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Method for preparing intermediate 2,2,6,6-tetramethyl-4-piperidylamine

A technology of tetramethylpiperidine amine and tetramethylpiperidine imine is applied in the field of preparation of pharmaceutical and plastic additive intermediates, and can solve the problem of low raw material reuse rate, low acetone conversion rate, easy deactivation of catalysts, etc. problems, to reduce the risk of inactivation or poisoning, prolong the service life and the number of cycles, and shorten the response time.

Active Publication Date: 2019-12-03
宁夏沃凯珑新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, the reaction time is longer, the conversion rate of acetone is not high, the catalyst is easily deactivated, and the recycling rate of raw materials is low.
In addition, in this method, a large amount of caustic soda (sodium hydroxide) is used to dehydrate the product, causing serious pollution and waste

Method used

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  • Method for preparing intermediate 2,2,6,6-tetramethyl-4-piperidylamine
  • Method for preparing intermediate 2,2,6,6-tetramethyl-4-piperidylamine
  • Method for preparing intermediate 2,2,6,6-tetramethyl-4-piperidylamine

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Experimental program
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Embodiment 1

[0048] Embodiment 1: Preparation of nickel-skeleton catalyst modified by sodium hydroxyphenyl phosphate

[0049] 1) In a 1L three-necked flask equipped with a stirring paddle, add 600ml of 10% sodium hydroxide aqueous solution, heat to 90°C, and under stirring, add 40g of nickel-aluminum-zinc (Ni3Al2Zn1) alloy in batches. The speed of addition should keep the temperature of the solution between 90 and 95°C, and the addition should be completed within about 20 to 30 minutes. Stirring was continued for another 1 hour. Let it stand, let the nickel sink, discard the supernatant, and then wash five times by decantation, each time using 200ml. Then wash five times with ethanol, 50ml each time. During the washing process, the nickel powder should always be covered by the liquid, and the catalyst should not be in contact with the air. The prepared catalyst should be stored in absolute ethanol for subsequent use;

[0050] 2) Take 50g of the skeleton nickel catalyst prepared above, ...

Embodiment 2

[0051] Example 2: Preparation of 2,2,6,6-tetramethylpiperidinium amine using a modified nickel skeleton catalyst. Add 100 L of acetone and 500 g of ammonium nitrate into a 300 L amination kettle, then start stirring and raise the temperature to 50 ° C, and start to add amine Ammonia gas is fed into the kettle at a rate of about 1kg / min. The reaction temperature of the amination process is controlled at 50-70° C., and the pressure is 0.2 MPa. After the completion of the ammonia flow, keep the reaction for 2 hours to complete the reaction, and then cool down to 30°C to release the pressure, and at the same time absorb ammonia with water to produce by-product ammonia water. Add 5g caustic soda in still, to destroy catalyst ammonium nitrate. After stirring for 30 minutes, the temperature was lowered to normal temperature and transferred to a still, and the reaction liquid was absorbed and treated for the ammonia in the system before being transferred into the still.

[0052] The...

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Abstract

The invention relates to a method for preparing intermediate 2,2,6,6-tetramethyl-4-piperidylamine. The method is characterized by comprising the following steps: step 1), in the presence of a catalyst1, reacting acetone with ammonia gas to produce 2,2,6,6-tetramethyl-4-piperidinone and water; and step 2), in the presence of a catalyst 2, reacting the 2,2,6,6-tetramethyl-4-piperidinone with ammonia gas to produce 2,2,6,6-tetramethyl-4-piperidylimine and water, and reacting the 2,2,6,6-tetramethyl-4-piperidylimine with hydrogen gas to produce the 2,2,6,6-tetramethyl-4-piperidylamine, wherein the catalyst 1 is ammonium nitrate, and the catalyst 2 is a sodium hydroxyphenyl phosphate modified framework nickel catalyst. The method provided by the invention has the advantages of short synthetictime, a high conversion rate of the acetone and a high repeating utilization rate of the raw materials.

Description

technical field [0001] The invention belongs to the field of intermediate synthesis, and more specifically relates to a preparation method of a medicine and plastic additive intermediate. Background technique [0002] 2,2,6,6-Tetramethylpiperidinamine (hereinafter referred to as TAM) is an important intermediate that can be used to synthesize a series of hindered amine light stabilizers with excellent performance. [0003] Currently, 2,2,6,6-tetramethylpiperidinamine is synthesized from 2,2,6,6-tetramethylpiperidone by hydrogenation reduction. There are two methods for the synthesis of 2,2,6,6-tetramethylpiperidone reported in the literature—indirect method and direct method. The indirect method is to use acetone as a raw material to generate acetonin, diacetone alcohol or phorone under the action of a catalyst, and then continue to react the obtained acetonin, diacetone alcohol and phorone under the action of a catalyst to obtain 2, 2,6,6-Tetramethylpiperidone. The direc...

Claims

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Application Information

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IPC IPC(8): C07D211/58C07D211/72B01J31/02
CPCC07D211/58C07D211/72B01J31/0269B01J31/0267
Inventor 郭徐良万学明
Owner 宁夏沃凯珑新材料有限公司
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