A kind of hydrogenation preparation method of petroleum resin
A technology for preparing petroleum resin and hydrogen, which is applied in the preparation field of saturated petroleum resin, can solve the problems of high price of Pt catalyst and high hydrogenation cost, and achieve the effects of reducing production cost, high hydrogenation efficiency and reducing process steps.
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Embodiment 1
[0030] Add 50mL chlorobenzene solvent in 100mL reactor, dissolve 20g of dicyclopentadiene petroleum resin; Take 0.15mg of metallocene compound titanocene dichloride, dissolve in 5mL chlorobenzene, add n-butyllithium reagent 0.002mmol (butadiene The molar ratio of the lithium-based reagent to the metallocene compound is 3:1) to form a catalyst solution; add the catalyst solution to the dicyclopentadiene petroleum resin solution and mix evenly, fully replace the air in the kettle with hydrogen, and then press the hydrogen to Charge to 3.0MPa, start to heat up, and start stirring. Control the heating rate to 60°C / h. Control the reaction temperature to 140°C and react for 3 hours. After the reaction, the solvent and other non-polymers are flashed off to obtain a hydrogenated dicyclopentadiene petroleum resin product.
[0031] The index analysis of the product shows that the resin yield reaches 95%, the hue is ≤1, the softening point is 115°C, and the bromine value is ≤3.
Embodiment 2
[0033] Add 30mL of chlorobenzene solvent into a 100mL reaction kettle to dissolve 20g of dicyclopentadiene petroleum resin; take 0.35mg of metallocene compound dichlorozirconocene, dissolve it in 5mL of chlorobenzene, add 0.0024mmol of ethyllithium reagent (butyl The molar ratio of the lithium reagent to the metallocene compound is 2:1) to form a catalyst solution; add the catalyst solution to the dicyclopentadiene solution and mix evenly, fully replace the air in the kettle with hydrogen, and then fill the hydrogen pressure to 5.0 MPa, start to heat up, start stirring. Control the heating rate to 60°C / h. Control the reaction temperature to 120°C and react for 4 hours. After the reaction, the solvent and other non-polymers are flashed off to obtain a hydrogenated dicyclopentadiene petroleum resin product.
[0034] The index analysis of the product shows that the resin yield reaches 94%, the hue is ≤1, the softening point is 118°C, and the bromine value is ≤3.
Embodiment 3
[0036]Add 70mL of chlorobenzene solvent into a 100mL reactor to dissolve 20g of dicyclopentadiene petroleum resin; take 0.10mg of metallocene compound dichloromethylene bridged titanocene, dissolve it in 5mL of chlorobenzene, add n-butyl lithium Reagent 0.0016mmol (the molar ratio of butyllithium reagent to metallocene compound is 4:1) is configured as a catalyst solution; the catalyst solution is added to the dicyclopentadiene solution and mixed evenly, and the air in the kettle is fully replaced with hydrogen, and then Fill the hydrogen pressure to 4.5MPa, start to heat up, and start stirring. Control the heating rate to 60°C / h. Control the reaction temperature to 100°C and react for 4h. After the reaction is finished, the solvent and other non-polymers are flashed off to obtain a hydrogenated dicyclopentadiene petroleum resin product.
[0037] The index analysis of the product shows that the resin yield reaches 95%, the hue is ≤1, the softening point is 122°C, and the bro...
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