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Method for carrying out catalytic conversion with high efficiency on cellulose at low temperature by utilizing compound ion liquid system

A compound ion and catalytic conversion technology, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, preparation of organic compounds, etc., can solve the problems of many intermediate steps, limited solubility, cumbersome operation, etc. Achieve the effects of low cost and operating expenses, reduced dosage, and simple process

Inactive Publication Date: 2014-07-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the limited solubility of cellulose in ionic liquids, the amount of ionic liquids in the above-mentioned system is relatively large, and the cellulose must be dissolved in ionic liquids to form a homogeneous solution, and then the homogeneous solution can be converted. There are many intermediate steps and the operation is cumbersome

Method used

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  • Method for carrying out catalytic conversion with high efficiency on cellulose at low temperature by utilizing compound ion liquid system
  • Method for carrying out catalytic conversion with high efficiency on cellulose at low temperature by utilizing compound ion liquid system
  • Method for carrying out catalytic conversion with high efficiency on cellulose at low temperature by utilizing compound ion liquid system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation of bmimCl (methyl butyl imidazolium chloride) ionic liquid solvent:

[0028] Fully mix 0.1mol N-methylimidazole and 0.12mol 1-chlorobutane, stir at 40°C for 12h, then raise the temperature to 70°C, and continue stirring for 24h to obtain a mixed solution; the mixed solution is washed with ethyl acetate and vacuum Dry to get Cl - Anionic liquid solvent.

Embodiment 2

[0030] Preparation of acidic ionic liquid catalyst:

[0031] Preparation of methylimidazole bisulfate acidic ionic liquid: fully mix 0.1mol N-methylimidazole and concentrated sulfuric acid with a mass fraction of 98% and stir in an ice-water bath for 1 hour, then fully wash with anhydrous ether, The solvent was removed from the obtained solution, and vacuum-dried at 70° C. for 10 h to obtain an acidic ionic liquid of methylimidazolium bisulfate.

[0032] Preparation of methyl butyl imidazolium bisulfate acidic ionic liquid: Weigh 0.1 mol of the corresponding cationic Cl - salt ionic liquid and dissolve it in 100 mL of methanol; then weigh the amount of the substance as Cl - Salt ionic liquid 2x KHSO 4 , dissolved in 30mL of methanol; the above solutions were combined, stirred at room temperature for 24h, filtered, the filtrate was removed by rotary evaporation, washed with anhydrous ether for 3 times, and then dried in a vacuum oven at 70°C for 12h to obtain methyl butyl im...

Embodiment 3

[0035] (1) Preparation of composite ionic liquid: in autoclave, 20g embodiment 1 gained bmimCl ionic liquid solvent and 3.5mmol embodiment 2 gained acidic ionic liquid catalyst are in N 2 Fully mixed in an ice-water bath under protection to obtain a composite ionic liquid;

[0036] (2) Catalytic conversion of cellulose: the compound ionic liquid gained in step (1) is mixed with 5g microcrystalline cellulose, adds 80ml normal hexane, through N 2 After 3 replacements, heat to 200°C and react for 15 minutes under 300r / min stirring condition. After the kettle body is cooled to room temperature, gas is released. The obtained product is extracted with n-hexane and ethyl acetate in sequence, and 50mL of CH is added to the raffinate. 3 OH, suction filtration, residue with CH 3 OH was fully washed, dried and weighed to calculate the conversion rate. The conversion rate and the yield of each phase product under different catalyst conditions are shown in Table 1:

[0037] Conversion r...

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Abstract

The invention discloses a method for carrying out catalytic conversion with high efficiency on cellulose at low temperature by utilizing a compound ion liquid system, comprising the following steps of: (1) preparation of a compound ion liquid: fully mixing an ion liquid solvent and an acid ion liquid catalyst in ice water bath under the protection of N2 to obtain the compound ion liquid; and (2) catalytic conversion of the cellulose: mixing the compound ion liquid and microcrystalline cellulose, adding a nonpolar solvent, and after N2 replacement, heating, stirring and reacting for 5-75 minutes to obtain a biochemical product. The cellulose is one of main components of biomass, and due to the adoption of the method provided by the invention, the cellulose in the biomass can be converted and prepared into bio-oil and biochemical products so that high-efficiency recycling of the cellulose is realized. The method has the advantages of simple process, mild conditions, small amount of ion liquid and realization of recycling, and the conversion rate of the cellulose under the optimized condition can be up to 100%.

Description

technical field [0001] The invention belongs to the fields of environmental protection technology and new energy technology development and utilization, and in particular relates to a method for using a composite ionic liquid system to catalyze and convert cellulose at low temperature and high efficiency. Background technique [0002] Modern scientific and technological progress has brought great convenience to people's production and life, but at the same time, it has also led to an increasing contradiction between the one-off fossil energy demand and its reserves. At the same time, CO released from burning fossil fuels x , NO x and SO x Harmful gases such as harmful gases have brought extremely serious environmental problems. In recent years, a large amount of CO has been emitted x Greenhouse effect, massive emission of NO x and SO x Environmental pollution such as acid rain caused by acidic gases such as acid rain has intensified, which has caused great harm to human...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07B41/12C07B41/04C07B41/06C07C49/603C07C45/00C07D307/34C10G1/00B01J31/02
Inventor 李雪辉龙金星郭斌于英豪王芙蓉王乐夫
Owner SOUTH CHINA UNIV OF TECH
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