Multi-element ionic liquid as well as preparation method and application thereof

A multi-ion and ionic liquid technology, applied in the preparation of carboxylate, the preparation of carboxylate, organic chemical methods, etc., can solve the problems of complex synthesis steps of imidazolium-based ionic liquids, a large number of toxic gases and waste water, severe environmental problems, etc., To achieve the effect of favorable dissolution, low cost and easy operation

Active Publication Date: 2022-03-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing cellulose dissolving system still has the following disadvantages: such as the cumbersome process flow of the viscose method, the production of a large amount of toxic gas and waste water, and severe environmental problems
At present, the ionic liquids that can be used for cellulose dissolution are mainly imidazole-based, but the synthesis steps of imidazole-based ionic liquids are complex, costly, and difficult to recycle, and there are still many challenges in large-scale industrial production and application.
Moreover, most imidazolium-based ionic liquids contain halogen anions, which cause corrosion to equipment and also have the disadvantage of polluting the environment

Method used

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  • Multi-element ionic liquid as well as preparation method and application thereof
  • Multi-element ionic liquid as well as preparation method and application thereof
  • Multi-element ionic liquid as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Synthesis and characterization of the present invention's gained polynary ionic liquid:

[0035]

[0036] Synthesis of ionic liquid DBNH-AdA: Take adipic acid 14.6g (0.1mol, 1.0eq.) and 1,5-diazabicyclo[4,3,0]non-5-ene 24.8g (DBN, 0.2mol , 2.0eq.) in a 150mL flask, heated to 90°C and stirred for 3h. After the reaction, without separation and purification, the product was cooled to room temperature, and 38.8 g of a light pink solid was precipitated, with a yield of 98.5%, which was sealed and stored for later use. The NMR spectrum of the product DBNH-AdA is shown in the attached figure 1 Shown, indicating the correct synthesis of the structure of the ionic liquid.

[0037] The synthesis of other polybasic ionic liquids can be replaced with different superbases, dibasic acids and tribasic acids according to the above steps, according to the molar ratio (organic base: dibasic acid = 2: 1, organic base: tribasic acid = 3: 1 ) synthesized to get, figure 2 (a) and (b) ...

Embodiment 2

[0043] The dissolving of cellulose by solvent system of the present invention gained, concrete steps are as follows:

[0044] 1. Preparation of solvent system: Take 16 g of multi-component ionic liquid DBNH-AdA obtained in Example 1 in a 100 mL flask, add 12 g of auxiliary agent dimethyl sulfoxide, heat to 80 ° C and stir evenly to obtain a solvent system with a mass fraction of 57.1%. , denoted as DBNH-AdA / DMSO-57.1.

[0045]2. Microcrystalline cellulose dissolving: take DBNH-AdA / DMSO-57.1 (14g) obtained in step 1, add 0.56g of microcrystalline cellulose (DP=180), heat to 80°C, and stir for 0.5h at a speed of 180rmp to obtain Clear cellulose solution. Take a little sample before and after dissolution and observe under the microscope, as shown in image 3 (a) As shown in (b), there is no microcrystalline cellulose in the solution sample, indicating that the solvent system completely dissolves microcrystalline cellulose.

[0046] 3. Maximum solubility test: Take 6g of part o...

Embodiment 3

[0054] The preparation of the gained regenerated cellulose film of the present invention, concrete steps are as follows:

[0055] Solvent systems DBNH-AdA-DMSO-60%, DBNH-PeA-DMSO-60%, DBUH-AdA-DMSO-60%, and DBUH-PeA-DMSO-60% were respectively prepared according to the method in step 3 of Example 2. Take 20 g of the prepared cellulose solvent system, raise the temperature to 85° C., add 0.40 g of wood pulp cellulose under stirring at 200 rpm, and continue stirring for 2 hours to obtain a clear and transparent cellulose solution. After dissolving, put the cellulose solution at 80°C for static defoaming, then pour it into a glass petri dish (diameter 5cm, 4.5g per dish) to form a film, then immerse it in the coagulation bath for a period of time, take it out, and continue to use water to form a film. After fully rinsing and drying, a regenerated cellulose film is obtained. The obtained regenerated cellulose is obtained by XRD spectrum through X-ray diffraction instrument, tensil...

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Abstract

The invention belongs to the technical field of cellulose solutions, and discloses a polybasic ionic liquid and a preparation method and application thereof, the ionic liquid has one of the following general formulas: C + A2-C + and C + A3-C +-C +, in the general formulas, C + is a super alkali cation, and A2-and A3-in the general formulas are binary and ternary organic acid anions. The ionic liquid disclosed by the invention is simple to prepare and low in cost, and is prepared only by reacting organic super alkali with binary and ternary organic acids under a solvent-free condition, and subsequent separation and purification are not needed. According to the invention, polybasic organic acid is introduced into the super-alkaline ionic liquid to prepare the polybasic super-alkaline ionic liquid. The multi-element ionic liquid has a multi-cation and multi-anion structure, can provide more hydrogen bond binding sites and is beneficial to dissolution of cellulose, and the cellulose membrane material can be obtained after the dissolved cellulose is solidified and regenerated by water.

Description

technical field [0001] The invention relates to a cellulose solvent and its preparation method and application, belonging to the technical field of cellulose solvents. Background technique [0002] Cellulose is the most abundant natural renewable resource in nature. Making full use of cellulose can reduce the consumption of petroleum resources and reduce environmental pollution. Biomass-based materials such as films, silks, gels, micelles, and microspheres developed from cellulose and its derivatives such as esters or ethers can be widely used in textiles, packaging, papermaking, biomass plastics, drug carriers, coatings, and Daily chemicals and many other fields. The development and application of these materials are closely related to the solubility of cellulose. However, due to the abundant intramolecular and intermolecular hydrogen bonds in cellulose, the complex aggregation state and crystal structure, cellulose cannot be dissolved in conventional solvents. Therefore,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04C07C51/41C07C59/245C07C59/255C07C55/07C07C55/08C07C55/10C07C55/12C07C55/14C07C55/16C07C55/18C07C55/20C07C55/02C07C57/15C07C57/145C07C227/18C07C229/24C08J3/09C08J5/18C08L1/04
CPCC07D487/04C07C51/412C07C59/245C07C59/255C07C55/07C07C55/08C07C55/10C07C55/12C07C55/14C07C55/16C07C55/18C07C55/20C07C55/02C07C57/15C07C57/145C07C227/18C07C229/24C08J3/096C08J3/095C08J5/18C08J2301/04C07B2200/07
Inventor 王小慧帅建波高相立赵俊萌
Owner SOUTH CHINA UNIV OF TECH
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