Preparation method of amine anti-aging agent
A solvent oil and catalyst technology, which can be used in the preparation of amino compounds from amines, chemical instruments and methods, and hydrogenation to hydrocarbons, etc. Improve the utilization rate of raw materials, reduce the three wastes, and optimize the effect of the synthesis process
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[0028] like figure 1 As shown, the present invention provides a preparation method of an amine antioxidant, comprising:
[0029] Step 1, carry out the alkylation reaction of α-methylstyrene, liquid diphenylamine and ion exchange resin catalyst;
[0030] Step 1 specifically includes:
[0031] In the reaction vessel, nitrogen is introduced to replace the air in the vessel, and α-methylstyrene, liquid diphenylamine, and ion exchange resin catalyst are added to carry out the alkylation reaction; wherein, the moles of α-methylstyrene and liquid diphenylamine are The ratio is (2.2~3.0):1, preferably (2.3~2.5):1; the ion exchange resin catalyst is a strong acid cation exchange resin, under the condition that the reaction temperature and solvent requirements are met, various types of commercially available Resin product; the amount of ion exchange resin catalyst added is 10% to 30% of the mass of α-methylstyrene, preferably 10% to 20%; the temperature of the alkylation reaction is 1...
Embodiment 1
[0058] In a 0.5L reactor with a stirring device, a condensation reflux device and a nitrogen protection device, use nitrogen to purge and replace the air in the reactor, put in 90g of liquid diphenylamine, 157.12g of α-methylstyrene and 20g of catalyst, Under nitrogen protection, the temperature was raised to 80°C, stirring was started and the temperature was continued to rise to 130°C. The raw material mixture was kept at this temperature for another 6 hours, then cooled to 107°C, and filtered while hot to obtain 221.3 g of filtrate. The filtrate was added to 400 g of 120# solvent oil at 5°C, fully stirred, and left to stand until the temperature of the 120# solvent oil dropped to 10°C, and then filtered to obtain a white crude product. Put the crude product into 400g of 120# solvent oil, fully disperse and let stand for 1h, and filter again to obtain a white finished product. After drying, the purity of the white product measured by gas chromatography was 98.3%, and the yiel...
Embodiment 2
[0060] In a 0.5L reactor with a stirring device, a condensation reflux device and a nitrogen protection device, use nitrogen to purge and replace the air in the reactor, put in 90g of liquid diphenylamine, 145g of α-methylstyrene and 40g of catalyst, under nitrogen Under the protection, the temperature was raised to 80°C, the stirring was started and the temperature was continued to rise to 120°C. The raw material mixture was kept at this temperature for another 4 hours, then cooled to 105°C, and filtered while hot to obtain 208.6 g of filtrate. The filtrate was added to 300 g of 120# solvent oil at 5°C, fully stirred, and left to stand until the temperature of the 120# solvent oil dropped to 10°C, and then filtered to obtain a white crude product. Put the crude product into 600g of 120# solvent oil, fully disperse and let stand for 1h, and filter again to obtain a white finished product. After drying, the purity of the white product measured by gas chromatography was 98.8%, a...
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