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Method for synthesizing ethyl palmitate by using deep eutectic solvent catalyst based on dodecyltrimethylammonium chloride

A technology of dodecyl trimethyl ammonium chloride and low eutectic solvent, applied in the field of organic chemical industry synthesis, can solve the problems of excessive catalyst consumption, large production energy consumption, low equipment utilization rate, etc., and achieves equipment corrosion. Small, mild reaction conditions, and the effect of reducing production costs

Pending Publication Date: 2020-05-15
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the method proposed in this patent, the amount of catalyst used is 50% to 70% of the mass of palmitic acid used, and the amount of catalyst used is too large, resulting in low utilization rate of equipment in industrial production and high production energy consumption.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 51.28 g (0.2 mol) of palmitic acid and 13.82 g (0.3 mol) of ethanol in a three-necked flask, stir and heat to 65°C, then weigh 2.60 g of catalyst DTAC-DES into the three-necked flask and carry out at this temperature For the reaction, the rotation speed was 600 rpm, and the reaction time was 4 h; after the reaction was completed, the reaction solution was separated into water and oil phases through a separatory funnel while it was hot, and the catalyst was recovered by vacuum drying the water phase at 60 °C. The oil phase is subjected to atmospheric distillation (temperature 85°C~95°C) to remove excess ethanol, and then vacuum distillation (temperature 150°C~155°C, pressure 235 Pa~265 Pa) to obtain fractions, which are anhydrous chlorinated The calcium was dried and identified as ethyl palmitate by GC-MS with a yield of 86.50%.

Embodiment 2

[0018] Weigh 51.28 g (0.2 mol) of palmitic acid and 18.42 g (0.4 mol) of ethanol in a three-necked flask, stir and heat to 75°C, then weigh 1.40 g of catalyst DTAC-DES into the three-necked flask and carry out at this temperature For the reaction, the rotation speed was 600 rpm, and the reaction time was 2.5 h. After the reaction was completed, the reaction solution was separated into water and oil phases through a separatory funnel while it was hot, and the catalyst was recovered by vacuum drying the water phase at 60 °C. The oil phase is subjected to atmospheric distillation (temperature 85°C~95°C) to remove excess ethanol, and then vacuum distillation (temperature 155°C~160°C, pressure 265 Pa~300 Pa) to obtain fractions, which are anhydrous chlorinated The calcium was dried and identified as ethyl palmitate by GC-MS with a yield of 87.65%.

Embodiment 3

[0020] Weigh 51.28 g (0.2 mol) of palmitic acid and 27.64 g (0.6 mol) of ethanol in a three-necked flask, stir and heat to 55°C, then weigh 3.16 g of catalyst DTAC-DES into the three-necked flask and carry out at this temperature For the reaction, the rotation speed was 600 rpm, and the reaction time was 4 h; after the reaction was completed, the reaction solution was separated into water and oil phases through a separatory funnel while it was hot, and the catalyst was recovered by vacuum drying the water phase at 60 °C. The oil phase is subjected to atmospheric distillation (temperature 85°C~95°C) to remove excess ethanol, and then vacuum distillation (temperature 145°C~150°C, pressure 200 Pa~235 Pa) to obtain fractions, which are anhydrous chlorinated Calcium was dried and identified as ethyl palmitate by GC-MS with a yield of 89.82%.

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Abstract

The invention discloses a method for preparing ethyl palmitate by using a deep eutectic solvent DTAC-DES based on dodecyltrimethylammonium chloride as a catalyst. The catalyst DTAC-DES is prepared bymixing dodecyltrimethylammonium chloride and p-toluenesulfonic acid according to a molar ratio of 1:3; and the ethyl palmitate is prepared by performing an esterification reaction on palmitic acid andexcessive anhydrous ethanol at a certain temperature, and sequentially performing phase separation, atmospheric distillation, reduced pressure distillation and other processes. The method has the advantages of mild reaction conditions, small corrosion of the catalyst to equipment, no waste acid discharge, no pollution and environmental friendliness; and the acidic eutectic solvent is high in catalytic activity, can be repeatedly used after being recycled, and is low in industrial production cost.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and relates to a method for preparing biodiesel ethyl palmitate, in particular to a method for synthesizing ethyl palmitate based on a dodecyltrimethylammonium chloride deep eutectic solvent catalyst. Background technique [0002] Biodiesel is a new type of renewable green energy. It has high flash point, good anti-knock performance, excellent combustion performance, and can effectively reduce SO x , NO x and other harmful greenhouse gas emissions. Biodiesel is a kind of high-grade fatty acid ester compound, which can be prepared by transesterification or esterification reaction of animal and vegetable fats and waste cooking oil with lower alcohols. In the traditional preparation process, concentrated sulfuric acid is often used as a catalyst. Although concentrated sulfuric acid has high catalytic activity when catalyzed, it is prone to side reactions, difficult to purify products, se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/24B01J31/02
CPCC07C67/08B01J31/0225B01J31/0229B01J2231/49C07C69/24
Inventor 曾作祥江珊周志远薛为岚张传炜张思琪
Owner EAST CHINA UNIV OF SCI & TECH
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