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Catalyst for synthesizing para-hydroxy-benzonitrile and its preparing method and use

A technology for p-hydroxybenzonitrile and catalyst is applied to the catalyst for synthesizing p-hydroxybenzonitrile and the fields of preparation and use thereof, which can solve problems such as lack of catalyst stability, and achieve small molar ratio, selectivity and yield The effect of high and good application prospects

Inactive Publication Date: 2006-08-23
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the bibliographical reports of the direct ammoxidation of p-cresol to produce p-hydroxybenzonitrile, the highest yield is 63-63.4mol%, and its catalyst is Fe 3 co 6 NiBiPMo 12 o x / SiO 2 and Bi 9 PMo 12 o 52 / SiO 2 , the reaction temperature is 370~380°C, but there is no record about catalyst stability (Martin A. et al, DD232693(1986.))

Method used

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  • Catalyst for synthesizing para-hydroxy-benzonitrile and its preparing method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Catalyst preparation

[0026] 3.6gCrO 3 , 1.2g (NH 4 ) 6 Mo 7 o 24 4H 2 O and 33.8g H 3 PO 4 Add deionized water to prepare a solution, and then add 3.1g FeCl to the solution 3 ·6H 2 O, 1.5 g Na 2 O, 0.8gK 2 O was carefully heated to make it a transparent solution, and then 40 g of calcined fine-grained SiO 2 (produced by Qingdao Ocean Chemical Co., Ltd.) was added to the above transparent solution, stirred evenly, dried at 373K, and then activated at 823K for 6 hours to obtain the required catalyst.

[0027] P-Hydroxytoluene Ammoxidation

[0028] In a quartz tube reactor with an internal diameter of 40mm, add 80ml of catalyst, after the temperature is raised to 633K, the reaction mixture is continuously sent into the reaction mixture at a molar ratio of p-cresol: ammonia: air: steam = 1: 1.2: 20: 10. and collect the reaction mixture from the outlet. After the catalyst was used continuously for 50...

Embodiment 2

[0030] Catalyst preparation

[0031] 6.5gCrO 3 , 1.5g (NH 4 ) 6 Mo 7 o 24 4H 2 O and 50.1 g H 3 PO 4Add deionized water to prepare a solution, and then add 4.1g K to the solution 2 O, 6.1 g FeCl 3 ·6H 2 O was carefully heated to make it a transparent solution, and then 40 g of calcined fine-grained SiO 2 (produced by Qingdao Ocean Chemical Co., Ltd.) was added to the above transparent solution, stirred evenly, dried at 373K, and then activated at 733K for 8 hours to obtain the required catalyst.

[0032] P-Hydroxytoluene Ammoxidation

[0033] In a quartz tube reactor with an internal diameter of 40mm, add 80ml of catalyst, after the temperature is raised to 633K, the reaction mixture is continuously sent into the reaction mixture at a molar ratio of p-cresol: ammonia: air: steam = 1: 1.2: 20: 10. and collect the reaction mixture from the outlet. After the catalyst was used continuously for 50 hours, ...

Embodiment 3

[0035] Catalyst preparation

[0036] 1.8gCrO 3 , 1.2g (NH 4 ) 6 Mo 7 o 24 4H 2 O and 16.1 g H 3 PO 4 Add deionized water to prepare a solution, and then add 0.3g Na to the solution 2 O, 0.75gK 2 O, carefully heated to make it a transparent solution, and then calcined 40g of fine particle SiO 2 (produced by Qingdao Ocean Chemical Co., Ltd.) was added to the above transparent solution, stirred evenly, dried at 433K, and then activated at 753K for 3 hours to obtain the required catalyst.

[0037] P-Hydroxytoluene Ammoxidation

[0038] In a quartz tubular reactor with an internal diameter of 40 mm, add 80 ml of catalyst, and after the temperature is raised to 633 K, the reaction mixture is continuously sent into the reaction mixture at a molar ratio of p-cresol: ammonia: air: water vapor=1: 1.3: 10: 5. and collect the reaction mixture from the outlet. After the catalyst was used continuously for 50 hours,...

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Abstract

The catalyst for synthesizing para-hydroxy-benzonitrile includes main catalyst and co-catalyst. The main catalyst has active matters MoO3, Cr2O3 and P2O5 in the atom ratio of Mo:Cr:P=1:1.3-10:15-75; and the co-catalyst has active matter of at least one of the oxide of Fe, Ti, Bi, Sb, Li, Na, K, Rb and Cs, and the atom ratio to Mo of 0.1-11. Using the catalyst of the present invention in ammoxidation process to synthesie para-hydroxy-benzonitrile has high product selectivity and yield, long catalyst service life, small ammonia ratio and excellent application foreground.

Description

technical field [0001] The invention relates to a special composite oxide supported catalyst for synthesizing p-hydroxybenzonitrile (p-HBN) by ammoxidation of p-cresol (p-CRL) and its preparation method and application. Background technique [0002] p-HBN is the important organic intermediate ( Fred C.L. et al, J. Org. Chem., 1974, 39(23), 3416-3418). It is widely used in the production of fine chemicals. [0003] Regarding the synthesis of p-HBN, the more method reported in the literature is the aldehyde or aldoxime method (Dewan, Sharwan K. et al, Synthetic Communications (2004), 34 (11), 2025-2029; Dewan, Sharwan K.; Singh , Ravinder.Synthetic Communications (2003), 33(17), 3085-3088.) and ethyl p-hydroxybenzoate (EHB) ammonolysis method (Ueno A et al, Patent 0074116(1981)). Since p-hydroxybenzaldehyde is obtained by liquid-phase oxidation of p-cresol as a raw material under alkaline conditions, the process route is long and the production cost is relatively high. The...

Claims

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Application Information

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IPC IPC(8): B01J27/188B01J27/14B01J32/00B01J37/02C07C253/02C07C255/36
Inventor 马玉龙廖振宇
Owner WUHAN UNIV
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