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Catalyst for preparing salicylonitrile as well as preparation method and application thereof

A catalyst, salicylonitrile technology, applied in the field of catalysis, can solve problems such as complex process, large amount of organic waste water, and high pressure on environmental protection, and achieve the effects of inhibiting decarboxylation reaction, prolonging service life, and high selectivity

Active Publication Date: 2021-04-27
CAC NANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest problem in the industrialization of this process is the need to use a large amount of solvents such as N-methylpyrrolidone and N,N-dimethylformamide (N,N-Dimethylformamide, DMF), which leads to a large amount of organic waste water, high production costs, and high pressure on environmental protection.
The third method is to use o-cresol as a raw material through etherification and ammoxidation, the process is complicated and the yield is low
[0005] Disclosed in CN108816256A is a preparation method for a catalyst for synthesizing salicylonitrile, comprising the following steps: (1) at 30°C-70°C, adding a phosphorus source into water to stir and dissolve, and sieving the calcium source in batches Add it; after filtering and washing, dry at 90°C-150°C, pulverize and sieve to obtain the precursor powder; (2) add the auxiliary agent to the sieved precursor powder and mix evenly, then add deionized water, Extrude to obtain a shaped catalyst precursor, dry to constant weight; (3) put the shaped catalyst precursor in a muffle furnace, and raise the temperature to 500°C-600°C at a heating rate of 2°C-5°C / min and keep it warm for 3 -7h, the catalyst for the synthesis of salicylonitrile, the catalyst described in this scheme is only suitable for the catalytic process of using salicylic acid as a raw material to synthesize salicylonitrile, and it is used to catalyze methyl salicylate as a raw material to prepare salicylonitrile. process, the catalytic activity is low

Method used

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  • Catalyst for preparing salicylonitrile as well as preparation method and application thereof
  • Catalyst for preparing salicylonitrile as well as preparation method and application thereof
  • Catalyst for preparing salicylonitrile as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Catalyst preparation method:

[0068] (1) Dissolve 168g of oxalic acid in 1500mL of water to obtain an oxalic acid solution, heat the temperature of the obtained oxalic acid solution to 85°C, and then add 56.8g of P 2 o 5 , 44.88g of Al 2 o 3 and 13.92g of B 2 o 3 Dissolve in gained oxalic acid solution, fully stir, dissolve completely, then slowly add 322.8g silica sol (SiO in silica sol) under stirring condition 2 The mass percentage composition is 40wt%) mix, obtain mixed solution;

[0069] (2) 23.28gCo(NO 3 ) 2 ·6H 2 O was dissolved in 100ml of water to obtain cobalt nitrate solution, and 16.16g KNO 3 Dissolve in 100ml of water to obtain a potassium nitrate solution; then add the cobalt nitrate solution and the potassium nitrate solution to the mixed solution in step (1), stir and mix to obtain a mixture slurry, then heat and evaporate to a solid content of 35wt.%, to obtain Viscous slurry, the viscous slurry is sprayed into shape, then dried at 120°C for ...

Embodiment 2

[0072] The composition of the catalyst described in this embodiment is P 1.0 al 1.1 B 0.7 K 0.2 co 0.1 o m / SiO 2 ; Wherein, the mass percentage of the carrier is 50%;

[0073] The difference between the preparation method of the catalyst described in this example and Example 1 is that the P 2 o 5 、Al 2 o 3 , B 2 o 3 , Co(NO 3 ) 2 ·6H 2 O and KNO 3 The proportioning that makes gained catalyst satisfy above-mentioned composition, other conditions are compared with embodiment 1 and are identical.

Embodiment 3

[0075] The composition of the catalyst described in this embodiment is P 1.0 al 1.1 B 0.6 K 0.2 co 0.1 o m / SiO2 ; Wherein the mass percentage of the carrier is 50%;

[0076] The difference between the preparation method of the catalyst described in this example and Example 1 is that the P 2 o 5 、Al 2 o 3 , B 2 o 3 , Co(NO 3 ) 2 ·6H 2 O and KNO 3 The proportioning that makes gained catalyst satisfy above-mentioned composition, other conditions are compared with embodiment 1 and are identical.

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Abstract

The present invention relates to a catalyst for preparing salicylonitrile, a preparation method and an application thereof, the catalyst comprises a carrier and an active component, the composition general formula of the active component is P1.0 AlaBbXcYdOm, and X is any one or a combination of at least two selected from lithium, sodium, potassium or cesium, Y is selected from any one or a combination of at least two of calcium, magnesium, barium, manganese, iron, cobalt, nickel, lead, molybdenum, tungsten or rare earth elements; wherein a is 0.5-2, b is 0.05-0.8, c is 0.01-0.7, d is 0.01-0.2, and m is the number of oxygen atoms required for meeting element valence balance in the active component; the catalyst provided by the invention has excellent catalytic performance and selectivity to salicylonitrile, the conversion rate of catalyzing conversion of methyl salicylate is greater than 98%, and the selectivity to salicylonitrile is greater than 94%.

Description

technical field [0001] The invention belongs to the field of catalysis, and relates to a catalyst for preparing salicylonitrile, a preparation method and application thereof. Background technique [0002] Salicylonitrile, also known as o-hydroxybenzonitrile, is slightly soluble in water and unstable to strong alkalis or strong oxidants. As a pharmaceutical intermediate, salicylonitrile is mainly used to produce Bunirolol hydrochloride, and as a pesticide intermediate, it is mainly used to produce the methoxyacrylate fungicide azoxystrobin. Salicylonitrile can also be used as an intermediate for some perfumes and liquid crystal materials. [0003] At present, the processes for synthesizing salicylonitrile mainly include the following three types. The first one is to generate salicylonitrile by one-step dehydration of salicylamide. The selection of dehydrating agent has become the biggest problem in the industrial production of this process. At present, triphosgene and Thion...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185C07C253/22C07C255/53
CPCB01J27/1853C07C253/22C07C255/53Y02P20/584
Inventor 李强王海波刘庆郝德新
Owner CAC NANTONG CHEM
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