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Synthesizing technology of hindered amine light stabilizer Tinuvin-770

A technology of tinuvin-770 and hindered amine light stabilizer, which is applied in the direction of organic chemistry, can solve the problems of large molecular structure of piperidinol, harsh selection, and difficulty in displacement reaction, etc., and is easy to implement, easy to operate, and beneficial to Promoted app performance

Inactive Publication Date: 2012-03-21
SUQIAN UNITECHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But piperidinol carries out transesterification reaction with dimethyl sebacate, because the molecular volume of piperidinol is big, the structure is comparatively complicated, its replacement reaction is comparatively difficult with respect to the replacement of aliphatic alcohol, so the conditions such as its solvent, catalyst Select more harsh

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In the first step, drop into 471g (3mol) of tetramethylpiperidinol, 303g (1.5mol) of sebacic acid, 15.5g of para Toluenesulfonic acid and 600g of toluene;

[0022] In the second step, start the agitator and heat up to 106-110°C, then reflux the water separator until no water drops are formed, and continue to reflux for 1 hour;

[0023] The third step is to cool the four-necked flask to 30-40°C after reflux, add water to wash twice, and then distill out toluene under reduced pressure;

[0024] In the fourth step, add water and stir, cool and recrystallize, and then filter and centrifugally wash to obtain 695.7 g of white crystalline powder bis-2,2,6,6-tetramethyl-4-piperidinate, which Yield: 96.6%, melting point: 83.4-85°C, GC: 99.0%.

Embodiment 2

[0026] In the first step, drop into 471g (3mol) of tetramethylpiperidinol, 303g (1.5mol) of sebacic acid, 15.5g of para Toluenesulfonic acid and 600g of xylene;

[0027] In the second step, start the agitator and heat up to 106-110°C, then reflux the water separator until no water drops are formed, and continue to reflux for 1 hour;

[0028] The third step is to cool the four-necked flask to 30-40°C after reflux, add water to wash twice, and then distill out xylene under reduced pressure;

[0029] The fourth step is to add water and stir, after cooling and recrystallization, and then through the filtration and centrifugal washing process, 697.5g of white crystalline powder bis-2,2,6,6-tetramethyl-4-piperidinate can be obtained, which Yield: 96.9%, melting point: 83.2-84.5°C, GC: 99.0%.

Embodiment 3

[0031] The first step, drop into 471g (3mol) tetramethylpiperidinol, 303g (1.5mol) of sebacic acid, the catalyst of 22.2g in the 2L four-necked flask that has cooling water pipe, stirring, water separator, thermometer p-toluenesulfonic acid and 600g of xylene;

[0032] In the second step, start the agitator and heat up to 106-110°C, then reflux the water separator until no water drops are formed, and continue to reflux for 1 hour;

[0033] The third step is to cool the four-necked flask to 30-40°C after reflux, add water to wash twice, and then distill out xylene under reduced pressure;

[0034] In the fourth step, add water and stir, cool and recrystallize, and then filter and centrifuge to obtain 699.5 g of bis-2,2,6,6-tetramethyl-4-piperidinate, a white crystalline powder. Yield: 97.2%, melting point: 83.7-84.8°C, GC: 99.0%. .

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Abstract

The invention discloses a synthesizing technology of a hindered amine light stabilizer Tinuvin-770, which comprises the steps of: step 1, adding 2,2,6,6-tetramethyl-4-piperidinol, sebacic acid, catalyst and solvent into a four-neck flask to mix; step 2, starting a stirrer, heating, backflow distributing through a water segregator until no water drop is generated, and keeping back flowing for 1h; step 3, after finishing the back flowing, cooling the four-neck flask to 30-40 DEG C, washing with water for two times, and then steaming the solvent through reducing the pressure; and step 4, adding water to stir, after cooling and recrystallizing, carrying out the filtering centrifuging washing technology, and obtaining white crystalline powder, i.e. the sebacic acid bis(2,2,6,6-tetramethyl-4-piperidinol). The technology utilizes the sebacic acid for esterification reaction to substitute dimethyl sebacate for interesterification reaction and uses water for recrystallization to substitute organic solvent, so the cost of raw materials is reduced, the Tinuvin-770 which is synthesized by the technology has high yield and purity, good color and quality, and the technology is convenient to operate and is easy to carry out.

Description

technical field [0001] The invention relates to a synthesis process of hindered amine light stabilizer Tinuvin-770. Background technique [0002] Hindered amine light stabilizer Tinuvin-770 chemical name bis-2,2,6,6-tetramethyl-4-piperidine sebacate, suitable for polypropylene, high-density polyethylene, polyurethane, polystyrene, ABS resin etc., the light stabilization effect of 770 is better than that of the light stabilizers commonly used at present. Used in combination with antioxidants can improve heat resistance, and used in combination with ultraviolet light absorbers can also have a synergistic effect, which can further improve the light stabilization effect. At present, the hindered amine light stabilizer Tinuvin-770 developed in my country has the disadvantages of large consumption of raw materials and high product cost, and there is still a gap between domestic scientific research and production levels compared with foreign advanced countries. There are few dome...

Claims

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Application Information

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