Method for activating adiponitrile hydrogenation catalyst

A technology of hydrogenation catalyst and activation method, which is applied in the field of activation of adiponitrile hydrogenation catalyst, can solve the problems of oxidation and dissolution reaction loss, catalyst surface loss, catalyst activity reduction, etc., and achieve the effect of reducing loss and large active specific surface area

Active Publication Date: 2014-08-13
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, Fe, Cr, Mo, Sn, W, etc. are commonly used as doping elements in the catalyst modification process, while catalyst activation generally uses a strong alkali solution, and the modifiers Cr, Mo, Sn, W in a strong Oxidation and dissolutio

Method used

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  • Method for activating adiponitrile hydrogenation catalyst

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Experimental program
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Effect test

Embodiment 1

[0025] 1. Preparation of modified Raney nickel catalyst:

[0026] The nickel-aluminum alloy that contains nickel is 50wt% is ground into 60-80 purpose powder, under ice-water bath condition, gets 100g and joins in the NaOH of 0.2mol / l, ammonium chloride, ammoniacal liquor mixed solution while stirring, its The molar ratio is 5:1:0.1; react at 20°C for 0.5h to partially dissolve the aluminum, remove the upper layer of lye and wash it with deionized water to neutrality, and then wash it several times with absolute ethanol; under the condition of 600w30000MHz microwave, Add the above powder into a mixed solution composed of ferric nitrate solution and chromium nitrate, wherein the molar ratio of iron to nickel is 0.01:1, and the molar ratio of chromium to nickel is 0.01:1; microwave heating to 80°C for hydrothermal aging for 1h , filtered and separated to obtain solid particles, after drying and roasting, hydrogen reduction was introduced at 0.1MPa500°C for 4h to obtain a modifie...

Embodiment 2

[0030] 1. Preparation of modified Raney nickel catalyst:

[0031] Grind the nickel-aluminum alloy containing 50wt% nickel into 60-80 mesh powder, take 100g and add it to 0.5mol / l NaOH, ammonium sulfate and ammonia mixed solution while stirring under ice-water bath condition, the mole The ratio is 10:1:1; react at 30°C for 1 hour to partially dissolve the aluminum, remove the upper layer of lye and wash it with deionized water until neutral, and then wash it several times with absolute ethanol; under microwave conditions, the above powder Add to the mixed solution composed of ferric nitrate solution and tin nitrate, wherein the molar ratio of iron to nickel is 0.02:1, and the molar ratio of tin to nickel is 0.02:1; microwave heating to 80°C for hydrothermal aging for 1h, filter and separate The obtained solid particles were dried and calcined, and then reduced by introducing hydrogen at 0.1 MPa at 500°C for 4 hours to obtain a modified Raney nickel catalyst.

[0032] 2. Cataly...

Embodiment 3

[0035] 1. Preparation of modified Raney nickel catalyst:

[0036] Grind the nickel-aluminum alloy containing 50wt% nickel into 60-80 mesh powder, take 100g and add it into 1mol / l NaOH, ammonium nitrate, ammonia water mixed solution while stirring under ice-water bath condition, the molar ratio The ratio is 7:1:0.3; react at 40°C for 1.5h to partially dissolve the aluminum, remove the upper layer of lye and wash with deionized water until neutral, and then wash with absolute ethanol several times; under the condition of 600w30000MHz microwave, the above Add the powder into a mixed solution composed of ferric nitrate solution and bismuth nitrate, wherein the molar ratio of iron to nickel is 0.05:1, and the molar ratio of bismuth to nickel is 0.05:1; microwave heating to 80°C for hydrothermal aging for 1h, filter The solid particles were separated, dried and calcined, and reduced by introducing hydrogen at 0.1 MPa at 500°C for 4 hours to obtain a modified Raney nickel catalyst. ...

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Abstract

The invention discloses a method for activating an adiponitrile hydrogenation catalyst. The method is characterized in that the catalyst is a modified raney nickel catalyst and is activated by the method comprising the following steps: preparing a mixing solution from iron, chromium, molybdenum, bismuth, manganese or tungsten soluble salts and NaOH respectively; slowly adding the modified raney nickel catalyst and ammonium salt; heating with microwave and reacting, and then washing; the modified raney nickel catalyst is prepared by the method comprises the following steps: grinding nickel-aluminum alloy into powder; adding to a mixing solution to dissolve part of aluminum, wherein the mixing solution is prepared through NaOH, ammonium salt and ammonium hydroxide in certain ratio; washing with deionized water and absolute ethyl alcohol; adding the powder to the mixing solution consisting of ferric nitrate and a modifier under a microwave condition and reacting to obtain a solid; drying and roasting the solid; and then charging hydrogen and reducing to obtain the modified raney nickel catalyst. With the adoption of the method for activating the adiponitrile hydrogenation catalyst, the prepared catalyst is relatively large in specific surface area, loss of the modifier is small, and high conversion rate of adiponitrile and high selectivity of hexamethylenediamine are achieved in the adiponitrile catalytic hydrogenation process.

Description

technical field [0001] The invention belongs to the technical field of petrochemical catalysis, and in particular relates to an activation method of adiponitrile hydrogenation catalyst. Background technique [0002] Raney catalyst is a widely used reduction catalyst, mainly used in the catalytic hydrogenation of organic compounds. According to the different metal active centers, there are Raney iron, Raney cobalt, Raney nickel, etc. Among them, the Raney nickel catalyst with nickel as the active center is the most widely used. For example, hexamethylenediamine is used as a monomer for the production of nylon-66. At present, adiponitrile is mainly used as a raw material, and Raney nickel catalyst is used to prepare it in a tank reactor or a fluidized bed reactor. At present, the main problems of this catalyst are low activity and selectivity, large amount of catalyst, and serious environmental pollution. Therefore, it is necessary to develop new and more efficient catalyst m...

Claims

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Application Information

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IPC IPC(8): B01J25/04B01J25/02B01J37/34C07C209/48C07C211/12
CPCY02P20/584
Inventor 耿玉侠杨克俭刘文杨琦武刘淼张津辉杨磊
Owner CHINA TIANCHEN ENG
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