Carbon-based catalyst, preparation method thereof and catalyst system for dicyclopentadiene polymerization
A carbon-based catalyst, dicyclopentadiene technology, applied in the direction of chemical recycling, etc., can solve the problems such as the power supply of the coordination group is not as good as that of the phenoxy group, the catalyst utilization rate is low, and the specific surface area is small.
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[0034] The invention provides a method for preparing a carbon-based catalyst, comprising the following steps:
[0035] (1) Pre-activating the carbon carrier with an acid to obtain an activated carbon carrier;
[0036](2) impregnating the activated carbon support and the mixed solution of active components to obtain a carbon-based catalyst; the active components in the mixed solution of active components include transition metal oxychloride complexes.
[0037] The invention uses acid to activate and pretreat the carbon support to obtain the activated carbon support. The invention uses acid to activate and pretreat the carbon support to obtain the activated carbon support. In the present invention, the carbon carrier is preferably one or more of activated carbon, carbon black and mesoporous carbon; the specific surface area of the carbon carrier is preferably 500-3000m 2 / g, more preferably 1500-2000m 2 / g, the particle size is preferably 1 to 20 μm, more preferably 1 to 5 ...
Embodiment 1
[0064] Embodiment 1: Preparation of carbon-supported tungsten catalyst
[0065] (1) Under the condition of nitrogen protection, tert-butanol, WCl 6 , dry toluene mixed and stirred for 10h, wherein WCl 6 The dosage is 20g, the volume of toluene is 70mL, tert-butanol and WC1 6 Molar ratio is 0.25, obtains the reaction solution, WC1 in the reaction solution 6 and WOC1 4 The total concentration of 0.73mol / L, WC1 6 with WOCl 4 The molar ratio is 3:1.
[0066] (2) 11.1g of nonylphenol is added in 30 milliliters of toluene to obtain nonylphenol solution, and the nonylphenol solution is added in the reaction solution of step (1), then use N 2 The HCl was removed by bubbling for 1 hour, after which 10.1 g of 2,4-pentanedione was added by syringe, again with N 2 The HCl was removed by bubbling for 1 h to obtain a solution of mixed active ingredients.
[0067] (3) The activated carbon is activated and pretreated with 1mol / L nitric acid, the weight ratio of carbon support and nitr...
Embodiment 2
[0069] Embodiment 2: Preparation of carbon-supported molybdenum catalyst
[0070] (1) Under the condition of nitrogen protection, di-tert-butyl-p-cresol, MoCl 5 , dry toluene mixed and stirred for 10h, where MoCl 5 The dosage is 10g, the volume of toluene is 50mL, di-tert-butyl p-cresol and MoCl 5 Molar ratio is 0.25, obtains reaction solution, and in reaction solution MoCl 5 and MoOC1 3 The total concentration of 0.73mol / L, MoC1 5 with MoOCl 4 The molar ratio is about 3:1.
[0071] (2) 11.1g of nonylphenol is added in 30 milliliters of toluene to obtain a nonylphenol solution, and the nonylphenol solution is added to the reaction solution of step (1), then use N 2 The HCl was removed by bubbling for 1 hour, after which 10.1 g of 2,4-pentanedione was added by syringe, again with N 2 The HCl was removed by bubbling for 1 h to obtain a solution of mixed active ingredients.
[0072] (3) The activated carbon is activated and pretreated with 1mol / L acetic acid, the weight r...
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Abstract
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