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Hindered amine light stabilizer 3346 preparation method

A technology of light stabilizers and hindered amines, applied in the field of compound preparation, can solve the problems of high energy consumption, post-processing of organic solvents and environmental problems.

Active Publication Date: 2015-06-24
江苏富比亚化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction at low temperature requires cooling the medium, which consumes a lot of energy, and the use of organic solvents has certain problems in post-processing and environmental protection.

Method used

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  • Hindered amine light stabilizer 3346 preparation method
  • Hindered amine light stabilizer 3346 preparation method
  • Hindered amine light stabilizer 3346 preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]Add 50.71g (0.275mol) of cyanuric chloride and 200mL of pure water to a 500mL four-neck flask, cool down in an ice bath to below 10°C, add dropwise 30.49g (0.35mol) of morpholine under stirring, maintain 0-10°C, drop Adding time is 1.5h; after dropping, add 10% sodium hydroxide dropwise, containing 14.8g (0.37mol) of sodium hydroxide, keep at 0-10°C, drop for 1h, keep at 0-10°C for 0.5h after dropping ;Heat up to 20°C, add dropwise 10% sodium hydroxide aqueous solution, containing 2.8g (0.07mol) of sodium hydroxide, add dropwise for 0.5h, keep at 20°C for 1h after dropping; heat up to 45°C for 1h, control pH =8~9 for 0.5h. Filter, wash with water to pH = 7, and dry at 80°C to obtain 67.12 g of white powder with a yield of 98.01%. HPLC analysis yields nI:nII = 8:3.

[0033] Add 68.43g of the product obtained by the above method in a 1L autoclave, 90.78g (0.23mol) of hexamethylenediamine piperidine, 400mL of dimethylbenzene, seal, nitrogen replacement under stirring to re...

Embodiment 2

[0035] Add 50.71g (0.275mol) of cyanuric chloride and 200mL of pure water to a 500mL four-neck flask, cool down in an ice bath to below 10°C, add dropwise 25.16g (0.29mol) of morpholine under stirring, maintain 0-10°C, drop Adding time is 1.5h; after dropping, add 10% sodium hydroxide dropwise, containing 11.6g (0.29mol) of sodium hydroxide, keep at 0-10°C, drop for 1h, keep at 0-10°C for 0.5h after dropping ;Heat up to 20°C, add dropwise 10% sodium hydroxide aqueous solution, containing 2.32g (0.058mol) of sodium hydroxide, add dropwise for 0.5h, keep at 20°C for 1h after dropping; heat up to 45°C for 1h, control pH =8~9 for 0.5h. Filter, wash with water to pH = 7, and dry at 80°C to obtain 64.36 g of white powder with a yield of 98.5%. HPLC analysis shows nI:nII = 8:0.5.

[0036] Add 50.58g of the product obtained by the above method into a 1L autoclave, 78.94g (0.2mol) of hexamethylenediamine piperidine, 400mL of xylene, remove the air in the autoclave by nitrogen replacem...

Embodiment 3

[0038] Add 50.71g (0.275mol) of cyanuric chloride and 200mL of pure water to a 500mL four-neck flask, cool down in an ice bath to below 10°C, add dropwise 35.94g (0.41mol) of morpholine under stirring, maintain 0-10°C, drop Adding time is 1.5h; after dropping, add 10% sodium hydroxide dropwise, containing 16.4g (0.41mol) of sodium hydroxide, keep at 0-10°C, drop for 1h, keep at 0-10°C for 0.5h after dropping ;Heat up to 20°C, add dropwise 10% sodium hydroxide aqueous solution, containing 3.28g (0.082mol) of sodium hydroxide, add dropwise for 0.5h, keep at 20°C for 1h after dropping; heat up to 45°C for 1h, control pH =8~9 for 0.5h. Filter, wash with water to pH = 7, and dry at 80°C to obtain 67.12g of white powder with a yield of 98.01%. HPLC analysis converted nI:nII = 2:1.

[0039] Add 75.58g of the product obtained by the above-mentioned method in a 1L autoclave, 94.72g (0.24mol) of hexamethylenediamine piperidine, 400mL of xylene, seal, remove the air in the autoclave by ...

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Abstract

The invention discloses a hindered amine light stabilizer 3346 preparation method. The method includes the steps: 1) preparing a mixture of an intermediate I and an intermediate II according to a specific ratio by reaction of cyanuric chloride and morpholine, wherein the intermediate I refers to 2-morpholinyl-4,6-dichloro-1,3,5-triazine, and the intermediate II refers to 2,4-dimorpholine-6-chloro-1,3,5-triazine; 2) subjecting the intermediate mixture and hexanediamine piperidine to temperature-gradient heating under a pressure to obtain the light stabilizer 3346. The preparation method has the advantages that economy and environment friendliness are realized due to adoption of water as solvent at the first step, and the mixture of the intermediates I and II in the specific ratio is synthesized under proper conditions without separation; at the second step, reaction difficulty is raised due to different substitute degrees of three chlorines, and a product narrow in relative molecular mass distribution and excellent in transparency is obtained by means of temperature-gradient heating under a certain pressure.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of hindered amine light stabilizer 3346. Background technique [0002] Light stabilizer 3346 is currently one of the best varieties of HALS in the world. It is a polymeric hindered amine light stabilizer with excellent performance developed by American cyanamide company in 1987. As a non-toxic industrial chemical, it has long been Obtained FDA approval. It is mainly used in various polymers such as polypropylene, polyethylene, polystyrene and nylon. It is particularly effective in the protection of colored or colorless polyolefin products that require high weather resistance, and is especially suitable for agricultural film, fiber and molding products, etc. In addition to the characteristics of excellent light stability, excellent compatibility with resin, light color, non-toxicity and low volatility at high temperature, it also has good thermal oxygen ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/14
CPCC07D401/14
Inventor 王春平刘冰宋君荣施波
Owner 江苏富比亚化学品有限公司
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