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Preparation method of 2, 2, 6, 6-tetramethyl-4-aminopiperidine

A technology of tetramethylpiperidone and aminopiperidine is applied in chemical instruments and methods, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, etc. Adverse effects and high production costs, achieving the effect of more application times, low price and less usage

Active Publication Date: 2020-09-22
江苏富比亚化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] And the method for preparing 2,2,6,6,-tetramethylpiperidinamine reported by domestic chemical companies mostly adopts the means of adding alkali to adjust pH, although it may have the effect of reducing the production of tetramethyl alcohol and increasing the concentration of tetramethylpiperidinium. The advantage of the selectivity of pyridine amine, but due to the adverse effect on the catalyst, the post-treatment and recovery, the difficulty of activating the catalyst is increased, and there is also the problem of high production cost

Method used

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  • Preparation method of 2, 2, 6, 6-tetramethyl-4-aminopiperidine
  • Preparation method of 2, 2, 6, 6-tetramethyl-4-aminopiperidine
  • Preparation method of 2, 2, 6, 6-tetramethyl-4-aminopiperidine

Examples

Experimental program
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Effect test

Embodiment 1

[0056] 329g mass concentration is 30% ammonia water, 3g supported nickel catalyst is added in the hydrogenation tank;

[0057] Add 200g of 2,2,6,6-tetramethylpiperidone into the hydrogenation kettle, and heat up after nitrogen replacement. When the temperature of the hydrogenation kettle rises to 120°C, the hydrogen gas will start the reaction, and the pressure in the hydrogenation kettle will be maintained at 2.0Mpa, the temperature is 120°C until the end of the reaction;

[0058] The GC content of the target product 2,2,6,6-tetramethyl-4-aminopiperidine is 96.54%, and the by-product piperidinol content is 2.06% (see attached figure 1 ).

[0059] Lower the temperature until it falls below 90°C, preferably below 80°C;

[0060] After settling, the reaction system is divided into upper and lower layers, and the catalyst is recovered from the lower layer for mechanical application;

[0061] Filter the supernatant liquid, then rectify, deammoniaize at normal pressure first, rec...

Embodiment 2

[0064] Add 329g30% ammonia water and 2.5g loaded nickel catalyst into the hydrogenation tank

[0065] Add 200g of 2,2,6,6-tetramethylpiperidone into the hydrogenation kettle, heat up after replacement, and when the temperature of the hydrogenation kettle rises to 120°C, the hydrogen gas will start to react, and the pressure in the hydrogenation kettle will be maintained at 2.5 Mpa, temperature is 120 ℃, until reaction finishes;

[0066] The GC content of the target product 2,2,6,6-tetramethyl-4-aminopiperidine is 95.95%, and the by-product piperidinol content is 1.99% ((as attached image 3 shown).

[0067] Lower the temperature until it falls below 90°C, preferably below 80°C;

[0068] After settling, the reaction system is divided into upper and lower layers, and the catalyst is recovered from the lower layer for mechanical application;

[0069] Filter the supernatant liquid, then rectify, deammoniaize at normal pressure first, rectify water at normal pressure, and recove...

Embodiment 3

[0072] It is basically the same as Example 1, except that the temperature in the reaction is 130° C. After the reaction, the GC content of the target product 2,2,6,6-tetramethyl-4-aminopiperidine is 92.39%, while The content of by-product piperidinol is 6.65%.

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Abstract

The invention relates to a preparation method of 2, 2, 6, 6-tetramethyl-4-aminopiperidine. The preparation method comprises the following steps: adding ammonia water into a hydrogenation kettle, adding a supported nickel catalyst, finally adding 2, 2, 6, 6-tetramethylpiperidone, mixing while stirring, heating the hydrogenation kettle, heating the kettle to 110-125 DEG C, introducing hydrogen, controlling the pressure to 1.5-2.5 MPa, and maintaining the hydrogenation kettle to react at a certain pressure and a certain temperature until the reaction is finished; and rectifying to obtain a finished product of 2, 2, 6, 6-tetramethyl-4-aminopiperidine. According to the method, the 2, 2, 6, 6-tetramethyl-4-aminopiperidine with the purity higher than 99% is obtained with high selectivity and highyield, and the production cost is reduced.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a preparation method of 2,2,6,6-tetramethyl-4-aminopiperidine. Background technique [0002] The hindered amine light stabilizer intermediate 2,2,6,6-tetramethyl-4-aminopiperidine can be used as a light stabilizer intermediate and can be used to synthesize bonded and polymeric hindered amine light stabilizers stabilizer. [0003] At present, there are a certain number of reports on the industrial synthesis method of 2,2,6,6-tetramethyl-4-aminopiperidine, the main preparation method is, in the presence of a certain concentration of ammonia, Raney nickel or Raney cobalt It can be prepared by hydrogenation under the same conditions. This method has extremely high requirements on raw materials and reaction conditions, and is not suitable for large-scale industrial production. [0004] V.A.Golubev et al. reported in 1982 that tetramethylpiperidone was used as raw material to prepare 4-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/58B01J23/755B01J37/08B01J37/18
CPCB01J23/755B01J37/086B01J37/18C07D211/58
Inventor 王福龙李焕成吴邦元杨钦
Owner 江苏富比亚化学品有限公司
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