Preparation method of morpholine

A technology of morpholine and equation, applied in the field of preparation of morpholine, can solve problems such as many by-products and low yield, and achieve the effects of reducing usage amount, improving separation efficiency and being beneficial to industrial application

Inactive Publication Date: 2017-03-08
王显权
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention intends to provide a process for preparing morpholine by using the diethanolamine method, which has solved the problem of many by-products and low yield due to the influence of the catalyst in the production of morpholine by the diethylene glycol method in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Preparation method of morpholine, the specific steps are:

[0018] Step 1. Dehydration: Add concentrated sulfuric acid to the dehydration tank, add diethanolamine liquid dropwise with stirring, the feed ratio of concentrated sulfuric acid and diethanolamine liquid is 1.8:1, the temperature rises after the reaction, and the temperature is controlled within the range of 190℃ , The reaction time is 80min, after dripping, the easy water cooling in the dehydration tank will be cooled to 60℃;

[0019] Step 2: Neutralization: Add 20% sodium hydroxide solution to the dehydration tank until the pH is 8-9 to obtain a neutralization solution;

[0020] Step 3. Vacuum steaming: Put the neutralized liquid in a horizontal distillation kettle. A horizontal stirring paddle is set in the kettle. The sodium sulfate at the bottom of the kettle is stirred by the horizontal stirring paddle, and the morpholine is evaporated in a vacuum. The vacuum degree is -0.05 MPa~-0.2MPa;

[0021] Ste...

Embodiment 2

[0022] Example 2: Preparation method of morpholine, the specific steps are:

[0023] Step 1. Dehydration: Add concentrated sulfuric acid to the dehydration tank, add diethanolamine solution dropwise with stirring, the feed ratio of concentrated sulfuric acid and diethanolamine solution is 1.85:1, the temperature rises after the reaction, and the temperature is controlled within 200℃ , The reaction time is 85min, after dripping, the easy water cooling in the dehydration tank is cooled to 60℃;

[0024] Step 2: Neutralization: Add 20% sodium hydroxide solution to the dehydration tank until the pH is 8-9 to obtain a neutralization solution;

[0025] Step 3. Vacuum steaming: Put the neutralized liquid in a horizontal distillation kettle. A horizontal stirring paddle is set in the kettle. The sodium sulfate at the bottom of the kettle is stirred by the horizontal stirring paddle, and the morpholine is evaporated in a vacuum. The vacuum degree is -0.05 MPa~-0.2MPa;

[0026] Step 4. Treatmen...

Embodiment 3

[0027] Example 3: Preparation method of morpholine, the specific steps are:

[0028] Step 1. Dehydration: Add concentrated sulfuric acid to the dehydration tank, add diethanolamine solution dropwise under stirring, the feed ratio of concentrated sulfuric acid and diethanolamine solution is 1.9:1, the temperature rises after the reaction, and the temperature is controlled within the range of 210℃ , The reaction time is 90min, after dripping, the temperature of the easy water cooling in the dehydration tank is cooled to 60℃;

[0029] Step 2: Neutralization: Add 20% sodium hydroxide solution to the dehydration tank until the pH is 8-9 to obtain a neutralization solution;

[0030] Step 3. Vacuum steaming: Put the neutralized liquid in a horizontal distillation kettle. A horizontal stirring paddle is set in the kettle. The sodium sulfate at the bottom of the kettle is stirred by the horizontal stirring paddle, and the morpholine is evaporated in a vacuum. The vacuum degree is -0.05 MPa~-...

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Abstract

The invention discloses a preparation method of morpholine in the technical field of chemical synthesis. A chemical reaction equation is shown as follows. The preparation method particularly includes steps: dewatering: adding concentrated sulfuric acid into a dewatering tank, stirring while dropwise adding diethanolamine liquid, increasing temperature after reaction, controlling the temperature within a range of 190-210 DEG C and reaction time to 80-100min, and water-cooling to 60 DEG C after dropwise adding is finished, wherein a feeding ratio of the concentrated sulfuric acid to the diethanolamine liquid is 1.8:1-1.9:1; neutralizing: dropwise adding 20% sodium hydroxide solution into the dewatering tank to obtain neutralizing liquid; putting the neutralizing liquid in a horizontal distillation kettle, stirring sodium sulfate at the bottom of the distillation kettle, and vacuum-evaporating out morpholine; scraping out sodium sulfate in the distillation kettle by stirring, collecting for recycling, and putting filtrate and kettle washing water into a recycling tank for treatment. By the preparation method, raw materials can be saved to greatest extent (consumption of the diethanolamine liquid is reduced), the process is simple, and wastewater is washing filtration water only and can be recycled, so that influence on environment is avoided; the preparation method is higher than 85% in yield, thereby being more convenient for industrial application.

Description

Technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of morpholine. Background technique [0002] Morpholine, molecular formula C 4 H 9 NO, or written as O(CH 2 CH 2 ) 2NH. Also known as morphine, it is a colorless oily liquid at room temperature. Melting point -4.76℃, boiling point 128.3℃. The density is 1.0005g / cm3 (20°C). The refractive index is 1.4548. The flash point is 38°C (open cup). Miscible with water, acetone, benzene, ether, alcohol, glycol, linseed oil, turpentine, castor oil. It is hygroscopic and smells of ammonia. It can be prepared by diethanolamine by sulfuric acid dehydration and cyclization. Industrially, it is mainly produced by diethylene glycol and ammonia in the presence of hydrogen conditions and catalysts. Mainly used in the production of rubber vulcanization accelerators, and also in the synthesis of surfactants, textile printing and dyeing auxiliaries, medicines and pes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/027C07D295/023
CPCC07D295/023C07D295/027
Inventor 王显权
Owner 王显权
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