Synthesis technology of tetramethylpiperidine

A technology of tetramethylpiperidol and tetramethylpiperidone is applied in the field of tetramethylpiperidol synthesis technology, and can solve the problems of expensive catalyst Ru/C, complex electrolyzer structure, expensive reducing agent and the like , to achieve the effect of reducing synthesis cost, easy implementation and no environmental pollution

Inactive Publication Date: 2012-02-15
SUQIAN UNITECHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 2. The chemical reduction method uses aluminum isopropoxide, sodium borohydride, etc. as reducing agents to reduce piperidinone to piperidinol, but the reducing agent is more expensive and the post-reaction treatment is more complicated, so it is rarely used in industry; 3. Electrochemical reduction method, piperidinone is reduced to piperidinol at the cathode of the electrolytic cell, but

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The first step, add tetramethylpiperidone 155g, catalyzer 15.5g, caustic soda 1.55g and water 400g in the 1L autoclave that has cooling water pipe, pressure gauge, stirring, thermocouple thermometer and heating system, and seal;

[0024] In the second step, N is introduced into the kettle 2 Replace the air, then pass H 2 replace N 2 , the ultimatum H 2 to a pressure of 0.8MPa;

[0025] The third step is to first control the pressure in the kettle to maintain at 0.8MPa. When the pressure in the kettle drops, add H to the kettle in time. 2 To 0.8MPa, stir and raise the temperature at the same time, control the temperature at 90°C, repeat the above operation until the pressure in the kettle is maintained at 0.8MPa for a certain period of time without changing, stop the reaction;

[0026] The fourth step is to feed N into the kettle 2 Substitution H 2 , and at the same time, feed cooling water into the inner coil of the kettle to reduce the temperature in the kettle ...

Embodiment 2

[0029] The first step, add tetramethylpiperidone 155g, catalyzer 15.5g, caustic soda 1.55g and water 400g in the 1L autoclave that has cooling water pipe, pressure gauge, stirring, thermocouple thermometer and heating system, and seal;

[0030] In the second step, N is introduced into the kettle 2 Replace the air, then pass H 2 replace N 2 , the ultimatum H 2 to a pressure of 0.8MPa;

[0031] The third step is to first control the pressure in the kettle to maintain at 0.8MPa. When the pressure in the kettle drops, the

[0032] In the second step, N is introduced into the kettle 2 Replace the air, then pass H 2 replace N 2 , the ultimatum H 2 to a pressure of 0.8MPa;

[0033] The third step is to first control the pressure in the kettle to maintain at 0.8MPa. When the pressure in the kettle drops, add H to the kettle in time. 2 To 0.8MPa, stir and raise the temperature at the same time, control the temperature at 70-100°C, repeat the above operation until the pressure...

Embodiment 5

[0036] The first step, add tetramethylpiperidone 155g, catalyzer 7.75g, caustic soda 1.55g and water 400g in the 1L autoclave that has cooling water pipe, pressure gauge, stirring, thermocouple thermometer and heating system, and seal;

[0037] In the second step, N is introduced into the kettle 2 Replace the air, then pass H 2 replace N 2 , the ultimatum H 2 to a pressure of 0.8MPa;

[0038] The third step is to first control the pressure in the kettle to maintain at 0.8MPa. When the pressure in the kettle drops, add H to the kettle in time. 2 To 0.8MPa, stir and raise the temperature at the same time, control the temperature at 90°C, repeat the above operation until the pressure in the kettle is maintained at 0.8MPa for a certain period of time without changing, stop the reaction;

[0039] The fourth step is to feed N into the kettle 2 Substitution H 2 , and at the same time, feed cooling water into the inner coil of the kettle to reduce the temperature in the kettle ...

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PUM

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Abstract

The invention discloses a synthesis technology of tetramethylpiperidine, comprising the steps of: first, adding triacetonamin, a catalyst, flake caustic soda and water into a high-pressure reaction kettle; second, introducing N2 to the kettle, then introducing H2 to replace N2; third, controlling the pressure within the kettle to be maintained at 0.8MPa, when the pressure in the kettle decreases, supplementing H2 timely to a pressure of 0.8MPa, conducting stirring simultaneously to raise the temperature which is controlled between 70 to 100DEG C, then repeating the above operations till the pressure in the kettle is constant at 0.8MPa; fourth, introducing N2 into the kettle to replace H2, and simultaneously delivering cooling water into a coiled pipe inside the kettle so as to lower the temperature in the kettle below 50DEG C, the stopping stirring, filtering out the catalyst, and distilling out part of the water; fifth, stirring and cooling the left oversaturated mother solution in ice water bath for crystallization, then carrying out filtering and washing, thus obtaining tetramethylpiperidine. The tetramethylpiperidine synthesized by the technology of the invention has the advantages of high yield and purity, good color and quality, and no environmental pollution, so that the technology provided in the invention is good for promotion and application.

Description

technical field [0001] The invention relates to a synthesis process of tetramethylpiperidinol. Background technique [0002] The chemical name of tetramethylpiperidinol is 2,2,6,6-tetramethyl-4-piperidinol, which is a synthetic hindered amine light stabilizer, medicine, bleaching agent, polymerization inhibitor, epoxy resin crosslinking agent, etc. An important intermediate of the product. At present, the hindered amine light stabilizers developed in my country are all piperidine derivatives, and all of them are products with piperidinol as the intermediate. Therefore, the production of piperidinol is an important link in the development of light stabilizers in my country. Therefore, the synthesis research of piperidinol has important practical significance. [0003] The method for preparing piperidinol by reduction of piperidone by piperidone reported at home and abroad mainly contains following several kinds at present: [0004] 1. Catalytic hydrogenation, including pre...

Claims

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Application Information

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IPC IPC(8): C07D211/46
Inventor 项瞻波苏宏镇田礼彬
Owner SUQIAN UNITECHEM CO LTD
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