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Method for preparing solvent system capable of dissolving cellulose under room temperature condition

A technology for dissolving cellulose and system, applied in the field of preparation of solvent system, can solve the problems of pollution, excessive raw material, product decomposition, etc., and achieve the effects of reducing environmental pollution, short reaction time and high conversion rate

Inactive Publication Date: 2014-02-05
NANKAI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Second, the preparation process of these ionic liquids is cumbersome and the efficiency is low
Microwave heating can greatly shorten the reaction time, but the reaction conditions are difficult to control, and it is easy to cause the decomposition of the product
Ultrasound-assisted synthesis of ionic liquids still requires heating and still requires a long reaction time
In addition, in the synthesis methods of these ionic liquids, an excess of a raw material is generally required, and an organic solvent needs to be used to remove unreacted raw materials after the reaction, which not only increases the cost, but also brings additional pollution
Third, the viscosity of the ionic liquid solution of cellulose is relatively high
Patent CN 101215725A discloses a mixed solvent composed of ionic liquid 1-butyl-3-methylimidazolium acetate (BMIMAc) and dimethyl sulfoxide (DMSO), which can dissolve cellulose at room temperature, but The solvent is prepared by adding dimethyl sulfoxide (DMSO) to 1-butyl-3-methylimidazolium acetate (BMIMAc), while 1-butyl-3-methylimidazole acetate ( The preparation process of BMIMAc) is loaded down with trivial details, and needs to use a large amount of organic solvents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1-allyl-3-methylimidazolium acetate (AMIMAc) and dimethyl sulfoxide (DMSO) with a mass ratio of 1:1 constitute a mixed solvent system, which is prepared by the following steps:

[0020] 1) Add N-methylimidazole and dimethyl sulfoxide into a three-necked flask with a mass ratio of 1:2.2, mix and fully dissolve to obtain a system solution;

[0021] 2) Slowly add allyl bromide dropwise under ice bath conditions, the molar ratio of added allyl bromide to N-methylimidazole is 1:1, after the addition is complete, keep the ice bath reaction for 1h;

[0022] 3) Keeping the temperature at 50°C, heat and reflux for 1 hour to prepare a solvent system composed of ionic liquid 1-allyl-3-methylimidazolium bromide (AMIMBr) and dimethyl sulfoxide;

[0023] 4) Add saturated silver acetate solution to the above solvent system, the molar ratio of silver acetate to propylene bromide is 1:1, fully stir the reaction, filter to remove the lead bromide precipitate, and then remove the water in...

Embodiment 2

[0026] A mixed solvent system consisting of 1-butyl-3-methylimidazole acetate (BMIMAc) and dimethyl sulfoxide (DMSO) with a mass ratio of 1:1 was prepared by the following steps:

[0027] 1) Add N-methylimidazole and dimethyl sulfoxide into a three-necked flask with a mass ratio of 1:2.4, mix and fully dissolve to obtain a system solution;

[0028]2) Under the condition of ice bath, slowly add bromobutane dropwise, the amount of bromobutane added is 1:1 to N-methylimidazole, after the dropwise addition, the ice bath reaction is kept for 1h.

[0029] 3) Keeping the temperature at 60°C, heat and reflux for 2 hours to prepare a solvent system composed of 1-butyl-3-methylimidazolium bromide and dimethyl sulfoxide;

[0030] 4) Add saturated lead acetate solution to the above solvent system, the molar ratio of lead acetate solution to bromobutane is 1:2, fully stir the reaction, filter to remove the silver bromide precipitate, and then remove the water in the filtrate by rotary evap...

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PUM

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Abstract

The invention discloses a method for preparing a solvent system capable of dissolving cellulose under a room temperature condition. The solvent system is composed of ionic liquid and dimethyl sulfoxide, wherein anions in the ionic liquids are acetate ions, cations are N-R1 and N-R2 imidazole cations; in the formula, R1 is methyl or ethyl, R2 is ethyl, allyl or butyl. The method comprises the following preparation steps: mixing and fully dissolving N-methylimidazole or N-ethylimidazole and the dimethyl sulfoxide; slowly dripping bromo-hydrocarbon R2Br under an ice bath condition to react; heating to carry out a reflux reaction at a temperature of 40-70 DEG C; and adding a saturated lead acetate or silver acetate solution, stirring to react, filtering precipitate, and removing water in filtrate through a rotary evaporation method to prepare the solvent system. The method disclosed by the invention has the advantages that the preparation method is short in reaction time, free of pollution and high in synthesis efficiency and conversion rate; and the solvent system can dissolve a large amount of non-activated or non-pretreated cellulose under the room temperature condition.

Description

technical field [0001] The invention relates to a preparation technology of a cellulose solvent system, in particular to a preparation method of a solvent system capable of dissolving cellulose at room temperature. Background technique [0002] As one of the most abundant renewable resources on earth, cellulose and its derivatives are widely used in the fields of food, medicine, composite materials, textiles and energy. During the production process, the cellulose needs to be dissolved first. However, natural cellulose has a high degree of crystallinity and a large number of hydrogen bonds in and between molecules, which makes it difficult to dissolve in water and common organic solvents. With the efforts of many researchers, people have discovered a variety of solvent systems for dissolving cellulose. These solvent systems mainly include: NaOH / CS 2 system, protonic acid system, DMAc / LiCI, TBAF / DMSO, DMF / N 2 o 4 , LiC1O 4 ·3H 2 O, LiSCN 2H 2 O and NMMO systems. Amo...

Claims

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Application Information

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IPC IPC(8): C08J3/09C08L1/02
CPCY02P20/54
Inventor 候其东李维尊鞠美庭邵超峰韩国林董文静刘乐江洋刘益良范丽丽蔡昀昭王雁南
Owner NANKAI UNIV
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