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Supported nickel-based catalyst and its preparation method and use

A nickel-based catalyst, supported technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. It is difficult to remove catalysts and other problems to achieve the effect of slowing down deactivation, improving conversion rate, and achieving significant effects.

Inactive Publication Date: 2013-04-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But from a theoretical point of view, we realize that most of the active centers of Raney nickel are located inside the catalyst. Even if high-speed stirring can remove the oxide layer on the surface of Raney nickel particles, it is difficult to remove the nickel oxide deposited in the micropores inside the particles and make the The catalyst remains active; in addition, the exfoliation of the oxide layer as a result of high-speed agitation seems to accelerate the oxidation of Raney nickel and hinder its reuse

Method used

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  • Supported nickel-based catalyst and its preparation method and use
  • Supported nickel-based catalyst and its preparation method and use
  • Supported nickel-based catalyst and its preparation method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-6

[0039] Preparation of activated carbon-supported nickel-based catalysts by impregnation method:

[0040] Pretreatment of the carrier: 1g of activated carbon (110-130 mesh, specific surface area 770m 2 ﹒ g -1 ) in a nitrogen atmosphere at 600°C for 6 hours to obtain treated activated carbon;

[0041] Precursor preparation: impregnate the treated activated carbon in 20ml of a mixed aqueous solution containing nickel nitrate and ammonium molybdate additives, wherein the mass of nickel in nickel nitrate is 5% of the mass of activated carbon (that is, nickel content), ammonium molybdate The mass of molybdenum in the medium is 1% of the mass of the activated carbon, and it is impregnated at 20 °C for 8 hours to prepare the Ni-Mo / AC catalyst precursor;

[0042] Catalyst reduction: The Ni-Mo / AC catalyst precursor was vacuum dried at 120°C for 6h, calcined at 800°C for 6h in a nitrogen atmosphere, and then reduced with hydrogen at 600°C for 10h to finally obtain the desired activate...

Embodiment 7-18

[0047] To evaluate the activity of the synthesized catalyst, the steps are as follows:

[0048] According to the mass ratio of phthalic anhydride: phthalide (reaction solvent): Ni5Mo1AC catalyst is 20g: 40g: 0.2g, add 100ml of high-pressure stirring reaction kettle in turn, replace the air with 1MPa nitrogen three times, then raise the temperature to 180°C, start stirring, and feed The hydrogen pressure was maintained at 4.0 MPa, and the reaction was terminated after 4 hours. After the reaction, let it cool down to 120°C, open the kettle, and heat filter to recover the catalyst. It was detected that the conversion rate of phthalic anhydride was 93.5%, and the yield of phthalide was 83.3%. The product was washed with 10% sodium carbonate solution and filtered. Then vacuum rectify the product at -0.09MPa (column size 3cm×70cm, triangular pyramid stainless steel packing), collect 40-80°C fraction; finally increase the vacuum to -0.097MPa, and further distill out the low boiling ...

Embodiment 19-21

[0055] The service life of the synthesized Ni-Mo / AC, Ni-Mn / AC and Ni-Fe / AC catalysts was evaluated in a high-pressure stirred reactor, and the steps were as follows:

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Abstract

The invention discloses a supported nickel-based catalyst and its preparation method and use. The supported nickel-based catalyst adopts active carbon as a carrier and the carrier carries one or more assistants and one of nickel and a nickel oxide, wherein the one or more assistants are selected from elemental iron, elemental manganese, elemental molybdenum, iron oxides, manganese oxides, and molybdenum oxides. The supported nickel-based catalyst is prepared by a dipping method, is convenient for operation and has a low cost. In a phthalic anhydride hydrogenation reaction for preparation of phthalide, the supported nickel-based catalyst has an anti-acid activity, can be recycled 5-7 times, and has activity decay less than 7%. In a phthalic anhydride one-step catalytic hydrogenation reaction for preparation of phthalide, the supported nickel-based catalyst has a high catalytic activity and a phthalic anhydride conversion ratio of 93.5 to 100% and a phthalide yield of 83.3 to 93.9%. Therefore, the supported nickel-based catalyst is obviously superior to the prior art and has obvious effects.

Description

technical field [0001] The invention relates to the field of catalytic hydrogenation of fine chemical industry, in particular to a supported nickel-based catalyst, a preparation method thereof and an application in catalytic hydrogenation of phthalic anhydride to prepare phthalide. Background technique [0002] Phthalide (o-hydroxymethylbenzoic acid lactone, English name Phthalide) is an important fine chemical intermediate, which is widely used in anticoagulant drugs phenylindanedione, phenylthiazine, anxiolytics and many more Production of Lupine, laxatives and fungicide tetrachlorophthalide, etc. In addition, it can also be used in the synthesis of dye intermediates 1,4-dichloroanthraquinone and 1-chloroanthraquinone. [0003] In the prior art, the process route of preparing phthalide by catalytic hydrogenation of phthalic anhydride (phthalic anhydride, English name o-Phthalic anhydride) is generally adopted, and a gold-based catalyst suitable for this catalytic reaction...

Claims

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Application Information

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IPC IPC(8): B01J23/883B01J23/889C07D307/88
CPCY02P20/584
Inventor 魏作君顾运江李振斌刘迎新
Owner ZHEJIANG UNIV
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