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Preparation method and application of Co/Ni and aluminum pyrophosphate composite hollow microsphere

A technology of aluminum pyrophosphate and aluminum phosphate, which is applied in the field of preparation of hollow microspheres, can solve the problems of no hollow microsphere catalysts, difficulty in uniform dispersion of catalysts, and high unit consumption of product catalysts, and achieve uniform size, smooth surface, and selectivity high effect

Active Publication Date: 2014-09-24
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The densities of these catalysts are greater than 6.7g / cm 3 , which will bring about two problems: the catalyst is not easy to disperse evenly in the reaction system, resulting in low catalyst efficiency and high unit consumption of the product catalyst; the design of a reactor with a certain production capacity requires a large size, resulting in high cost
The main problem with the preparation of hollow microspheres by the current template method is that the template is easy to cause the rupture of the sphere and the collapse of the structure during the removal process.
And also do not find the report that hollow microsphere catalyst is used for preparing IPDA at present

Method used

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  • Preparation method and application of Co/Ni and aluminum pyrophosphate composite hollow microsphere
  • Preparation method and application of Co/Ni and aluminum pyrophosphate composite hollow microsphere
  • Preparation method and application of Co/Ni and aluminum pyrophosphate composite hollow microsphere

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Preparation of Solution A: Weigh 500g of distilled water, add 4g of 85% H 3 PO 4 Adjust its pH value to about 2; weigh 9.15g Ni (NO 3 ) 2 and 91.5gCo(NO 3 ) 2 Add to pH ≈ 2 phosphoric acid aqueous solution, stir to dissolve. Preparation of solution B: weigh 53.25gAl(NO 3 ) 3 and 30gNaH 2 PO 4 Add to 400g distilled water, stir to dissolve. Preparation of Solution C: Weigh 39.9g of urea and 55g of diethylenetriamine into 500g of distilled water, stir to dissolve. Heat the 2L autoclave (Weihai Chemical Machinery Equipment Co., Ltd.) and set the temperature to 120°C. When the temperature in the autoclave reaches 120°C, inject solution B into the autoclave with an advection pump (Beijing Satellite Manufacturing Factory), and stir The speed is 348 rpm, and the reaction is 5 minutes; then put the solutions A and C into the autoclave at the same time, after the feeding is completed, react at 120°C for 5 hours, then stop heating, wait until the temperature in the kettl...

Embodiment 2

[0044] Preparation of Solution A: Weigh 500g of distilled water, add 4g of 85% H 3 PO 4 Adjust its pH value to about 2; weigh 8.28gNi(CH 3 COO) 2 and 125g Co(CH 3 COO) 2 Add to pH ≈ 2 phosphoric acid aqueous solution, stir to dissolve. Preparation of Solution B: Weigh 120g Al(NO 3 ) 3 and 74.4g (NH 4 ) 2 HPO 4 Add to 500g distilled water, stir to dissolve. Preparation of Solution C: Weigh 60.2g of urea and 80.8g of triethylenetetramine into 500g of distilled water, stir to dissolve. Heat the 2L autoclave (Weihai Chemical Machinery Equipment Co., Ltd.) and set the temperature to 150°C. When the temperature in the autoclave reaches 150°C, inject solution B into the autoclave with an advection pump (Beijing Satellite Manufacturing Factory), and stir The speed is 492 rpm, and the reaction is 7 minutes; then put the solutions A and C into the autoclave at the same time, after the feeding is completed, react at 150°C for 4 hours, then stop heating, wait until the temperat...

Embodiment 3

[0046] Preparation of Solution A: Weigh 500g of distilled water, add 4g of 85% H 3 PO 4 Its pH value is adjusted to about 2; Weigh 16.6gNi (NO 3 ) 2 and 166gCo(NO 3 ) 2 Add to pH ≈ 2 phosphoric acid aqueous solution, stir to dissolve. Preparation of solution B: weigh 193.2gAl(NO 3 ) 3 and 123.4gKH 2 PO 4 Add to 500g distilled water, stir to dissolve. Preparation of Solution C: Weigh 126.8g of urea and 120.1g of tetraethylenepentamine into 500g of distilled water, stir to dissolve. Heat the 2L autoclave (Weihai Chemical Machinery Equipment Co., Ltd.) and set the temperature to 180°C. When the temperature in the autoclave reaches 180°C, inject solution B into the autoclave with an advection pump (Beijing Satellite Manufacturing Factory), and stir The speed is 564 rpm, and the reaction is 10 minutes; then put the solutions A and C into the autoclave at the same time, after the feeding is completed, react at 180°C for 4 hours, then stop heating, wait until the temperatur...

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Abstract

The invention relates to a preparation method of a Co / Ni and aluminum pyrophosphate composite hollow microsphere. The preparation method comprises the following steps of: preparing a mixed water solution A which contains 10wt%-25wt% of cobalt salt and 1wt%-3.5wt% of nickel salt; preparing a mixed water solution B of aluminum salt and phosphate; preparing a mixed water solution C of vinylamine and carbamide; firstly adding the mixed water solution B to a reaction kettle, then simultaneously adding the mixed water solution A and the mixed water solution C to the reaction kettle, and reacting to obtain a Co / Ni hydroxide and aluminum phosphate composite microsphere; filtering, washing, drying, and then calcinating to obtain a CoO / NiO and aluminum pyrophosphate composite hollow microspher; reducing the CoO / NiO and aluminum pyrophosphate composite hollow microspher by using H2 or CO to obtain the Co / Ni and aluminum pyrophosphate composite hollow microsphere. The whole preparation process flow is simple and can be put into industrial production easily. The prepared Co / Ni and aluminum pyrophosphate composite hollow microsphere is used for catalyzing ammoniation and hydrogenation of IPN (Interpenetrating Polymer Network) to prepare IPDA (Isophorone Diamine), is high in catalysis efficiency and has the IPDA selectivity being higher than 98%.

Description

Technical field: [0001] The invention relates to a preparation method and application of hollow microspheres, in particular to a preparation method of Co / Ni and aluminum pyrophosphate composite hollow microspheres and its use as a catalyst for preparing IPDA by ammoniation 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. [0003] At present, the commonly used catalysts for preparing IPDA are composite oxides mainly composed of cobalt oxide, related patents such as EP0742045A1 and CN1675166; and Raney-Co (Raney-Co), related patents su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J35/08C07C211/36C07C209/48
Inventor 王磊初乃波黎源叶飞王同济易光铨
Owner WANHUA CHEM GRP CO LTD
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