A hindered amine light stabilizer intermediate and its preparation method and application
A technology of hindered amine light stabilizer and intermediate, which is applied in the field of hindered amine light stabilizer intermediate and its preparation, can solve the problems of poor compatibility and poor synergistic effect, and achieves improved photostability and simple and easy reaction method. Controlled, high-yield effects
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Embodiment 1
[0038] A preparation method of a hindered amine light stabilizer intermediate, comprising the steps of:
[0039] Add 155g of triacetone amine, 81g of dimethylamine, 400g of xylene and 120g of formic acid in a 2L reactor, under the protection of nitrogen, start stirring and heat up to 130-135°C. After 6 hours, the sampling test is qualified, and the The reaction solution was down to room temperature, washed with aqueous sodium hydroxide solution (30%, wt.) and deionized water to weak alkalinity successively, and distilled under negative pressure to obtain the compound shown in the intermediate formula II (wherein, R is a methyl group), and the yield was 97.5%.
[0040] Put 179.44g of the compound represented by the intermediate formula II obtained above into a 2L reaction kettle, and add 126g of dimethyl malonate, 200g of xylene and 10g of lithium amide into the kettle, start stirring and raise the temperature to 130-135°C, After 4 hours, the sampling test was qualified, quenc...
Embodiment 2
[0044] A preparation method of a hindered amine light stabilizer intermediate, comprising the steps of:
[0045]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 down to room temperature, washed with aqueous sodium hydroxide solution (30%, wt.) and deionized water to weak alkalinity successively, and distilled under negative pressure to obtain the compound shown in the intermediate formula II (wherein, R is a methyl group), and the yield was 98.3%.
[0046] Put 180.87g of the compound represented by the intermediate formula II obtained above into a 2L reaction kettle, and add 131g of dimethyl malonate, 300g of xylene and 10g of lithium amide into the kettle, start stirring and raise the temperature to 130-135°C, After 5 hours, the sample was tested to be quali...
Embodiment 3
[0048] A preparation method of a hindered amine light stabilizer intermediate, comprising the steps of:
[0049] Add 155g of triacetone amine, 50g of dimethylamine and 320g of toluene into a 2L reactor, under the protection of nitrogen, start to stir and preheat to 105°C, then add 115g of formic acid, the reaction temperature rises to 105-110°C, 7 Hours later, the sampling test was qualified, and the reaction solution was down to room temperature, washed with aqueous sodium hydroxide solution (30%, wt.) and deionized water to weak alkalinity successively, and negative pressure distillation obtained the compound shown in the intermediate formula II (wherein, R is methyl), the yield is 96.7%.
[0050] Put 177.93g of the compound represented by the intermediate formula II obtained above into a 2L reaction kettle, and add 140g of dimethyl malonate, 300g of toluene and 11g of lithium amide into the kettle, start stirring and raise the temperature to 105-110°C, 8 Hours later, the s...
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