Method for synthesizing diethyleneglycol diformate by composite catalyst

A technology for compounding catalysts and diformate esters, which is applied in the fields of organic chemistry, reaction preparation of ester groups and hydroxyl groups, etc., can solve the problems of increased purification difficulty of by-products, unfavorable industrial production, equipment corrosion environment, etc. The effect of industrialized continuous production, mature production technology and no environmental pollution

Inactive Publication Date: 2017-01-25
SHENZHEN PRECHEM FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The esterification yield of this reaction is 55% to 61%, the reaction time is long, the raw material price is high, and the toxicity is high, which is not conducive to industrial production
The direct esterification of diethylene glycol and formic acid is a method commonly used in industry at present. It uses toluene, cyclohexane, and benzene as dehydrating agents, and uses Lewis acid catalysts such as zinc chloride, ferric chloride, and p-toluenesulfonic acid as catalysts. , the disadvantage of this method is that it produces acid-containing wastewater, which seriously corrodes equipment and pollutes the environment, and under acidic catalysts and high temperatures (temperatures greater than 130 ° C), diethylene glycol and diethylene glycol monocarboxylate are prone to dehydration reactions, resulting in by-products. The product increases the difficulty of purification

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The method for the synthesis of diethylene glycol dicarboxylate using common catalysts of the present embodiment comprises the following steps: potassium carbonate, diethylene glycol and sec-butyl formate are added to the rectifying tower and After heating the distillation pot of the agitator until the temperature at the top of the tower is stable, extract the azeotrope of sec-butanol and sec-butyl formate with a reflux ratio of 6:1, and add the remaining sec-butyl formate in 3 times; sec-butyl formate The total addition is 3.5 times (mol ratio) of diethylene glycol, in the feed process of sec-butyl formate, the tower still temperature is kept 110-130 ℃, and the adding speed of sec-butyl formate is controlled by tower still temperature, The feeding time lasts for 3 hours, and the feeding is completed in three times. At the same time, the temperature at the top of the rectification tower is adjusted to 100-120°C, so that the azeotrope of sec-butanol and sec-butyl formate ...

Embodiment 2

[0029]The method for the synthesis of diethylene glycol dicarboxylate using common catalysts in this embodiment comprises the following steps: adding sodium ethylate, sec-butanol and sec-butyl formate to a rectifying tower with stirring according to a molar ratio of 0.02:1:0.65 After heating the distillation tank of the device until the temperature at the top of the tower is stable, extract the azeotrope of sec-butanol and sec-butyl formate with a reflux ratio of 7:1, and add the remaining sec-butyl formate in 3 times. The total amount of sec-butyl formate added is 4.5 times (molar ratio) of diethylene glycol. During the feeding process of sec-butyl formate, the temperature of the tower still is maintained at 110-130°C, and the addition speed of sec-butyl formate passes through the tower still. The temperature was controlled, and the addition time lasted 3 hours. After the feeding is completed, continue to react and extract the azeotrope of sec-butanol and sec-butyl formate un...

Embodiment 3

[0031] The method for synthesizing diethylene glycol dicarboxylate using a compound catalyst in this example is as follows: the compound catalyst (the ratio of tetraisobutyl titanate to triisobutoxyaluminum is 1:10), two Glycol and sec-butyl formate are added to the distillation still with a rectification tower and agitator according to the molar ratio of 0.003:1:1.0, and after the temperature at the top of the tower is stable, sec-butanol and sec-butyl formate are extracted at a reflux ratio of 8:1 Azeotrope of ester, while continuously adding the remaining sec-butyl formate. The total amount of sec-butyl formate added is 4.5 times (molar ratio) of diethylene glycol. During the feeding process of sec-butyl formate, the temperature of the tower still is maintained at 120-140 °C, and the addition speed of sec-butyl formate passes through the tower still. The temperature was controlled, and the addition time lasted 3 hours. After the feeding is completed, continue to react and ...

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Abstract

The invention relates to a method for synthesizing diethyleneglycol diformate by a composite catalyst. The synthesis method is characterized in that butyl chloroformate and ethylene glycol are taken as raw materials, diethyleneglycol diformate is generated through ester exchange under the action of a compositecatalyst, and a by-product is diglycol monoformate, and thus the synthesis method solves a problem that a conventional catalyst is difficult to react and has low yield. The mass fraction yield of diethyleneglycol diformate is above 90%; diethyleneglycol diformate is mild in reaction condition and high in yield, has no corrosion and environmental pollution, and is easy to separate and purify the product; the separation and purification process is simple and low in energy consumption; in a reaction process, raw materials can be reused,so that a production cost is saved; besides, with mature production technologies and abundance and cheap price of raw material resources, the synthesis method is convenient to achieve extensive industrialization production in the future.

Description

technical field [0001] The invention belongs to the field of organic compound synthesis, and in particular relates to a method for synthesizing diethylene glycol dicarboxylate by using a composite catalyst. Background technique [0002] Diethylene glycol dicarboxylate, also known as diethylene glycol dimethyl ester, is a colorless liquid with a boiling point of 230.2 °C. It is an efficient, safe, non-toxic and environmentally friendly organic solvent. Widely used in the pharmaceutical industry; organic ester curing agent for casting resins; also used as an excellent solvent for various organic resins, especially nitrocellulose, and raw materials for leather brighteners; used as nitro spray paint, printing ink, cellulose ester in paints and coatings , Fluorescent paint solvent. [0003] The traditional methods for the synthesis of diethylene glycol dicarboxylate include formate esterification, diethylene glycol and formic acid direct esterification. The formate esterificati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/03C07C69/08
CPCC07C67/03C07C69/08
Inventor 罗鑫鹏张春雨
Owner SHENZHEN PRECHEM FINE CHEM CO LTD
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