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Method for preparing eggshell type Co-Ni-Fe@SiO2 catalyst, prepared catalyst and application thereof

A technology of co-ni-fesio2 and co-ni-feoxsio2, which is applied in the field of preparation of eggshell-type Co-Ni-FeSiO2 catalysts, can solve the problem of weak combination of active components and supports, poor catalyst stability, and high catalyst costs and other problems, to achieve the effect of reducing catalyst cost, good stability and small bulk density

Active Publication Date: 2015-11-11
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest disadvantage of this type of catalyst is: 1. The bulk density is about 2.7g / cm 3 , causing the reactor to bear a considerable load; 2. During the activation process, only the surface layer is activated, the depth is generally about 100-150 μm, and there is a large amount of active component Co (existing in the form of Co-Al alloy) only as a support , the utilization rate is low, and the cost of the catalyst is increased; 3. A large amount of alkaline waste liquid containing heavy metals is produced during the cleaning of the Raney cobalt catalyst. Generally, about 30 tons of waste water is produced by preparing 1 t of Raney cobalt catalyst
At present, the main problem of using this method to prepare catalysts is that the active components are not firmly combined with the carrier, and the active components are easily lost during use, and the stability of the catalyst is poor.

Method used

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  • Method for preparing eggshell type Co-Ni-Fe@SiO2 catalyst, prepared catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Such as figure 1 As shown, put 100g of B-type silica gel pellets into a quartz reaction tube with an inner diameter of 20mm, and the temperature of the reaction tube is 160°C; use N 2 Purging the silica gel pellets, the flow rate is 200ml / min (N 2 The linear velocity in the reaction tube is 1.06cm / s), and the time is 120min.

[0046] 6.61gCoCl 2 , 0.33gNiCl 2 , 0.62gFe(NO 3 ) 3 Add to vaporizer. The temperature of the vaporizer is 87°C, and the N 2 Switch to the gasification pipeline system, use a flow rate of 100ml / min(N 2 The linear velocity in the reaction tube is 0.53cm / s) N 2 The molten Co, Ni, Fe salts are brought into the reaction tube to chemically react with the silica gel pellets.

[0047] After the Co, Ni, and Fe salts in the gasification tank are all brought into the reaction system, at 350°C, the flow rate of 100ml / min N 2 Roast in the atmosphere for 30min; then at 500°C, the flow rate is 50ml / min (NH 3 The linear velocity in the reaction tube is...

Embodiment 2

[0052] Put 100g of B-type silica gel beads into a quartz reaction tube with an inner diameter of 20mm, and the temperature of the reaction tube is 200°C; use N 2 Purging the silica gel pellets, the flow rate is 300ml / min (N 2The linear velocity in the reaction tube is 1.59cm / s), and the time is 180min.

[0053] 9.92gCoCl 2 , 0.74gNiCl 2 , 1.38gFe(NO 3 ) 3 Add to vaporizer. The temperature of the vaporizer is 90°C, and the N 2 Switch to the gasification pipeline system, use a flow rate of 150ml / min(N 2 The linear velocity in the reaction tube is 0.796cm / s) N 2 The molten Co, Ni, Fe salts are brought into the reaction tube to chemically react with the silica gel pellets.

[0054] After the Co, Ni, and Fe salts in the gasification tank are all brought into the reaction system, at 400°C, the flow rate of 150ml / min N 2 Roasting in atmosphere for 45min; then at 500°C, the flow rate is 75ml / min (NH 3 The linear velocity in the reaction tube is 0.398cm / s) NH 3 Roasting in a...

Embodiment 3

[0059] Put 100g of B-type silica gel beads into a quartz reaction tube with an inner diameter of 20mm, and the temperature of the reaction tube is 260°C; use N 2 Purging the silica gel pellets, the flow rate is 460ml / min (N 2 The linear velocity in the reaction tube is 2.44cm / s), and the time is 240min.

[0060] 12.12gCoCl 2 , 1.21gNiCl 2 , 2.26gFe(NO 3 ) 3 Add to vaporizer. The temperature of the gasification tank is 120°C, and the N 2 Switch to the gasification pipeline system, use a flow rate of 200ml / min(N 2 The linear velocity in the reaction tube is 1.06cm / s) N 2 The molten Co, Ni, Fe salts are brought into the reaction tube to chemically react with the silica gel pellets.

[0061] After the Co, Ni, and Fe salts in the gasification tank are all brought into the reaction system, at 450°C, the flow rate of 100ml / min N 2 Roast in the atmosphere for 60min; then at 600°C, the flow rate is 100ml / min 3 Roasting in the atmosphere for 240min.

[0062] Add 402.7g of dis...

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Abstract

The invention relates to a method for preparing an eggshell type Co-Ni-Fe@SiO2 catalyst, the prepared catalyst and application thereof. The method comprises the following steps: using N2 to take molten Co salt, Ni salt and Fe salt into a reaction tube filled with dry spherical silica gel to perform chemical vapor deposition reaction; first performing roasting in N2 and then performing roasting in NH3 to obtain Co-Ni-FeOx@SiO2; and then using H2 or CO to perform reduction to obtain Co-Ni-Fe@SiO2. The active components Co, Ni and Fe of the catalyst are in high in strength of bonding with a carrier, are not liable to loss and are small in bulk density; the catalyst is applied to IPN catalysis to prepare IPDA through ammoniation hydrogenation, the catalytic efficiency is high, the IPDA selectivity can be as high as 98.8%, and the selectivity for a decyanation product is lower than 0.48%.

Description

Technical field: [0001] The present invention relates to the preparation method of eggshell type catalyst and the prepared catalyst and its application, specifically eggshell type Co-Ni-FeSiO 2 The preparation method of the catalyst and the use of the catalyst prepared according to the method as a catalyst for the preparation of IPDA by the hydrogenation and hydrogenation of IPN. Background technique: [0002] 3-Aminomethyl-3,5,5-trimethylcyclohexylamine (isophoronediamine, referred to as IPDA) is a raw material for the preparation of isophorone diisocyanate, polyamide, etc., and can also be used as an epoxy resin Hardener. It is usually composed of 3-cyano-3,5,5-trimethylcyclohexanone (isophorone nitrile, referred to as IPN), NH 3 and H 2 It can be obtained through ammoniation and hydrogenation under the action of a hydrogenation catalyst. Commonly used hydrogenation catalysts are Raney cobalt and shaped cobalt or ruthenium catalysts. [0003] Raney cobalt catalyst is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755C07C209/48C07C209/26C07C211/36
Inventor 王磊初乃波王同济叶飞杨立超周游易光铨詹吉山黎源华卫琦
Owner WANHUA CHEM GRP CO LTD