A hindered amine light stabilizer containing hindered phenol and its preparation method and application
A technology of hindered amine light stabilizer and hindered phenol is applied in the field of hindered amine light stabilizer containing hindered phenol and its preparation, which can solve the problems of low cost addition and the like, and achieve the advantages of simple preparation method, prolonged service life and easy implementation. Effect
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Embodiment 1
[0055] The preparation of the compound shown in formula II comprises the steps:
[0056]Add 155g of triacetoneamine, 68g of dimethylamine, 110g of formic acid and 330g of xylene in a 2L reaction kettle, and start stirring and warming up to 130-135°C under nitrogen protection. After 5 hours, the sampling test is qualified, and the The reaction solution was lowered to room temperature, washed with aqueous sodium hydroxide solution (30%, wt.) and deionized water to weak alkalinity, and distilled under negative pressure to obtain the compound represented by the intermediate formula IV with a yield of 98.3%.
[0057] Put the compound represented by the intermediate formula IV obtained above into a 2L reaction kettle, and add 131g dimethyl malonate, 300g xylene and 10g ammonium lithium to the kettle, start stirring and heat up to 130-135°C, 5 Hours later, the sample was tested to pass the test. After cooling, it was quenched with an organic acid, washed and dried with water, and vac...
Embodiment 2
[0061] A preparation method of a hindered amine light stabilizer containing hindered phenol, comprising the steps of:
[0062] Add 300g of the compound shown in formula II prepared in Example 1, 350g of tetramethylpiperidinol and 800g of xylene in a 3L reactor, and start stirring and heat up to 130-135°C for 0.5 hours under nitrogen protection Then add 12g of sodium methoxide, the reaction is steamed out with methanol, and keep warm for 10 hours, and the content of the compound shown in the intermediate formula III is qualified by HPLC. After the above reaction solution was cooled to 70°C, 320g of 2,6-di-tert-butyl-4-((dimethylamino)methyl)phenol, 2.1g of ammonium lithium, and 380g of xylene were added to it. , the temperature of the reaction was raised to 170-175°C, along with the dimethylamine distilled out, the sample was tested after 8 hours, and the pH was adjusted to 8-9, then the product was filtered, washed and recrystallized to obtain the light yellow target product w...
Embodiment 3
[0066] A preparation method of a hindered amine light stabilizer containing hindered phenol, comprising the steps of:
[0067] Add 300g of the compound shown in formula II prepared in Example 1, 364g of tetramethylpiperidinol and 810g of xylene in a 3L reactor, start stirring and heat up to 130-135°C for 0.5 hours under nitrogen protection Finally, 25 g of tetraethyl titanate was added, the reaction was distilled out with methanol, and kept for 11 hours, and the content of intermediate III was qualified by HPLC. After the above reaction solution was cooled to 70°C, 306g of 2,6-di-tert-butyl-4-((dimethylamino)methyl)phenol, 1.7g of ammonium lithium, and 370g of xylene were added to it. , the temperature of the reaction was raised to 170-175°C, accompanied by the distillation of dimethylamine, and the sample was tested after 7 hours, and the pH was adjusted to 8-9, and the light yellow target product was obtained by suction filtration, water washing and recrystallization, with a...
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