A kind of preparation method of ultraviolet absorber
An absorbent and ultraviolet technology, applied in the field of polymers, can solve the problems of low atom utilization, complicated operation, and environmental pollution, and achieve the effect of avoiding low atom utilization, high conversion rate, and high selectivity
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Embodiment 1
[0033] Take 10g 16g of xylene, 3.4g of water, 3.4g of diethanolamine (DEA) and 0.5g of ruthenium phosphide (Ru-P) were loaded into a 100mL reactor, and hydrogen was passed through, and reacted at 1.0MPa and 60°C until the hydrogen pressure remained constant. After the reaction, the temperature was lowered to obtain a brown-black reaction solution. Filter the reaction solution, remove the catalyst, extract the organic phase, add absolute ethanol and ice water at a volume ratio of 1:1 overnight, and filter to obtain 2.5 g of light yellow crystals, namely the ultraviolet absorber.
[0034] figure 1 For the nuclear magnetic pattern of the azo intermediate that embodiment 1 makes, by figure 1 It can be seen that the single peak at δ=2.455ppm is -CH 3 The peak of three hydrogens on the top; the single peak at δ=12.25ppm is the peak of active hydrogen on -OH; the multi-peak at δ=6.99-8.15ppm is the peak of seven hydrogens on two benzene rings, which is consistent with the azo int...
Embodiment 2
[0037] Take 10g 16g of xylene, 3.4g of water, 3.4g of DEA additives and 1.0g of Ru-P were loaded into a 100mL reactor, hydrogen was passed through, and the reaction was carried out at 1.0MPa and 60°C until the hydrogen pressure remained constant. After the reaction, the temperature was lowered to obtain a brown-black reaction solution. Filter the reaction solution, remove the catalyst, separate the water layer, add absolute ethanol at a volume ratio of 1:1, and put it in ice water overnight, and filter to obtain 2.7g of light yellow crystals, that is, the ultraviolet absorber. The test results are shown in Table 1.
Embodiment 3
[0039] Take 10g 16g of xylene, 3.4g of water, 3.4g of DEA additives and 0.5g of Ru-P were loaded into a 100mL reactor, hydrogen was passed through until the hydrogen pressure remained constant, and the reaction was carried out at 1.5MPa and 60°C. After the reaction, the temperature was lowered to obtain a brown-black reaction solution. Filter the reaction liquid, remove the catalyst, extract to obtain the organic phase, add absolute ethanol at a volume ratio of 1:1, and spend the night in ice water, and filter to obtain 2.7 g of light yellow crystals, which are ultraviolet absorbers. The test results are shown in Table 1.
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