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2,2,6,6,-tetramethyl-4-piperidone continuous synthesis method

A synthesis method and piperidone technology are applied in the field of synthesis of 2,2,6,6-tetramethyl-4-piperidone, and can solve the problems of increased production cost, reduced selectivity, easy inactivation and the like, Achieve the effect of avoiding pollution, low cost and improving product purity

Active Publication Date: 2015-04-08
安徽兴欣新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And react under the temperature condition of 120-240 ℃, energy consumption is very high, increased production cost and can make the selectivity of 2,2,6,6 tetramethyl-4-piperidone greatly reduce simultaneously; In addition, this The patent covers a wide range of catalysts, and some of them, such as supported metal halides and supported inorganic organic ammonium salt catalysts, are easily deactivated during the reaction process

Method used

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  • 2,2,6,6,-tetramethyl-4-piperidone continuous synthesis method
  • 2,2,6,6,-tetramethyl-4-piperidone continuous synthesis method
  • 2,2,6,6,-tetramethyl-4-piperidone continuous synthesis method

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Effect test

Embodiment 1

[0024] A kind of 2,2,6,6-tetramethyl-4-piperidone continuous synthesis method, comprises the steps:

[0025] (1) The reactor is a fixed-bed single-tubular reactor with an inner diameter of 14mm and a tube length of 650mm. It is filled with 40mL of sulfonic acid resin D061, and heated to keep the temperature of the fixed-bed single-tubular reactor at 60°C;

[0026] (2) Acetone and ammonia gas are passed into the reactor from the upper end of the fixed-bed single-tubular reactor through the preheater according to the molar ratio of 6:1, and the volume space velocity of acetone is 0.39h -1 , the volumetric space velocity of ammonia gas is 20.7h -1 ;

[0027] (3) The reaction product flows out from the lower end of the fixed-bed single-tubular reactor, and the effluent is cooled and gas-liquid separated to obtain the crude product of 2,2,6,6-tetramethyl-4-piperidone. After gas chromatography analysis, the selectivity was 65%.

Embodiment 2

[0029] A kind of 2,2,6,6-tetramethyl-4-piperidone continuous synthesis method, comprises the steps:

[0030] (1) The reactor is a fixed-bed single-tubular reactor with an inner diameter of 14mm and a tube length of 650mm. It is filled with 40mL of sulfonic acid resin D072 and heated to keep the temperature of the fixed-bed single-tubular reactor at 50°C;

[0031] (2) Pass acetone and ammonia gas into the reactor from the upper end of the fixed-bed single-tubular reactor through the preheater according to the molar ratio of 9:1, and the volumetric space velocity of acetone is 0.15h -1 , the volumetric space velocity of ammonia gas is 5.25h -1 ;

[0032] (3) The reaction product flows out from the lower end of the fixed-bed single-tubular reactor, and the effluent is cooled and gas-liquid separated to obtain the crude product of 2,2,6,6-tetramethyl-4-piperidone. After gas chromatography analysis, the selectivity was 60%.

Embodiment 3

[0034] A kind of 2,2,6,6-tetramethyl-4-piperidone continuous synthesis method, comprises the steps:

[0035] (1) The reactor is a fixed-bed tubular reactor with an inner diameter of 14 mm and a tube length of 650 mm. It is filled with 40 mL of sulfonic acid resin NKC-9, and heated to keep the temperature of the fixed-bed single-tubular reactor at 70 ° C;

[0036] (2) Pass acetone and ammonia gas into the reactor from the upper end of the fixed-bed single-tubular reactor through the preheater according to the molar ratio of 3:1, and the volume space velocity of acetone is 1.17h -1 , the volume space velocity of ammonia gas is 124.2h -1 ;

[0037] (3) The reaction product flows out from the lower end of the fixed-bed single-tubular reactor, and the effluent is cooled and gas-liquid separated to obtain a crude 2,2,6,6-tetramethyl-4-piperidone as a liquid. After gas chromatography analysis, the selectivity was 54%.

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Abstract

The invention discloses a 2,2,6,6,-tetramethyl-4-piperidone continuous synthesis method. The 2,2,6,6,-tetramethyl-4-piperidone continuous synthesis method comprises the following steps of 1, filling an acidic resin into a fixed bed reactor, and carrying out heating so that a temperature of the fixed bed reactor is in a range of 40 to 70 DEG C, and 2, feeding acetone and ammonia gas into the fixed bed reactor according to a mole ratio of 3-9: 1 under the conditions of acetone hourly space velocity of 0.15 to 1.17h<-1> and ammonia gas hourly space velocity of 5.25 to 124.20h<-1>, and cooling the product to obtain a 2,2,6,6,-tetramethyl-4-piperidone crude product. The 2,2,6,6,-tetramethyl-4-piperidone continuous synthesis method has simple processes and a low cost, is suitable for industrial continuous production, does not adopt an organic solvent or water as a solvent, avoids the pollution produced by the organic solvent on the environment, has mild reaction conditions, can be carried out at a temperature of 40 to 70 DEG C, has low energy consumption, and avoids the influence caused by impurities produced at a high temperature on the product.

Description

technical field [0001] The invention relates to a synthesis method of 2,2,6,6-tetramethyl-4-piperidone. Background technique: [0002] Since the late 1960s, when Murayama Keisuke and others of Japan Sankyo Company first discovered the miraculous light-stabilizing activity of hindered amine piperidine compounds on polymer resins, hindered amine light stabilizers have always been the focus of research and development. There are more than a thousand patents on amine light stabilizers, and industrialized products emerge in endlessly. And 2,2,6,6-tetramethyl-4-piperidone is the basic raw material of most hindered amine light stabilizers such as Tinuvin622, Tinuvin770 and Chimassorb944, which are widely used at present, and is an intermediate of hindered amine light stabilizers Such as 2,2,6,6,-tetramethyl-4-piperidinol, 2,2,6,6,-tetramethyl-4-piperidinamine and N,N-bis(2,2,6 ,6,-Tetramethyl-4-piperidinyl) the derivative parent of 1,6-hexanediamine. Due to the important role of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/74
Inventor 陈立功李阳闫喜龙田军宋歌
Owner 安徽兴欣新材料有限公司
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