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Caprolactam basic ionic liquid as well as preparation method and application thereof

A caprolactam, basic ion technology, applied in liquid carbon-containing fuels, chemical instruments and methods, fatty acid esterification, etc., can solve the problem of low activity of biodiesel, achieve strong alkalinity, mild reaction conditions and simple synthesis. Effect

Active Publication Date: 2013-08-28
南通东湖国际旅行社有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] In view of the problem that acidic caprolactam-based ionic liquids are not highly active in catalyzing waste oils to prepare biodiesel in the prior art, a dual-functional catalyst (that can be used as a catalyst and as a solvent, simultaneously catalyzing two steps of esterification and transesterification) is provided. Reaction) active caprolactam-based alkaline ionic liquid, a one-step catalytic method for preparing biodiesel from waste oil

Method used

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  • Caprolactam basic ionic liquid as well as preparation method and application thereof
  • Caprolactam basic ionic liquid as well as preparation method and application thereof
  • Caprolactam basic ionic liquid as well as preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0043] Weigh 10g of N-methyl caprolactam, dissolve it in ethanol solvent and put it into a four-necked flask. The amount of ethanol is 10% of the mass of N-methyl caprolactam. In the constant pressure separatory funnel, the molar ratio of N-methyl caprolactam and bromo-n-butane is 1:0.8, and the dripping speed is controlled to slowly drip into the flask, and N 2 , insert a condenser tube, a thermometer, turn on stirring, take out a constant pressure separatory funnel after the dropwise addition and continue to stir and react for 4 hours. After the reaction is completed, pour out the unreacted solution of the upper layer, wash the intermediate with ethyl acetate for several times, rotate it to evaporate, put it in Dry to constant weight in a vacuum drying oven at 70°C to obtain an intermediate with higher purity. Weigh the intermediate in a three-necked flask, add solvent methanol to make a solution, the volume-to-mass ratio of the added methanol and the intermediate is 1 mL / g,...

Embodiment 2

[0045] Weigh 10 g of caprolactam, dissolve it in acetonitrile solvent, put it into a four-necked flask, and the amount of acetonitrile is 50% of the mass of caprolactam. The molar ratio to methyl bromide is 1:2, and the dripping speed is controlled to slowly drip into the flask, and N is fed at the same time. 2 , insert a condenser tube, a thermometer, turn on stirring, take out a constant pressure separatory funnel after the dropwise addition and continue to stir for 12 hours, pour out the unreacted solution of the upper layer after the reaction, wash the intermediate with ethyl acetate several times, rotate it evaporate, put it in Dry to constant weight in a vacuum drying oven at 70°C to obtain an intermediate with higher purity. Weigh the intermediate in a three-necked flask, add solvent methanol to make a solution, the volume-to-mass ratio of the methanol added to the intermediate is 4 mL / g, and then weigh the methanol solution of NaOH, where the volume-to-mass ratio of me...

Embodiment 3

[0047] Weigh 10g of N-ethyl caprolactam, dissolve it in acetonitrile solvent, put it into a four-necked flask, the amount of acetonitrile is 30% of the mass of caprolactam, place it in an oil bath and heat it up to 110 ° C, weigh bromo-n-butane in a constant pressure fraction. In the liquid funnel, the molar ratio of N-ethyl caprolactam and bromo-butane is 1:1, and the dripping speed is controlled to slowly drop into the flask, while feeding N 2 , insert a condenser tube, a thermometer, turn on stirring, take out a constant pressure separatory funnel after the dropwise addition and continue to stir and react for 8 hours, pour out the unreacted solution of the upper layer after the reaction is completed, wash the intermediate with ethyl acetate for several times, rotary evaporation, put in Dry to constant weight in a vacuum drying oven at 70°C to obtain an intermediate with higher purity. Weigh the intermediate in a three-necked flask, add solvent methanol to make a solution, t...

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Abstract

The invention discloses a method for preparing biodiesel by catalyzing waste oil with a caprolactam basic ionic liquid and belongs to the technical field of ionic liquid catalysis. According to the method for preparing the biodiesel by catalyzing waste oil with the caprolactam basic ionic liquid, the waste oil and alkyl alcohol are taken as raw materials, and the caprolactam basic ionic liquid is taken as a catalyst to prepare the biodiesel; and after reaction is finished, the ionic liquid and products are subjected to phase split automatically. The method for preparing the biodiesel by catalyzing waste oil with the caprolactam basic ionic liquid is simple in preparation process and low in cost. The method for preparing the biodiesel by catalyzing waste oil with the caprolactam basic ionic liquid has the advantages that firstly activity of the catalyst is high, and less catalyst is used; secondly, the catalyst is low in toxicity and can be easily biologically degraded; thirdly, reaction conditions are mild, and reaction time is short; and fourthly a reaction process is simple, products are easy to separate, no pollution is produced, and raw material utilization rate is high.

Description

technical field [0001] The invention relates to the technical field of ionic liquid catalysis, in particular to caprolactam ionic liquids. Background technique [0002] Biodiesel refers to a clean alternative fuel for compression ignition engines produced from renewable biological resources such as plants and animal fats. Biodiesel has the advantages of high cetane number, basically free of sulfur and aromatic hydrocarbons, high energy density, good lubricity, good anti-knock, biodegradable, renewable, and high safety. . The preparation process is obtained by reacting raw materials such as vegetable and animal oils with alcohols in the catalytic action of liquid alkali (KOH, NaOH, etc.), but it is necessary to repeatedly wash the liquid alkali in the product. Therefore, the process produces more industrial sewage. [0003] Ionic liquids refer to salt compounds that are liquid at room temperature and consist entirely of ions, also known as "room temperature ionic liquids". ...

Claims

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Application Information

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IPC IPC(8): C07D223/10B01J31/02C11C3/10C11C3/04C10L1/02
CPCY02E50/10
Inventor 李为民左同梅邱玉华任庆功姚超
Owner 南通东湖国际旅行社有限公司
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