Method for preparing N,N-dimethyl cyclohexylamine
A technology of dimethylcyclohexylamine and cyclohexylamine, which can be used in the preparation of reductive alkylation, chemical instruments and methods, purification/separation of amino compounds, etc. The problems of low amine yield and complex dimethylamine recovery and utilization can achieve the effects of reasonable acidity distribution, less side reactions, and high product yield.
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[0045] Example 1
[0046] 1# Modified carrier preparation:
[0047] Weigh 95g of hydrogen type ZSM-5 (with a silicon-to-aluminum ratio of 100), mix magnesium nitrate hexahydrate with 100ml of deionized water to prepare an impregnation solution containing 5g of magnesium oxide (that is, magnesium nitrate can eventually be oxidized to 5g of magnesium oxide), and then heat To form a uniform solution at 80℃, add the weighed hydrogen type ZSM-5 to the dipping solution, immerse it at 80℃ for 12h, and bake it in an oven at 110℃ for 12h; finally move to the muffle furnace, in an air atmosphere It is heated at 3°C / min to 400°C for 8h and calcined to obtain a modified carrier containing 5% MgO+95% hydrogen type ZSM-5.
[0048] 1# Preparation of supported palladium-based catalyst precursor:
[0049] Prepare a nitrate impregnation solution containing 6g palladium, 0.5g cobalt, and 0.2g zinc with 100ml deionized water, heat it to 80℃ to form a homogeneous solution, add 93.3g 1# modified carrier, ...
Example Embodiment
[0050] Example 2
[0051] 2# Modified carrier preparation:
[0052] Weigh 90g of hydrogen type ZSM-5 (with a silicon-to-aluminum ratio of 400), mix barium nitrate hexahydrate with 150ml of deionized water to prepare an immersion solution containing 10g of barium oxide, and then heat to 75°C to form a uniform solution. Hydrogen type ZSM-5 was added to the impregnation solution, immersed at 75°C for 12h, and baked in an oven at 120°C for 12h; finally moved to a muffle furnace, heated at 3°C / min to 450°C for 8h in an air atmosphere, A modified carrier containing 10% BaO+90% hydrogen type ZSM-5 is prepared.
[0053] 2# Preparation of supported palladium-based catalyst precursor:
[0054] Prepare a nitrate impregnation solution containing 4g palladium, 0.5g ruthenium, and 0.05g iron with 100ml deionized water, heat it to 80℃ to form a homogeneous solution, then add 95.45g 2# modified carrier, immerse it at 80℃ for 12h, and then Bake in an oven at 120°C for 12h; finally move to a muffle f...
Example Embodiment
[0055] Example 3
[0056] 3# Modified carrier preparation:
[0057] Weigh 95g of hydrogen type ZSM-5 (with a silicon-to-aluminum ratio of 200), mix magnesium nitrate hexahydrate and barium nitrate hexahydrate with 100ml deionized water to prepare an impregnation solution containing 3g magnesium oxide and 2g barium oxide, and then heat to 90°C to form To homogenize the solution, add the weighed hydrogen type ZSM-5 to the dipping solution, immerse it at 90℃ for 24h, and bake it in an oven at 110℃ for 12h; finally move it to the muffle furnace and place it at 3℃ in an air atmosphere. The temperature is increased to 500°C per minute and calcined for 8 hours to prepare a modified carrier containing 3% MgO + 2% BaO + 95% hydrogen type ZSM-5.
[0058] 3# Preparation of supported palladium-based catalyst precursor:
[0059] Use 200ml of deionized water to prepare a nitrate impregnation solution containing 15g of palladium, 0.1g of ruthenium, 0.1g of cobalt, and 0.4g of cerium, and heat to 80...
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