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Catalyst and method for preparing m-xylylenediamine by hydrogenation of isophthalonitrile

A technology of isophthalonitrile and metaxylylenediamine is applied in the field of nitrile hydrocarbon hydrogenation, which can solve the problems of catalyst coking and deactivation, and achieve the effects of improving reaction activity, enhancing stability and prolonging life.

Active Publication Date: 2016-11-30
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, resulting in the coking and deactivation of the catalyst. A new isophthalonitrile is provided A catalyst for hydrogenation to prepare m-xylylenediamine, which has the advantages of strong anti-coking ability, high activity and selectivity, and good stability

Method used

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  • Catalyst and method for preparing m-xylylenediamine by hydrogenation of isophthalonitrile
  • Catalyst and method for preparing m-xylylenediamine by hydrogenation of isophthalonitrile
  • Catalyst and method for preparing m-xylylenediamine by hydrogenation of isophthalonitrile

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Experimental program
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Embodiment 1

[0029] 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

[0031] 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 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 oReduction at C for 24 hours yielded metallic Ni / SiO 2 Catalyst, denoted as catalyst C2. ...

Embodiment 3

[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 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 hydrogenating isophthalonitrile, which mainly solves the problem that the catalyst is easily coked and deactivated in the prior art. The present invention comprises the following components in parts by weight: (a) 5.0-40.0 parts of metallic nickel or its oxides; (b) 0.01-25.0 parts selected from the periodic table of elements At least one element or oxide thereof in A; (c) 0.01-10.0 parts are selected from at least one element or oxides thereof in Mo, Zr and Ti; (d) 0.01-10.0 parts are selected from Sn, Fe and Cu (e) 0.01 to 6.0 parts of at least one element or its oxides selected from rare earths; (f) 9 to 95 parts of carrier silicon dioxide The technical scheme solves the problem of This problem can be applied to the process of producing m-xylylenediamine by continuous hydrogenation of fixed bed.

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 using 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 hydrog...

Claims

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Application Information

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