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The preparation method of recyclable n-butyldiethanolamine

A technology of butyldiethanolamine and butylethanolamine, which is applied in the preparation of organic compounds, the preparation of aminohydroxyl compounds, chemical instruments and methods, etc., can solve the problems of high reaction temperature, increase of three wastes, large salty wastewater, etc., and achieve reaction Moderate conditions, low cost, environmental protection, and good safety

Active Publication Date: 2021-10-12
ZHEJIANG HISUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current preparation method is time-consuming and labor-intensive, the three wastes are high, the cost is high, and it is often not easy to obtain high-purity products
In the prior art, N-butyldiethanolamine is mainly prepared by reacting chlorobutane or bromobutane with diethanolamine. This process will produce a large amount of saline wastewater, and the cost is high, which is not conducive to industrial production.
[0003] Japanese patent JP2011178664A discloses a synthesis method of N-tert-butyldiethanolamine, which requires extremely high reaction temperature, which will lead to excessive pressure and affect the feeding of ethylene oxide, making it difficult to realize industrial mass production
[0004] Chinese patent CN103373930A discloses a synthetic method of N-tert-butyldiethanolamine, which adopts feeding under negative pressure in the reactor and selectively adds catalyst to accelerate the reaction process, but the catalyst zinc chloride, aluminum chloride and lithium chloride etc. will chemically react with n-butylamine to form corresponding ammonia salts, which will affect the purity of the product; and this type of catalyst will corrode the equipment, and it is difficult to separate and recycle, which will increase the production cost, and at the same time increase the three wastes, causing environmental pollution
When the molar ratio of ethylene oxide to n-butylamine is greater than 2:1, unexpected side reactions will occur, the product impurities will increase, and the quality and yield will decrease

Method used

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  • The preparation method of recyclable n-butyldiethanolamine
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  • The preparation method of recyclable n-butyldiethanolamine

Examples

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Effect test

Embodiment 1

[0024] The preparation of embodiment 1 N-butyldiethanolamine

[0025] Batch 01: After the reactor was evacuated twice for nitrogen replacement, 73.1kg of n-butylamine was pumped into the reactor under normal pressure, and then vacuumed again for nitrogen replacement. Then slowly raise the temperature in the reactor to 130°C, press 88.1kg of ethylene oxide into the reactor, control the flow rate at 6kg / min, keep the pressure of the reactor at 0-0.6MPa, and keep the reaction temperature at 130-135°C; After the feeding of ethylene oxide was completed, the heat was kept for 1 hour to obtain the crude product of N-butyldiethanolamine. The crude product of N-butyldiethanolamine is degassed and then transferred to the rectification tank. The temperature of the rectification tank is controlled at 120-140°C, the vacuum degree is 3-6mmHg, and the temperature at the top of the tank is 75-80°C. Ethanolamine 7.0kg. Control the rectification kettle temperature at 140-170°C, vacuum degree ...

Embodiment 2

[0032] Embodiment 2: the preparation of N-butyldiethanolamine

[0033]Batch 01: After the reactor was evacuated twice for nitrogen replacement, 73.1kg of n-butylamine was pumped into the reactor under normal pressure, and then vacuumed again for nitrogen replacement. Then slowly raise the temperature in the reactor to 130°C, press 79.2kg of ethylene oxide into the reactor, control the flow rate at 6kg / min, keep the pressure of the reactor at 0-0.6MPa, and keep the reaction temperature at 130-135°C; After the feeding of ethylene oxide was completed, the heat was kept for 1 hour to obtain the crude product of N-butyldiethanolamine. The crude product of N-butyldiethanolamine is degassed and then transferred to the rectification tank. The temperature of the rectification tank is controlled at 120-140°C, the vacuum degree is 3-6mmHg, and the temperature at the top of the tank is 75-80°C. Ethanolamine 15.2kg. Control the rectification kettle temperature to 140-170°C, vacuum degree...

Embodiment 3

[0040] Embodiment 3: the preparation of N-butyldiethanolamine

[0041] Batch 01: After the reactor was evacuated twice for nitrogen replacement, 65.8kg of n-butylamine was pumped into the reactor under normal pressure, and then evacuated for nitrogen replacement again after pumping. Then slowly raise the temperature in the reactor to 130°C, press 79.2kg of ethylene oxide into the reactor, control the flow rate at 6kg / min, keep the pressure of the reactor at 0-0.6MPa, and keep the reaction temperature at 165-170°C; After the feeding of ethylene oxide was completed, the heat was kept for 1 hour to obtain the crude product of N-butyldiethanolamine. The crude product of N-butyldiethanolamine is degassed and then transferred to the rectification tank. The temperature of the rectification tank is controlled at 120-140°C, the vacuum degree is 3-6mmHg, and the temperature at the top of the tank is 75-80°C. Ethanolamine 8.1kg. Control the rectification kettle temperature at 140-170°C...

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Abstract

The present invention relates to a method for the preparation of high-yield N-butyldiethanolamine which can be recycled and applied mechanically. It is different from the existing route for synthesizing N-butyldiethanolamine. It uses n-butylamine and ethylene oxide as reaction raw materials, especially The most important thing is to recycle the by-product N-butylethanolamine produced in the synthesis process and use it as a reaction raw material to prepare the final product N-butyldiethanolamine, which greatly reduces the cost and is environmentally friendly, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for preparing high-yield N-butyldiethanolamine by recyclable intermediate product N-butylethanolamine. Background technique [0002] As a chemical material intermediate, butyldiethanolamine is widely used in plastic products, coatings, synthetic fibers, adhesives and other fields. The current preparation method is time-consuming and labor-intensive, the three wastes are high, the cost is high, and it is often not easy to obtain high-purity products. In the prior art, N-butyldiethanolamine is mainly produced by reacting chlorobutane or bromobutane with diethanolamine. This process will generate a large amount of saline wastewater, and the cost is high, which is not conducive to industrial production. [0003] Japanese patent JP2011178664A discloses a synthesis method of N-tert-butyldiethanolamine. This method requires extremely high reaction temperature, which will lead ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/04C07C213/10C07C215/12
CPCC07C213/04C07C213/10C07C215/12
Inventor 包如胜蒋富国戴咸本唐子英肖静辉
Owner ZHEJIANG HISUN CHEM