Catalyst and method for preparing m-xylylenediamine by hydrogen isophthalonitrile
A technology of isophthalonitrile and m-xylylenediamine, which is applied in the field of nitrile hydrocarbon hydrogenation, can solve problems such as catalyst coking and deactivation, and achieve the effects of improving reaction activity, preventing coking and high nickel content
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Embodiment 1
[0030] With nitric acid in [H + ] / [SiO 2 ] Under the condition that the molar ratio is 0.25, the 100gSiO 2 Peptized for 24 hours to obtain SiO 2 Sol, keep the temperature of the sol at 40 o c. An aqueous solution containing 92 g of magnesium nitrate was added to the SiO 2 In the sol, add the aqueous solution containing 94g nickel nitrate to SiO 2 In the sol, add the aqueous solution containing 5.6g zirconium nitrate, the aqueous solution containing 4.5g copper nitrate and the aqueous solution containing 4.6g lanthanum nitrate successively at last, and the temperature is raised to 100 o C aging, keep for 24 hours. After aging, the powder was obtained by filtration, and then passed through 80 o C drying to obtain the corresponding catalyst precursor. catalyst precursor at 400 o C roasting for 4 hours to obtain oxidized NiO / SiO 2 catalyst. Catalyst in 1.5 L / min pure hydrogen flow, at 450 o Reduction at C for 24 hours yielded metallic Ni / SiO 2 Catalyst, denoted as cat...
Embodiment 2
[0033] With nitric acid in [H + ] / [SiO 2 ] Under the condition that the molar ratio is 0.25, the 100gSiO 2 Peptized for 24 hours to obtain SiO 2 Sol, keep the temperature of the sol at 40 o c. An aqueous solution containing 92 g of magnesium nitrate was added to the SiO 2 In the sol, add the aqueous solution containing 94g nickel nitrate to SiO 2 In the sol, add the aqueous solution containing 13.8g ammonium molybdate, the aqueous solution containing 4.5g copper nitrate and the aqueous solution containing 4.6g lanthanum nitrate successively at last, and be warming up to 100 o C aging, keep for 24 hours. After aging, the powder was obtained by filtration, and then passed through 80 oC drying to obtain the corresponding catalyst precursor. catalyst precursor at 400 o C roasting for 4 hours to obtain oxidized NiO / SiO 2 catalyst. Catalyst in 1.5 L / min pure hydrogen flow, at 450 o Reduction at C for 24 hours yielded metallic Ni / SiO 2 Catalyst, denoted as catalyst C2. ...
Embodiment 3
[0036] With nitric acid in [H + ] / [SiO 2 ] Under the condition that the molar ratio is 0.25, the 100gSiO 2 Peptized for 24 hours to obtain SiO 2 Sol, keep the temperature of the sol at 40 o c. An aqueous solution containing 92 g of magnesium nitrate was added to the SiO 2 In the sol, add the aqueous solution containing 94g nickel nitrate to SiO 2 In the sol, add 60.0g titanium tetrachloride, the aqueous solution containing 9.0g copper nitrate and the aqueous solution containing 4.6g lanthanum nitrate successively at last, then be warming up to 100 o C aging, keep for 24 hours. After aging, the powder was obtained by filtration, and then passed through 80 o C drying to obtain the corresponding catalyst precursor. catalyst precursor at 400 o C roasting for 4 hours to obtain oxidized NiO / SiO 2 catalyst. Catalyst in 1.5 L / min pure hydrogen flow, at 450 o Reduction at C for 24 hours yielded metallic Ni / SiO 2 The catalyst is denoted as catalyst C3. The catalyst composi...
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