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Method of preparing catalyst camied by composite oxides and application

A technology for supporting catalysts and composite oxides, which is used in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, hydrocarbon ammoxidation preparation, etc. Problems such as low selectivity, to achieve the effect of high atomic utilization, small environmental impact, and few reaction steps

Inactive Publication Date: 2007-09-05
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Liu Lin and Ma Yulong once used cobalt salt and manganese salt commonly used in liquid phase oxidation as catalysts to carry out the research on the synthesis of PTBN by liquid phase ammoxidation of PTT (Liu Lin, Ma Yulong. Journal of Wuhan University (Natural Science Edition) 2002, 48 (2 ): 167-170), the results show that the catalyst is also difficult to recycle, and the selectivity of the ammoxidation reaction rate and PTBN is still low,

Method used

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  • Method of preparing catalyst camied by composite oxides and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Catalyst preparation

[0030] 1. Add 4g CoCl 2 ·6H 2 O, 4.5g NiCl 2 ·6H 2 O is added into deionized water to prepare a solution; 2. Add 2.8g (NH 4 ) 6 Mo 7 o 24 4H 2 O and 1g Na 2 O, heated in a water bath (about 333K) to make it a transparent solution; 3. 40g of calcined fine particle SiO 2 (produced by Qingdao Ocean Chemical Co., Ltd.) was added to the above-mentioned transparent solution, and stirred evenly; 4. After drying at 373K, it was activated at 823K for 8 hours to obtain the required catalyst, and its atomic ratio was Co 3 o 4 :NiO:MoO 2 :Na 2 O=1:3.38:2.83:2.89.

[0031] Liquid-phase ammoxidation of p-tert-butyltoluene

[0032] Add 172.2g (1.164mol) p-tert-butyltoluene and 5g catalyst into the autoclave, tighten the lid symmetrically, control the temperature at 453K, and feed air and ammonia with the material ratio of air:ammonia as 13:1.0 , and use an oxygen detector to track and detect the oxygen content in the tail gas online. After reacti...

Embodiment 2

[0034]Catalyst preparation

[0035] 4g CoCl 2 ·6H 2 O, 4.5g NiCl 2 ·6H 2 O was added into deionized water to prepare a solution, and then 2.8 g (NH 4 ) 6 Mo 7 o 24 4H 2 O and 1.6g LiCl, carefully heated to make it a transparent solution of active components, and then calcined 40g fine particle SiO 2 (produced by Qingdao Ocean Chemical Co., Ltd.) join in the above-mentioned solution and stir evenly, activate then, its activation condition is identical with embodiment 1, atomic ratio is Co 3 o 4 :NiO:MoO 2 : Li 2 O=1:3.38:2.83:3.36.

[0036] Liquid-phase ammoxidation of p-tert-butyltoluene

[0037] In the autoclave described in Example 1, add 5 g of catalysts prepared by the method described in this example, 172.2 g (1.164 mol) of p-tert-butyltoluene, and control the same reaction conditions as in Example 1 to react for 10 hours. The product was separated by the same method, the conversion rate of p-tert-butyltoluene was 54%, and the selectivity of p-tert-butylbenz...

Embodiment 3

[0039] Catalyst preparation

[0040] 4g CoCl 2 ·6H 2 O, 4.5g NiCl 2 ·6H 2 O was added to deionized water to prepare a solution, and 4 g of FeCl was added to the solution 3 and 1g Na 2 O, carefully heated to make it a transparent solution of active components, and then calcined 40g fine particle SiO 2 (produced by Qingdao Ocean Chemical Co., Ltd.) join in the above-mentioned solution and stir evenly, activate then, its activation condition is identical with embodiment 1, atomic ratio is Co 3 o 4 :NiO:Fe 2 o 3 :Na 2 O=1:3.38:1.32:3.36.

[0041] Liquid-phase ammoxidation of p-tert-butyltoluene

[0042] Add 5 g of catalysts prepared by the method described in this example, and the rest are the same as in Example 1. The conversion rate of p-tert-butyltoluene is 50.5%, and the selectivity of p-tert-butylbenzonitrile is 93.56%.

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Abstract

A carried composite oxide catalyst is prepared through dissolving the Co, Ni and cocatalyst in water or organic solvent, immersing the calcined carrier in it, baking, and activating. The used catalyst can be re-activated for cyclic used. Its application is also disclosed.

Description

technical field [0001] The invention relates to a preparation method of a composite oxide supported catalyst, and also relates to an application in the preparation of p-tert-butylbenzonitrile. technical background [0002] Aromatic nitrile is an important intermediate for the synthesis of dyes, pesticides, medicines, and various materials, and has a wide range of uses. At present, the most simple and economical method for synthesizing aromatic nitrile compounds is to use toluene and its derivatives as raw materials in the presence of a catalyst and to synthesize them in one step by gas-phase ammoxidation. However, the reaction temperature of gas-phase ammoxidation is generally between 400 and 500°C. There are not many toluene derivatives and methyl-containing heterocyclic derivatives that can withstand such high temperatures. The common ones are toluene, chlorotoluene and picolines, etc., and most toluene derivatives (such as tert-butyl-substitute...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J37/02B01J23/74C07C253/28
Inventor 马玉龙冯俊刘琳
Owner WUHAN UNIV