Preparation method of hydroxypropyl diethylenediamine

A technology of hydroxypropyl diethylene diamine and epichlorohydrin, applied in the field of preparation of hydroxypropyl diethylene diamine, can solve the problems of low product yield, complicated process and the like

Inactive Publication Date: 2018-11-02
安庆精益精化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods require high temperature to realize, the pr

Method used

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  • Preparation method of hydroxypropyl diethylenediamine
  • Preparation method of hydroxypropyl diethylenediamine

Examples

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Synthetic example

[0018] The following synthesis examples serve as reference for the preparation method of hydroxypropyldiethylenediamine of the present invention, but the present invention is not limited to the following examples. The chemical reagents used in the following synthesis examples are commercially available analytically pure chemical reagents.

Synthetic example 1

[0020] In the 500 milliliters of four-neck round bottom flasks equipped with stirrer, thermometer and reflux condenser, add respectively the benzyltriethylammonium chloride of 1% of 86 gram piperazine, 200 gram water, reactant weight, be warming up to At 45°C, start to slowly add 95 grams of epichlorohydrin dropwise, and control the temperature below 85°C during the dropwise addition to prevent the temperature from rising sharply. After the dropwise addition, the temperature was raised to reflux, and the reaction was carried out at reflux for 3 hours. After cooling to room temperature, 146 g of 30% sodium hydroxide was added dropwise. After the dropwise addition, the temperature was raised to reflux, and the reaction was carried out at reflux for 8 hours. Then all the water was evaporated, cooled, and then 200 ml of methanol was added, fully stirred, the by-product sodium chloride was filtered out, and the filter cake was washed with methanol. The filtrates were combined, con...

Synthetic example 2

[0022] In the 500 milliliters of four-neck round bottom flasks equipped with stirrer, thermometer and reflux condenser, add respectively the benzyltriethylammonium chloride of 1% of 86 gram piperazine, 200 gram water, reactant weight, be warming up to At 45°C, start to slowly add 95 grams of epichlorohydrin dropwise, and control the temperature below 85°C during the dropwise addition to prevent the temperature from rising sharply. After the dropwise addition, the temperature was raised to reflux, and the reaction was carried out at reflux for 3 hours. After cooling to room temperature, 122 g of triethylamine was added dropwise. After the dropwise addition, the temperature was raised to reflux, and the reaction was carried out at reflux for 6 hours. Then all the water is evaporated, cooled, and then 200 ml of methanol are added, fully stirred, the by-product triethylamine hydrochloride is filtered out, and the filter cake is washed with methanol. The filtrates were combined, c...

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Abstract

The invention relates to a preparation method of hydroxypropyl diethylenediamine taking piperazine and epoxy chloropropane as raw materials. (The formal is shown in the description.).

Description

technical field [0001] The invention relates to a preparation method of hydroxypropyl divethylenediamine. Background technique [0002] Hydroxypropyldiethylenediamine can be used in pharmaceutical and pesticide intermediates, organic synthesis catalysts, polyurethane catalysts and other fields. [0003] In the manufacture of polyurethane resin or polyurethane products (foam), the traditional catalysts are tertiary amine compounds. Due to the volatility of tertiary amine compounds, a strong odor is produced, which leads to the deterioration of the operating environment during the manufacture of polyurethane resin or polyurethane products (foam). . When polyurethane products are used as decorative materials, the tertiary amine catalyst will be slowly eliminated in the form of volatile components, which will cause odor and discolor the surface of the material. Therefore, the development of catalysts that do not produce volatile matter is very important for environmental prote...

Claims

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Application Information

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IPC IPC(8): C07D487/08
CPCC07D487/08
Inventor 罗长青
Owner 安庆精益精化工有限公司
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