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Preparation method of diallylamine and hydrochloride thereof

A technology of diallylamine hydrochloride and diallylamine, which is applied in the field of preparation of diallylamine and its hydrochloride, and can solve the problems of excessive waste generation, large amount of waste water, and increased workload , to achieve the effect of less pollution and low energy consumption

Inactive Publication Date: 2019-02-22
邹平铭兴化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The traditional preparation process of diallylamine and hydrochloride is: lime nitrogen and 3-chloropropene generate cyanamide under the action of catalyst, and cyanamide generates crude diallylamine under the catalysis of concentrated sulfuric acid, and then rectifies to obtain the finished product; Among them, solid waste calcium chloride and sodium sulfate are generated, resulting in more waste and a large amount of waste water, which is difficult to handle. There is also a centrifugal process in the production process, which increases the workload. At the same time, the process yield is low, at 60-65 %about

Method used

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  • Preparation method of diallylamine and hydrochloride thereof
  • Preparation method of diallylamine and hydrochloride thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] 1. Process for preparing diallylamine

[0049] (1) Synthesis section: pump 76.53 g of 3-chloropropene into the drip tank through a feeding pump, put 15% ammonia water into the reaction kettle, add catalyst cuprous chloride, cuprous chloride accounts for the total mass of raw materials 0.5%, the molar ratio of ammonia water to 3-chloropropene is 2.0, turn on the cooling water system to cool down to normal temperature (about 25°C), drop 3-chloropropene (completely added in 1 hour), and slowly heat up to 50- 55°C, raise the temperature by 10°C every 1 hour, control the pressure in the kettle within 0.3MPa, keep the temperature for 1 hour, then cool down to 35-40°C, after the reaction is completed, GC sampling analysis, after passing the test, enter the next section.

[0050](2) Neutralization and distillation section: open the stirring system in the neutralization distillation kettle, add quantitative 32% liquid caustic soda and recovery liquid caustic soda to the neutrali...

Embodiment 2

[0057] 1. Process for preparing diallylamine

[0058] (1) Synthesis section: 153.06 g of 3-chloropropene is pumped into the dripping tank through a feeding pump, the prepared 17% ammonia water is put into the reaction kettle, and the catalyst cuprous chloride is added, and cuprous chloride accounts for the total mass of raw materials 1%, the molar ratio of ammonia water to 3-chloropropene is 2.2:1, turn on the cooling water system to cool down to normal temperature (about 25°C), drop 3-chloropropene (completely added in 1 hour), and slowly heat up to 50-55°C, raise the temperature by 10°C every 1 hour, control the pressure in the kettle within 0.3MPa, keep the temperature for 1 hour, then cool down to 35-40°C, after the reaction is over, GC sampling analysis, after passing the test, enter the next section.

[0059] (2) Neutralization and distillation section: open the stirring system in the neutralization distillation kettle, add quantitative 32% liquid caustic soda and recove...

Embodiment 3

[0066] 1. Process for preparing diallylamine

[0067] (1) Synthesis section: 91.54g of 3-chloropropene is pumped into the dripping tank through a feeding pump, 13% ammonia water prepared is put into the reaction kettle, and the catalyst cuprous chloride is added, and the mass of cuprous chloride accounts for the total amount of raw materials. 1.5% of the mass, the molar ratio of ammonia water to 3-chloropropene is 2.5:1, turn on the cooling water system to cool down to normal temperature (about 25°C), drop 3-chloropropene (completely added in 1 hour), and slowly heat up To 50-55°C, raise the temperature by 10°C every 1 hour, control the pressure in the kettle within 0.3MPa, keep it warm for 1 hour, then lower the temperature to 35-40°C, after the reaction is completed, GC sampling analysis, after passing the test, enter the next section.

[0068] (2) Neutralization and distillation section: open the stirring system in the neutralization distillation kettle, add quantitative 32...

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Abstract

The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of diallylamine and hydrochloride thereof. The preparation method comprises the following steps: inputting ammonia water into a reaction kettle, adding a catalyst, dropwise adding 3-chloropropene at a constant temperature and a constant pressure, heating the mixture to 50-55 DEG C after dropwise addition, keeping the temperature for 1 hour, and reducing the temperature to 35-40 DEG C to obtain slurry; extracting the slurry to a distilling kettle, adding sodium hydroxide and a byproduct ammonium chloride into the distilling kettle to react, absorbing generated ammonia water with water and reusing the same, neutralizing the same, starting distillation till a water phase is obtained, adding caustic soda flakes to dehydrate, cyclically using the dehydrated alkaline liquor t o obtain a diallylamine coarse product; and inputting the coarse product into a rectifying kettle, taking a small amount of precomponent first, then receiving diallylamine, and returning the precomponent to a reaction kettle to be used. The diallylamine and hydrochloride thereof are prepared by adopting an amination process, so that the method is safe and is guaranteed, and meanwhile, excessive ammonia water and alkaline water are fully recycled, so that the preparation method is low in energy consumption and little in pollution, and the three wastes can be recycled.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of diallylamine and its hydrochloride. Background technique [0002] Diallylamine is a high-grade organic amine, colorless and transparent liquid, flammable, melting point: -88.4°C; lightning: 7°C; boiling point: 111-112°C; solubility: 5-6; refractive index (20°C) 1.440; CAS No.: 124-02-7; EINECS No.: 204-671-2; Chemical Structural Formula: NH(CH 2 -CH=CH 2 ) 2 ; Molecular formula: C 6 h 11 N; molecular weight: 97.16; its hydrochloride structural formula: NH(CH 2 -CH=CH 2 ) 2 • HCl. [0003] Diallylamine is mainly used in the following two aspects: (1) As raw material for organic synthesis, ionic water purifier, polymer monomer, pharmaceutical intermediate, etc.; (2) Organic intermediate. Diallylamine hydrochloride is mainly used to make cross-linking formaldehyde-free color fixing agent, cross-linking agent, amphoteric polymer,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/08C07C209/00C07C211/21
CPCC07C209/08C07C209/00C07C211/21
Inventor 陈强张鹏许小波王涛孙凡通杜晓阳张俊玲
Owner 邹平铭兴化工有限公司
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