a 100ml three-necked flask under nitrogen protection. Open the oil bath pot for magnetic stirring and heating, set the temperature to 60°C, and set the stirring rate to 180 r / 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 stable reflux occurs, 2.1 g of 4-hydroxyazobenzene is weighed and dissolved in 20 ml of acetone, and slowly added dropwise for 1 h. After the dropwise addition, the reaction was carried out at the current temperature and rotation speed for 24h.

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

Embodiment 2

[0078] The preparation method of the cellulose-soluble light-responsive ionic liquid comprises the following steps:

[0079] (1) 1.889g KOH, 0.287g KI catalyst, 4.00ml 1,3-dichloropropane and 10ml acetone were added to a 100ml three-necked flask under nitrogen protection. Open the oil bath pot for magnetic stirring and heating, set the temperature to 65°C, and set the stirring rate to 190 r / 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 stable reflux occurs, weigh 2.517 g of 4-hydroxyazobenzene, dissolve it in 18 ml of acetone, and slowly add it dropwise for 1 h. After the dropwise addition, the reaction was carried out at the current temperature and rotation speed for 24h.

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

Embodiment 3

[0089] The preparation method of the cellulose-soluble light-responsive ionic liquid comprises the following steps:

[0090] (1) 1.903 g of KOH, 0.201 g of KI catalyst, 4.5 ml of 1,3-dichloropropane and 12 ml of acetone were added to a 100 ml three-necked flask under nitrogen protection. Open the oil bath pot for magnetic stirring and heating, set the temperature to 62°C, and set the stirring rate to 185 r / 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 stable reflux occurs, weigh 2.713 g of 4-hydroxyazobenzene, dissolve it in 20 ml of acetone, and slowly add it dropwise for 1 hour. After the dropwise addition, the reaction was carried out at the current temperature and rotation speed for 24h.

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

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Abstract

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. Under nitrogen protection, 1,3-dichloropropane, acetone, KOH and KI were stirred and refluxed to obtain a mixed solution; 4-hydroxyazobenzene was dissolved in acetone and then added to the mixed solution to continue the stirring reaction; petroleum ether was added and allowed to stand After cooling, precipitate, filter, collect and dry the filter residue to obtain 1-chloro-3-(4-oxygenazobenzene) propane; 1-chloro-3-(4-oxygenazobenzene) propane, 1-methyl ‑1H‑imidazole and ethanol were refluxed under nitrogen protection to obtain a photoresponsive ionic liquid that can dissolve cellulose. The photoresponsive ionic liquid prepared by the invention has photoisomerization and can dissolve cellulose, and its hydrophilicity and hydrophobicity can be adjusted by light to realize the effective separation of the ionic liquid and water, so that the ionic liquid can be easily recycled and reused.

Description

technical field [0001] The invention belongs to the technical field of ionic liquids, and in particular relates to a light-responsive ionic liquid that can dissolve cellulose and a preparation method and application thereof. Background technique [0002] The dissolution of cellulose has always been a difficult problem in the processing and conversion of cellulose. As a new type of green solvent, ionic liquids have the advantages of low volatility, good thermal stability, and good solubility, and have shown a broad range of cellulose dissolution. application prospects. Ionic liquids have good solubility for 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. It is necessary to recycle them efficiently. [0003] Existing ionic liquid recovery methods include distillation, aqu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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