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Method for preparing 2,2,6,6-tetramethyl-4-piperidinamine

A technology of tetramethyl and piperidine amine, which is applied in the field of preparation of piperidine amine, to achieve the effect of improving the purity of rectification and improving the conversion rate

Active Publication Date: 2014-05-21
安徽奥瑞化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing direct synthesis method of 2,2,6,6-tetramethyl-4-piperidone has the defect of many by-products, resulting in time-consuming and labor-intensive product separation and purification, long production cycle and high synthesis cost

Method used

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  • Method for preparing 2,2,6,6-tetramethyl-4-piperidinamine
  • Method for preparing 2,2,6,6-tetramethyl-4-piperidinamine

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Experimental program
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Embodiment 1

[0030] A preparation method of 2,2,6,6-tetramethyl-4-piperidinamine, comprising the steps of:

[0031] (1) Synthesis of 2,2,6,6-tetramethyl-4-piperidone:

[0032] Put 2600L of acetone into the synthesis kettle, add 57.5kg of catalyst and stir, raise the temperature to 30°C, start charging ammonia (100kg) once, control the ammonia charging speed to 100kg / h, during the process of ammonia filling, the temperature of the synthesis kettle will continue to rise, properly raise the temperature, and control The temperature of the kettle is 30±1°C; keep warm for 5 hours after the first ammonia filling, start the second ammonia filling (36kg), and keep warm after the second ammonia filling.

[0033] Sampling analysis: At this time, the content should be about 20%. If the content is not reached, continue to keep warm for 1 hour, and then take a sample for analysis.

[0034] The sample analysis adopts gas chromatography, and the chromatographic conditions are as follows: the initial temp...

Embodiment 2

[0045] Compared with Example 1, the feed ratio of 2,2,6,6-tetramethyl-4-piperidone hydrogenation reaction in step (2) is shown in the table below, and the rest remain unchanged.

[0046] raw material 100kg water 33kg catalyst 3kg liquid ammonia 28kg

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Abstract

The invention discloses a method for preparing 2,2,6,6-tetramethyl-4-piperidinamine. The method comprises the following steps: synthesizing 2,2,6,6-tetramethyl-4-piperidone and carrying out a hydrogenation reaction of the 2,2,6,6-tetramethyl-4-piperidone. The key synthesis steps are controlled, the addition amount for acetone recovery is controlled, and the rectification purity and conversion rate of the product are improved through the optimized distillation, crystallization and hydrogenation reduction process.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of piperidinamine. Background technique [0002] 2,2,6,6-Tetramethyl-4-piperidinamine belongs to the hindered amine piperidine compound, which has good light stabilizing activity on polymer materials and is an important intermediate for the synthesis of hindered amine light stabilizers . Due to the important role of hindered amine light stabilizers in polymer material additives, its development is getting faster and faster, and its demand is also increasing. As an important intermediate of hindered amine light stabilizers, 2,2,6,6-tetramethyl-4-piperidinamine has an increasing demand, and there is a domestic demand of tens of thousands of tons every year. [0003] At present, 2,2,6,6-tetramethyl-4-piperidinamine is synthesized by hydrogenation reduction of 2,2,6,6-tetramethyl-4-piperidinone, while the synthesis of 2, There are two m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/58
CPCC07D211/58
Inventor 祝梓琦
Owner 安徽奥瑞化工有限公司