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Basic ionic liquid catalyst and preparation method thereof

A liquid catalyst, basic ion technology, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc.

Active Publication Date: 2021-07-06
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most production workshops use sodium methoxide as a catalyst, which has a good catalytic effect, but the static reaction is used, and the conversion rate is low. The dynamic reaction is used to increase the conversion rate, but the amount of catalyst used is large, and side reactions are prone to occur, which is the cause of catalyst deactivation. , and generate sodium salt to block the reaction pipeline, the related reactions of sodium methoxide deactivation and blocked pipeline are as follows

Method used

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  • Basic ionic liquid catalyst and preparation method thereof
  • Basic ionic liquid catalyst and preparation method thereof
  • Basic ionic liquid catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] First, add a certain mass of n-bromobutane and N-methylimidazole into a 250ml round bottom flask at a molar ratio of 1:1.2 and condense and reflux, add a magnet to stir at a speed of 150-200r / min, and condense and reflux , take it out after reacting at 80°C for 48h, then wash it with ethyl acetate three times to obtain a light yellow viscous liquid, remove the ethyl acetate by rotary evaporation at 70°C and 0.08Mpa under reduced pressure, and then put it in a vacuum drying oven for 70 After drying at ℃ for 24h, the ionic liquid intermediate [Bmim]Br was obtained.

[0051] Dissolve an appropriate amount of [Bmim]Br in 50 mL of methanol, then add equimolar solid sodium methoxide, stir at room temperature for 10 h, slowly raise the temperature to 50 °C for 3 h, then raise the temperature to 80 °C for 3 h to obtain [Bmim] CH 3 O mixed with NaBr. Then use a suction filtration device to remove the NaBr precipitate, and remove methanol by rotary evaporation at 55° C. and 0.08...

Embodiment 2

[0054] In the same equipment used in Example 1, under the same conditions, bromobutane was changed into dodecane bromide to obtain methoxylated 1-dodecyl-3-methylimidazolium ionic liquid [ C 12 MIM]CH 3 O. The catalyst was used to catalyze the transesterification reaction of methanol and ethylene carbonate, and the yield of dimethyl carbonate was 71.6%.

Embodiment 3

[0056] In the same equipment used in Example 1, under the same conditions, brominated n-butane was changed into brominated octadecane to obtain methoxylated 1-octadecyl-3-methylimidazolium ionic liquid [ C 18 MIM]CH 3 O. The catalyst was used to catalyze the transesterification reaction of methanol and ethylene carbonate, and the yield of dimethyl carbonate was 72.5%.

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Abstract

The invention relates to a preparation method of an alkaline ionic liquid catalyst for methanol transesterification, in particular to a preparation method of a methoxylated alkylimidazole ionic liquid catalyst. In the preparation process of the catalyst, the invention firstly synthesizes the halogenated alkylimidazolium ionic liquid, and then uses the active methoxy anion to replace the halogen anion through a replacement reaction to synthesize the methoxylated alkylimidazolium ionic liquid. The ionic liquid catalyst has the same ion effect and synergistic effect with the methanol raw material, and exerts a strong catalytic effect in the methanol transesterification reaction. The generated dimethyl carbonate can form an azeotrope with methanol. During the reaction, the azeotrope is distilled and methanol raw material is added, which can break the static equilibrium, promote the reaction to move in the positive direction, form a new dynamic reaction equilibrium, and then realize Continuous industrial production.

Description

technical field [0001] The invention relates to a preparation method of an alkaline ionic liquid catalyst for methanol transesterification, in particular to a preparation method of a methoxylated alkylimidazole ionic liquid catalyst. Background technique [0002] Dimethyl carbonate is a green solvent with excellent properties and an important organic synthesis intermediate. Because it is non-toxic and harmless, it can replace highly toxic phosgene, methyl chloroformate, dimethyl sulfate and other methylating reagents or Hydroxylation reagents are widely used in textiles, printing and dyeing, leather, synthetic fibers, papermaking and machinery industries, and are known as "the new building block in the field of organic synthesis in the 21st century". With the advancement of science and technology and the popularization of high-end electronic products, the demand for dimethyl carbonate continues to increase. In terms of industrial production, dimethyl carbonate can replace hi...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C68/06C07C69/96
CPCB01J31/0284B01J2231/49C07C68/065C07C69/96
Inventor 郭立颖王逸蓉金先超吴昊马恩庆崔钟艺石开宇杜晶华王浩志
Owner SHENYANG POLYTECHNIC UNIV