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Method of using macroporous strongly acidic type cation exchange resin to catalytically synthesize ethyl palmitate

A technology of strong acidic cations and ethyl palmitate, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., to achieve the effects of mild reaction conditions, reduced production costs, and high yields

Inactive Publication Date: 2012-08-01
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no relevant report on its use in the synthesis of ethyl palmitate

Method used

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  • Method of using macroporous strongly acidic type cation exchange resin to catalytically synthesize ethyl palmitate
  • Method of using macroporous strongly acidic type cation exchange resin to catalytically synthesize ethyl palmitate

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Example 1 : In a 100 ml round bottom flask, add 10.26 g (40 mmol) palmitic acid, 3.50 ml (60 mmol) absolute ethanol, 2.17 ml (20 mmol) cyclohexane, 5.13 g NKC-9 macroporous dry hydrogen catalytic resin , heated to reflux at 65°C under agitation, and water was continuously released from the water separator; the reaction was stopped when no more water was separated; the reaction solution was filtered to separate the resin, and the resin was washed with cyclohexane (10 ml for 2 times), separate and recover the resin, the washing liquid and the filtrate are combined to be separated; the reaction liquid is distilled at 80°C~90°C under normal pressure, and excess ethanol and cyclohexane are distilled off (ethanol and cyclohexane can be further recycled and reused), The resulting reaction solution was then distilled under reduced pressure at 65°C-67°C and a pressure of 1.33 kPa-1.35 kPa to collect fractions with a yield of 92%; the fractions were identified as ethyl palmitate...

Embodiment 2

[0019] Example 2 : In a 100 ml round bottom flask, add 10.26 g (40 mmol) palmitic acid, 4.67 ml (80 mmol) absolute ethanol, 2.17 ml (20 mmol) cyclohexane, 5.13 g NKC-9 macroporous dry hydrogen catalytic resin , heated to reflux at 70°C under agitation, and the water separator continuously released water, and stopped the reaction when no more water was separated; the reaction solution was filtered to separate the resin, and the resin was washed with cyclohexane (10 ml for 2 times), separate and recover the resin, the washing liquid and the filtrate are combined to be separated; the reaction liquid is distilled at 80°C~90°C under normal pressure, and excess ethanol and cyclohexane are distilled off (ethanol and cyclohexane can be further recycled and reused), The resulting reaction solution was then distilled under reduced pressure at 65°C-67°C and a pressure of 1.33 kPa-1.35 kPa to collect fractions with a yield of 95%; after drying, the fractions were identified as ethyl palm...

Embodiment 3

[0020] Example 3 : In a 250 ml round bottom flask, add 25.64 g (100 mmol) palmitic acid, 14.58 ml (250 mmol) absolute ethanol, 6.52 ml (60 mmol) cyclohexane, 12.82 g NKC-9 macroporous dry hydrogen catalytic resin , heated to reflux at 75°C under agitation, the water separator continued to leak water, and stopped the reaction when no more water was separated; the reaction solution was filtered to separate the resin, and the resin was washed with cyclohexane (20 ml for 2 times), separate and recover the resin, the washing liquid and the filtrate are combined to be separated; the reaction liquid is distilled at 80°C~90°C under normal pressure, and excess ethanol and cyclohexane are distilled off (ethanol and cyclohexane can be further recycled and reused), The resulting reaction solution was then distilled under reduced pressure at 73°C~75°C under a pressure of 2.00 kPa~2.05 kPa to collect fractions with a yield of 90%; after drying, the fractions were identified as ethyl palmit...

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Abstract

The invention discloses an ethyl palmitate preparation method, which belongs to the field of organic chemical industrial synthesis. The method includes: using strongly acidic type cation exchange resin which is NKC-9 macroporous dry hydrogen catalyst resin as catalyst, using cyclohexane as a water carrying agent, and reacting palmitic acid with excessive absolute ethyl alcohol; subjecting the solution containing resin after reaction to filtering, cyclohexane washing and separating to recover the catalyst, removing redundant ethanol and cyclohexane through atmospheric distillation, and obtaining ethyl palmitate after reduced pressure distillation and drying. The ethyl palmitate preparation method is mild in reaction condition, the catalyst is noncorrosive to equipment, waste acid discharge is avoided, and accordingly pollution is avoided while environment friendliness is achieved. The strongly acidic type cation exchange resin is high in catalytic activity and recyclable after recovery and activation, so that catalyst production cost is reduced. Moreover, the ethyl palmitate preparation method is simple in synthesis process and high in yield and meets the green synthesis process requirements.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and relates to a method for preparing organic chemical raw material ethyl palmitate, in particular to a method for catalytically synthesizing ethyl palmitate by using a macroporous strongly acidic cation exchange resin. Background technique [0002] Ethyl palmitate is a colorless needle-shaped crystal obtained by esterification of palmitic acid and absolute ethanol. It can be used as a softener and lubricant, and is also an important raw material for the synthesis of sucrose esters and sucrose polyesters. In addition, ethyl palmitate can also be used as a plant acaricide for the control of economic crops such as fruit trees and vegetables (application number: CN200910180615.6; publication number: CN101692811A) and a pine wood nematode control agent (application number: CN201010198691.2; Publication number: CN101849539A). At present, the synthesis of higher fatty acid esters basically us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/24C07C67/08
CPCY02P20/584
Inventor 孔维宝来宝鹏唐东杰张娟景洋张继
Owner NORTHWEST NORMAL UNIVERSITY
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