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

Active Publication Date: 2014-11-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] One of the technical problems to be solved by the present invention is that the catalyst existing in the prior art is easy to condense and self-polymerize due to the intermediate product under the condition of continuous hydrogenation in a fixed bed,

Method used

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  • Catalyst and method for preparing m-xylylenediamine by hydrogen isophthalonitrile

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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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Abstract

The invention relates to a catalyst and a method for preparing m-xylylenediamine by hydrogen isophthalonitrile and mainly solves the problem that in the prior art, a catalyst easily cokes and loses activity. The catalyst is composed of the follow components in parts by weight: (a) 5.0-40.0 parts of metallic nickel or nickel oxide, (b) 0.01-25.0 parts of at least one element or oxide of the element selected from the IIA column in the Periodic Table, (c) 0.01-10.0 parts of at least one of Mo, Zr, and Ti or oxide of Mo, Zr and Ti, (d) 0.01-10.0 parts of at least one of Sn, Fe, and Cu or oxide of Sn, Fe and Cu, (e) 0.01-10.0 parts of at least one element or oxide of the element selected from rare earth and (f) 9-95 parts of silicon dioxide carrier. By adopting the technical scheme, the problem is well solved and the catalyst can be used in the technical scheme for fixed bed continuous hydrogenation production of m-xylylenediamine.

Description

technical field [0001] The invention relates to a method for hydrogenation of nitrile hydrocarbons, in particular to a method which can be used for hydrogenation of isophthalonitrile to prepare m-xylylenediamine. Background technique [0002] m-Xylylenediamine is an important fine chemical raw material. It can be used in the production of special plastics and paints, and can also be used in the synthesis of pesticides, fiber finishing agents, antirust agents, chelating agents, lubricants and other products. A large number of reports have been reported on the synthesis of m-xylylenediamine by catalytic hydrogenation of isophthalonitrile, mainly by kettle-type indirect hydrogenation or fixed-bed continuous hydrogenation process. The tank-type indirect hydrogenation process mainly uses Raney Ni catalyst. The modified Raney Ni can be greatly improved in terms of activity, selectivity and stability, and is widely used in industrial production. The fixed-bed continuous hydrogena...

Claims

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Application Information

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IPC IPC(8): B01J23/83B01J23/887C07C211/27C07C209/48
Inventor 任杰王建强赵多刘仲能
Owner CHINA PETROLEUM & CHEM CORP
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