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Application of propane 1, 2, 2, 3 - ethyl ester tetracarboxylic acid as plasticizer, and preparation method thereof

A technology of ethyl tetracarboxylate and diethyl malonate, applied in the field of application and preparation of ethyl propane-1,2,2,3-tetracarboxylate as a plasticizer, can solve the problem of citric acid The development of ester plasticizers, the tight supply of citric acid market, unfavorable recycling and reuse, etc., achieve the effect of simple post-processing, short reaction time and mild reaction conditions

Inactive Publication Date: 2009-04-01
JINGGANGSHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the pollution control measures adopted by most production plants are basically terminal treatment methods, which are not only not conducive to the recovery of useful resources that can be reused, but also require a large investment in equipment and high operating costs, resulting in tight market supply of citric acid, which in turn affects the Development of Citrate Plasticizers
[0004] The application of propane-1,2,2,3-tetracarboxylic acid ethyl ester as a plasticizer has not been reported yet

Method used

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  • Application of propane 1, 2, 2, 3 - ethyl ester tetracarboxylic acid as plasticizer, and preparation method thereof
  • Application of propane 1, 2, 2, 3 - ethyl ester tetracarboxylic acid as plasticizer, and preparation method thereof

Examples

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Embodiment 1

[0029] Embodiment 1, the preparation method of propane-1,2,2,3-tetracarboxylic acid ethyl ester, get diethyl malonate and strong alkali solution to obtain intermediate product A at 70 ℃ of reaction in advance for 10 minutes, then to intermediate product Add in A the catalyst that is 0.5% by weight ratio of diethyl malonate, and dropwise add ethyl halogenated carboxylate in 30 minutes to continue reaction, after dropping ethyl halogenated carboxylate, the temperature is 70 ℃ Under the condition of reaction for 3 hours, remove the inorganic salt impurities after the reaction, and distill under reduced pressure to obtain ethyl propane-1,2,2,3-tetracarboxylate; wherein: the strong alkali solution is sodium methoxide or ethanol with a mass percentage concentration of 18% Ethanol solution of sodium; catalyst is potassium iodide, sodium iodide or elemental iodine; ethyl chloroacetate or ethyl bromoacetate is the catalyst; diethyl malonate: sodium methoxide or sodium ethoxide: ethyl ha...

Embodiment 2

[0030] Embodiment 2, the preparation method of propane-1,2,2,3-tetracarboxylic acid ethyl ester, get diethyl malonate and strong base solution to obtain intermediate product A at 80 ℃ of reaction in advance for 30 minutes, then to intermediate product Add in A the catalyst that is 1% by weight ratio of diethyl malonate, and dropwise add ethyl halogenated carboxylate in 50 minutes to continue reaction, after dropping ethyl halogenated carboxylate, the temperature is 80 DEG C Under the condition of reaction for 15 hours, remove the inorganic salt impurities after the reaction, and distill under reduced pressure to obtain ethyl propane-1,2,2,3-tetracarboxylate; wherein: the strong alkali solution is sodium methoxide or ethanol with a concentration of 21% by mass Ethanol solution of sodium; catalyst is potassium iodide, sodium iodide or elemental iodine; ethyl chloroacetate or ethyl bromoacetate is the catalyst; diethyl malonate: sodium methoxide or sodium ethoxide: ethyl haloaceta...

Embodiment 3

[0031] Embodiment 3, the preparation method of propane-1,2,2,3-tetracarboxylic acid ethyl ester, get diethyl malonate and strong alkali solution and obtain intermediate product A at 75 ℃ of reaction in advance for 20 minutes, then to intermediate product Add the catalyst that is 0.8% by weight ratio of diethyl malonate in A, and dropwise add ethyl halocarboxylate in 40 minutes to continue the reaction, after the dropwise addition of ethyl halocarboxylate, the temperature is 75°C React under the conditions for 10 hours, remove inorganic salt impurities after the reaction, and distill under reduced pressure to obtain ethyl propane-1,2,2,3-tetracarboxylate; wherein: the strong alkali solution is sodium methoxide or ethanol with a mass percentage concentration of 20% Ethanol solution of sodium; catalyst is potassium iodide, sodium iodide or elemental iodine; ethyl chloroacetate or ethyl bromoacetate is the catalyst; diethyl malonate: sodium methoxide or sodium ethoxide: ethyl haloa...

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Abstract

This invention relates to a method for preparing ethyl propane-1, 2, 2, 3-tricarboxylate as a plasticizer. The method comprises: (1) reacting diethyl malonate and strong alkali solution at 70-80 deg.C for 10-30 min to obtain intermediate A; (2) adding catalyst (0.5-1 wt.% of diethyl malonate), dropping halogenated ethyl carboxylate within 30-50 min, and reacting at 70-80 deg.C for 3-15 h; (3) removing inorganic salt impurities, and vacuum-distilling to obtain ethyl propane-1,2,2,3-tricarboxylate. The method has such advantages as simple process, low apparatus investment, mild reaction conditions, short reaction time, no obvious waste discharge (only NaCl or NaBr as byproduct), and simple post-treatment.

Description

technical field [0001] The invention relates to the application of propane-1,2,2,3-tetracarboxylic acid ethyl ester as a plasticizer and the preparation method of propane-1,2,2,3-tetracarboxylic acid ethyl ester. Background technique [0002] Citrate and acetyl citrate are non-toxic "green" environmentally friendly plastic plasticizers recognized in the world, widely used in food and medical equipment packaging, cosmetics, daily necessities, toys, military supplies, etc. It has the advantages of high plastic efficiency, non-toxic, easy to be biodegraded and low volatility, excellent cold resistance, light resistance and water resistance, and has shock resistance in the resin, and does not grow mold. Citrate plasticizers have become an ideal substitute for the current traditional plasticizer phthalates. [0003] The traditional synthetic method of citrate plasticizer is to use citric acid and alcohol to prepare in the presence of sulfuric acid as catalyst (Edited by Song Qih...

Claims

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Application Information

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