2,2,6,6-tetramethylpiperidone synthesis method for setting end-point determination mode

A technology of tetramethylpiperidone and synthesis method, applied in the direction of organic chemistry, etc., to achieve the effects of less side reactions, high yield, and reducing the amount of by-products

Active Publication Date: 2018-04-17
YANTAI XINXIU CHEM TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The by-product cannot be converted into the target product 2,2,6,6-tetramethylpiperidone under the reaction conditions

Method used

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  • 2,2,6,6-tetramethylpiperidone synthesis method for setting end-point determination mode
  • 2,2,6,6-tetramethylpiperidone synthesis method for setting end-point determination mode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1, add acetone 87g (1.5mol), 8g (0.1mol) ammonium nitrate in the autoclave of 250mL; Pass into liquid ammonia 8.5g (0.5mol), heat up to 60 ℃ under stirring; Continuous detection in the reaction process When the pH value of the reaction system does not change within 30 minutes, the heating can be stopped, thereby terminating the reaction. At this time, the reaction time is about 4 hours, and the pressure of the autoclave is about 0.1 MPa; the concentration of the product in the GC is 48%.

[0024] After the reaction is completed, the reaction solution is suction-filtered in a Buchner funnel first, and the obtained filtrate is roughly steamed under normal pressure, and the obtained light components are recovered and used mechanically (that is, acetone is recovered by distillation); Sodium hydroxide is used to absorb the water generated by the reaction. The mass ratio of sodium hydroxide to the crude steamed heavy component (that is, the distillation substrate) ...

Embodiment 2

[0025] Embodiment 2, the reaction temperature of embodiment 1 is changed from 60 ℃ to 65 ℃, and the rest are equal to embodiment 1.

[0026] The final yield of 2,2,6,6-tetramethylpiperidone was 81.8%.

Embodiment 3

[0027] Embodiment 3, change the consumption of raw material into: acetone 87g (1.5mol), 4g (0.05mol) ammonium nitrate; Feed liquid ammonia 8.5g (0.5mol), all the other are equal to embodiment 1.

[0028] The final yield of 2,2,6,6-tetramethylpiperidone was 80.5%.

[0029] Embodiment 3, change the consumption of raw material into: acetone 87g (1.5mol), 12g (0.15mol) ammonium nitrate; Feed liquid ammonia 8.5g (0.5mol), all the other are equal to embodiment 1.

[0030] The final yield of 2,2,6,6-tetramethylpiperidone was 81.8%.

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Abstract

The invention discloses a 2,2,6,6-tetramethylpiperidone synthesis method for setting an end-point determination mode. A synthesis reaction comprises the steps of using acetone and ammonia as raw materials and heating for reaction under the action of ammonium nitrate as a catalyst; recovering the acetone by distillation after the reaction, alkali-washing distillation substrate and rectifying to obtain 2,2,6,6-tetramethylpiperidone; detecting pH value during the reaction, determining that the end of the reaction is reached if the pH value remains unchanged within 30 minutes, and stopping the heating to end the above reaction. The synthesis method has mild conditions, cheap and easily available raw materials and catalyst, and less side reactions. Since the amount of by-products is reduced, the post-treatment is relatively simple and the yield is high.

Description

technical field [0001] The invention relates to a synthesis method of 2,2,6,6-tetramethylpiperidone with an end point judgment mode set. Background technique [0002] 2,2,6,6-Tetramethylpiperidone, which has the formula C 9 h 17 NO, the structural formula is as follows: [0003] [0004] The secondary amine group of 2,2,6,6-tetramethylpiperidone can be converted into a stable nitroxide free radical under thermal and photooxidative conditions, which can effectively free the alkoxylate in the polymer 2,2,6,6-Tetramethylpiperidone is an important raw material for the preparation of hindered amine light stabilizers . At present, in literature reports, the method for producing 2,2,6,6-tetramethylpiperidone mainly contains the following: [0005] Method 1: Using acetone and liquid ammonia as raw materials, first generate acetonin, diacetone alcohol or phorone, separate and purify acetonin, diacetone alcohol or phorone, and then pass ammonia gas to generate 2,2,6 ,6-Tetram...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/74C07D211/02
CPCC07D211/02C07D211/74
Inventor 史雅静王轲钱超张秀秀
Owner YANTAI XINXIU CHEM TECH CO LTD
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