Preparation method for metal-free catalyst used for hydrochlorination of acetylene to prepare vinyl chloride in fixed bed, and application method
A metal-free technology for acetylene hydrochlorination, which is applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, hydrogen halide addition preparation, etc., and can solve cumbersome preparation steps and harsh conditions. problems, to achieve the effects of simplifying the preparation process, reducing production costs, and clear structure
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Embodiment 1
[0041] (1) Add 10 g of coal-based carbon to 100 g of sulfuric acid solution with a mass concentration of 10%, stir at 85 °C for 8 h, then filter and separate the activated carbon, and wash it with deionized water until it is neutral. And the resulting filter cake was dried at 100 °C for 24 h to obtain sample A;
[0042] (2) Using atomic layer deposition (ALD) technology, at 120 °C, deionized water and the vapor of the precursor diethyl zinc were alternately passed through the ALD reaction tube equipped with sample A to uniformly deposit 5 Atomic layer Zn(OH) 2 thin layer, and then baked at 400 °C for 1.5 h in an argon atmosphere, and the Zn(OH) deposited on the surface of activated carbon 2 Converted to ZnO, cooled to room temperature to obtain sample B;
[0043] (3) Put 2 g of sample B into a 50 mL autoclave lined with polytetrafluoroethylene, and put 5 g of imidazole at the same time, then seal the autoclave and heat it at 180 °C for 24 h, then The obtained sample was was...
Embodiment 2
[0046] (1) Add 10 g of coconut shell carbon to 30 g of sulfuric acid solution with a mass concentration of 10%, stir at 85 °C for 8 h, then filter and separate the activated carbon, and wash it fully with deionized water until neutral. And the resulting filter cake was dried at 100 °C for 24 h to obtain sample A;
[0047] (2) Using atomic layer deposition (ALD) technology, under the condition of 120 ℃, deionized water and the vapor of the precursor diethyl zinc were alternately passed through the ALD reaction tube equipped with sample A, and uniformly deposited on the surface of sample A for 15 Atomic layer Zn(OH) 2 thin layer, and then baked at 400 °C for 1.5 h in an argon atmosphere, and the Zn(OH) deposited on the surface of activated carbon 2 Converted to ZnO, cooled to room temperature to obtain sample B;
[0048] (3) Put 2 g of sample B into a 50 mL autoclave lined with polytetrafluoroethylene, and put 5 g of benzimidazole at the same time, then seal the autoclave and ...
Embodiment 3
[0051] (1) Add 10 g of coal-based carbon to 50 g of sulfuric acid solution with a mass concentration of 10%, stir at 85 °C for 8 h, then filter and separate the activated carbon, and wash it with deionized water until it is neutral. And the resulting filter cake was dried at 100 °C for 24 h to obtain sample A;
[0052] (2) Using atomic layer deposition (ALD) technology, at 120 °C, deionized water and the vapor of the precursor diethyl zinc were alternately passed through the ALD reaction tube equipped with sample A to uniformly deposit 5 Atomic layer Zn(OH) 2 thin layer, and then baked at 400 °C for 1.5 h in an argon atmosphere, and the Zn(OH) deposited on the surface of activated carbon 2 Converted to ZnO, cooled to room temperature to obtain sample B;
[0053] (3) Put 2 g of sample B into a 50 mL autoclave lined with polytetrafluoroethylene, and put 5 g of 1-methylimidazole at the same time, then seal the autoclave and heat it at 180 °C After 24 h, the obtained sample was...
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