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Rare-earth oxide modified high-selectivity catalyst for adiponitrile hydrogenation and hexylenediamine production, preparation method and application thereof

A rare earth metal, high-selectivity technology, applied in the direction of metal/metal oxide/metal hydroxide catalyst, preparation of organic compounds, preparation of amino compounds, etc. High mechanical strength, reduced environmental pollution, mild reaction conditions

Inactive Publication Date: 2019-04-19
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the coexistence of hexamethylenediamine and 6-aminocapronitrile in the product cannot achieve the high selectivity of the targeted product hexamethylenediamine

Method used

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  • Rare-earth oxide modified high-selectivity catalyst for adiponitrile hydrogenation and hexylenediamine production, preparation method and application thereof
  • Rare-earth oxide modified high-selectivity catalyst for adiponitrile hydrogenation and hexylenediamine production, preparation method and application thereof
  • Rare-earth oxide modified high-selectivity catalyst for adiponitrile hydrogenation and hexylenediamine production, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Prepare a certain concentration of nickel nitrate, aluminum nitrate and cerium nitrate metal salt precursors, and mix them uniformly by ultrasonic to form a mixed solution A. Sodium carbonate solution B with pH = 11 was prepared in deionized water. Under constant temperature and stirring conditions of 45°C, the above two clear solutions A and B were dripped into deionized water side by side, and the dropping speed was controlled to be 3 s / drop. Continue to adjust with sodium carbonate solution until pH=10. After aging for 8 hours, filter, wash, and dry at 110°C for 10 hours with deionized water and methanol, and roast the ground powder in a tube furnace at 400°C for 4 hours to obtain a catalyst precursor. Catalyst precursor in H 2 / Ar mixed gas at 400°C for 6 h to obtain catalyst powder. figure 1 Exhibit 2wt% CeO 2 X-ray diffraction (XRD) pattern of the modified nickel-based catalyst. figure 2 Exhibit 2wt% CeO 2 Modified Ni-based catalyst samples (2%) in NH 3 Te...

Embodiment 2

[0032] 2.5g of adiponitrile, 25ml of absolute ethanol and reduction pretreated 0.5g of CeO 2 The mass percentage is 2wt% Ni / CeO 2 / Al 2 o 3 Add the catalyst into a 50ml high-pressure closed reaction kettle, and replace the air in the kettle with hydrogen for 2-3 times. The stirring speed is 800rpm, and the reaction time is 3h. image 3 and Figure 4 Demonstration of 2wt% CeO after pretreatment 2 Modified Ni / CeO 2 / Al 2 o 3 Transmission electron micrograph of the catalyst. See Table 1 below for Ni / CeO under different reaction conditions 2 / Al 2 o 3 Test results for liquid-phase catalytic hydrogenation of adiponitrile.

[0033] Table 1 2wt% CeO at different reaction temperatures 2 Modified Ni / CeO 2 / Al 2 o 3 Test results of liquid-phase catalytic hydrogenation of adiponitrile

[0034]

Embodiment 3

[0036] 2.5g of adiponitrile, 25ml of absolute ethanol and reduction pretreated 0.5g of CeO 2 The mass percentage is 1wt% Ni / CeO 2 / Al 2 o 3 Catalyst The catalyst is added to a 50ml high-pressure reaction kettle, and the air in the kettle is replaced with hydrogen for 2-3 times. The stirring speed is 800 rpm, the reaction time is 3 h, the reaction temperature is 90° C., the hydrogen pressure is 7 MPa, the conversion rate of adiponitrile is 100%, and the selectivity of hexamethylenediamine is 70%. High-purity hexamethylenediamine can be obtained after distillation and purification under reduced pressure.

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Abstract

The invention discloses a rare-earth oxide modified high-selectivity catalyst for adiponitrile hydrogenation and hexylenediamine production, a preparation method and application thereof. An alumina-supported nickel-based catalyst is used as an active component, and at 25-90 DEG C and through a parallel flow precipitation process, a low-content rare-earth oxide is used for the modification. A tankreactor is adopted at the low temperature and without an alkaline reagent to carry out a reaction at the pressure of 1-9 MPa for 1-6 h so as to achieve adiponitrile catalytic conversion for high-selectivity preparation of hexylenediamine. No alkaline reagent or NH3 is added during the reaction process to inhibit side reaction of cyclization. The environmental pollution is reduced; and the catalysthas high mechanical strength, the reaction post-treatment is simple and the reaction condition is relatively mild. According to the method and in part of the embodiments, the conversion rate of adiponitrile reaches up to 100% according to set reaction parameters, and selectivity of the product hexylenediamine can reach up to 90%. The invention has good economic benefit and industrial applicationprospects.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and in particular relates to a rare earth metal oxide-modified high-selectivity catalyst for the hydrogenation of adiponitrile to hexamethylenediamine and a preparation method thereof, which is based on a nickel-based catalyst supported by alumina. The components are modified by co-current precipitation with low content rare earth metal oxides. Using a tank reactor, adiponitrile is subjected to a liquid-phase catalytic hydrogenation reaction at a relatively low temperature and without an alkaline reagent to prepare the target product hexamethylenediamine with high selectivity. Background technique [0002] Catalytic hydrogenation of nitriles is an important industrial route to prepare a variety of amines, and the products of hydrogenation of nitriles are mainly composed of a mixture of primary, secondary and tertiary amines. Among them, hexamethylenediamine (HMD), as an importa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83C07C209/48C07C211/12
CPCB01J23/002B01J23/83C07C209/48C07C211/12
Inventor 梁长海张春兴罗靖洁陈霄
Owner DALIAN UNIV OF TECH
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