Synthetic method of amino-2,2,6,6-tetramentylniperidine with specific pH range

A technology of tetramethylpiperidinium synthesis method, applied in the field of chemical industry, can solve the problems of not adjusting the pH of the reaction system, not conforming to the concept of green chemistry, and high economic cost, so as to reduce ring-opening products, mild reaction conditions, reduce The effect of reaction temperature

Pending Publication Date: 2019-06-04
安徽新秀化学股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using strong acid as the electrolyte will cause great corrosion to the equipment and high cost, which does not conform to the concept of green chemistry
[0009] The above-mentioned existing production process of tetramethylpiperidinamine has relatively large energy consumption and high economic cost because the pH of the reaction system has not been adjusted, resulting in high reaction temperature and high energy consumption.

Method used

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  • Synthetic method of amino-2,2,6,6-tetramentylniperidine with specific pH range
  • Synthetic method of amino-2,2,6,6-tetramentylniperidine with specific pH range
  • Synthetic method of amino-2,2,6,6-tetramentylniperidine with specific pH range

Examples

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Embodiment 1

[0038] Embodiment 1, a synthesis method of 2,2,6,6-tetramethylpiperidinamine in a specific pH range, the following steps are carried out in sequence:

[0039] (1) Add 30ml of water into the autoclave, 10g (0.0644mol) of raw material 2,2,6,6-tetramethylpiperidone, 15g (0.22mol of ammonia) with a mass fraction of 25%, add NaOH for about 0.05g, thereby adjusting the pH value of the system=12.0, and then adding 0.5g framework nickel as a catalyst.

[0040] (2) feed nitrogen to replace the air in the still, and after nitrogen replacement, feed hydrogen to replace the nitrogen in the still, and now the pressure in the still is 0Mpa. Turn on the stirring and heating device, so that the material in the kettle is raised to 60°C, and the stirring speed is 400 rpm.

[0041] (3) After stirring for 2 hours, start to feed hydrogen into the kettle until the pressure is 2.5MPa, and keep it warm for reaction; when the hydrogen in the kettle drops to ≤1.5MPa, continue to feed hydrogen until th...

Embodiment 2

[0044]Example 2. In Example 1, "add about 0.05 g of NaOH" is changed to "add about 0.1 g of NaOH". At this time, the pH of the system is 12.7, and the rest are the same as in Example 1. The product yield was 96.2%, and the purity was 99.1%.

[0045] Explanation: Add a small amount of NaOH appropriately to adjust the pH of the system to 13; the rest are the same as in Example 2 above; the yield and purity of the obtained product are basically the same as in Example 2.

Embodiment 3

[0046] Embodiment 3. In embodiment 1, "make the material in the kettle rise to 60°C" is changed to "raise the temperature to 55°C". The rest are equal to Example 1.

[0047] The product yield was 96.1%, and the purity was 99.1%.

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Abstract

The invention discloses a synthetic method of amino-2,2,6,6-tetramentylniperidine with a specific pH range, and the method comprises the following steps: taking 2,2,6, 6-tetramethyl piperidone as a raw material, adding the raw material and ammonia water into a high-pressure kettle, first adjusting the pH value to 12.0-13.0, adding framework nickel serving as a catalyst, carrying out hydrogenationreaction at temperature of 55-65 DEG C under a set pressure value of 1.5-2.5 mpa, stopping the reaction until the pressure in the kettle is always not lower than 2% of a set pressure value in one hour; and carrying out normal pressure distillation on the reaction liquid, and then carrying out reduced pressure rectification to obtain the product amino-2,2,6,6-tetramentylniperidine. According to themethod disclosed by the invention, the conversion rate of the tetramethyl piperidone is improved, and the product yield is improved.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a synthesis method of 2,2,6,6-tetramethylpiperidinamine in a specific pH range. Background technique [0002] 2,2,6,6-Tetramethylpiperidinamine, the structural formula is as follows: Formula 1, molecular formula C 9 h 10 N 2 . English abbreviation TAD, Chinese abbreviation Tetramethylpiperidinamine, is an important chemical intermediate, mainly used in the synthesis of bonded and polymer hindered amine light stabilizers. [0003] [0004] At present, the synthetic methods of 2,2,6,6-tetramethylpiperidinamine are as follows: [0005] 1. Synthesis of tetramethylpiperidinamine by catalytic amination method. Literature (Journal of Tianjin University, 1999 (04): 96-99) proposes the suitable process condition of catalytic amination method, with tetramethylpiperidone (2,2,6,6-tetramethylpiperidone) and ammonia As a raw material, skeleton nickel is used as a catalyst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/58
Inventor 万文静钱超张秀秀唐赟
Owner 安徽新秀化学股份有限公司
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