Preparation and application of isopropyl diethyl carboxylate

A technology of isopropyl diethyl carboxylate and diethyl malonate, which is applied in the field of preparation of isopropyl diethyl carboxylate, can solve the problems of environmental pollution, large emissions, and long process , to achieve the effects of short reaction time, mild reaction conditions, and simple post-treatment process

Inactive Publication Date: 2009-09-09
JINGGANGSHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional synthesis method of citrate plasticizers is to use citric acid and corresponding alcohols in the presence of sulfuric acid as a catalyst. Currently, the raw material citric acid is mainly prepared by microbial fermentation. This method has a long process, especially for producing A large amount of organic pollutants and solid wastes, these pollutants not only pollute the environment, but also discharge a large amount
Therefore, environmental problems have long been the main factor restricting the development of the citric acid industry, which in turn has affected the widespread promotion and application of citric acid ester plasticizers.

Method used

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  • Preparation and application of isopropyl diethyl carboxylate
  • Preparation and application of isopropyl diethyl carboxylate
  • Preparation and application of isopropyl diethyl carboxylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Add diethyl malonate into ethanol solution with a concentration of 20.0% by mass percentage of sodium ethoxide under stirring, the molar ratio of diethyl malonate to sodium ethoxide is 1:1, heat up to 85°C and react for 30 minutes;

[0029] 2) Add catalyst potassium iodide, the mass ratio of potassium iodide to diethyl malonate is 1:120;

[0030] 3) Add isopropyl bromoacetate dropwise, the molar ratio of isopropyl bromoacetate to diethyl malonate is 1:1, the dropwise addition time is 20 minutes, react at 85°C for 4 hours, and cool down to room temperature;

[0031] 4) adding water to dissolve the separated inorganic salts, separating the oil layer and distilling under reduced pressure to collect products in the boiling point range, while reclaiming unreacted raw materials and solvent ethanol. The yield was 90% based on diethyl malonate.

Embodiment 2

[0033] 1) Add methanol solution with a mass percentage concentration of 19.5% sodium methoxide to diethyl malonate under stirring, the molar ratio of diethyl malonate to sodium methoxide is 1:1.1, heat up to 80°C and react for 20 minutes;

[0034] 2) adding catalyst elemental iodine, the mass ratio of elemental iodine to diethyl malonate is 1:180;

[0035] 3) Add isopropyl chloroacetate dropwise, the molar ratio of isopropyl chloroacetate to diethyl malonate is 1.03:1, the dropwise addition time is 30 minutes, react at 80°C for 10 hours, and cool down to room temperature;

[0036] 4) filter the separated out inorganic salt, distill under reduced pressure, collect the product of boiling point range, reclaim unreacted raw material and solvent methanol simultaneously. The yield was 89% based on diethyl malonate.

Embodiment 3

[0038] 1) Diethyl malonate was added to the ethanol solution with a concentration of 20.0% by mass percentage of sodium ethoxide under stirring, the molar ratio of diethyl malonate to sodium ethoxide was 1:1.05, and the temperature was raised to 75°C for 15 minutes;

[0039] 2) adding catalyst elemental iodine, the mass ratio of elemental iodine to diethyl malonate is 1:200;

[0040] 3) Add isopropyl chloroacetate dropwise, the molar ratio of isopropyl chloroacetate to diethyl malonate is 1.01:1, the dropwise addition time is 30 minutes, react at 75°C for 12 hours, and cool down to room temperature;

[0041] 4) filter the separated out inorganic salt, distill under reduced pressure, collect the product of boiling point range, reclaim unreacted raw material and solvent ethanol simultaneously. The yield was 90% based on diethyl malonate.

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Abstract

The invention discloses a preparation method and application of isopropyl diethyl carboxylate. It uses diethyl malonate and isopropyl chloroacetate or isopropyl bromoacetate as starting materials, and synthesizes DIET through a one-step reaction under the action of a strong base and a catalyst. After the reaction, it is filtered or washed to remove inorganic salts, and then The product was obtained by distillation under reduced pressure. The substance is a colorless or slightly yellowish transparent liquid, and DIET is similar in structure to citrate triester. Through the plasticizing performance comparison experiment between DIET and DOP, it can be found that the plasticizing efficiency of the new structural compound DIET is at the same level as DOP, the compatibility is better than DOP, and the cold resistance is slightly weaker than DOP. These performance test results show that DIET has fully met As a plasticizer, it is a plasticizer with a new structure.

Description

technical field [0001] The invention relates to a preparation method and application of isopropyl diethyl carboxylate. Background technique [0002] With the improvement of environmental protection awareness in various countries in the world, plastic products such as medicine and food packaging, daily necessities, toys, etc. have put forward higher purity and sanitation requirements for the main plasticizer dioctyl phthalate DOP. DOP has a potential carcinogenic risk, and international measures have been taken to limit the scope of use of DOP: the U.S. Environmental Protection Agency has stopped the use of six phthalate plasticizers according to the research results of the National Cancer Institute. Industrial production; the Swiss government has decided to ban the use of DOP in children's toys; Germany has banned the use of DOP in all plastic products related to the human body and hygienic food; in Japan, DOP as a plastic additive is limited to industrial plastic products. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/34C07C67/00C07C67/333C08K5/11
Inventor 隋岩曾锡瑞李新发方小牛
Owner JINGGANGSHAN UNIVERSITY
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