Method for preparing m-xylylenediamine from m-phthalodinitrile through hydrogenation

A technology for producing m-xylylenediamine and isophthalonitrile, which is applied in the field of nitrile hydrocarbon hydrogenation, can solve the problems of unsatisfactory product selectivity, large amount of catalyst, high temperature or pressure, and achieves improvement of reaction operation period, prolongation of Longevity and effect of improving stability

Active Publication Date: 2014-01-29
CHINA PETROLEUM & CHEM CORP +1
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  • Claims
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AI Technical Summary

Benefits of technology

This patented process describes how certain chemical substances called Ni (nickel) atoms form tiny clusters that help them mix together better than other molecules like iron or copper. These clusterings create spaces where there're many smaller metal particles around each particle, allowing it to move freely within these areas without losing its effectiveness due to their own weight. By adding this type of atomized solid solution into an organosiloxane fluid containing water vapor at low temperatures, they become very stable when mixed properly. They also have holes inside, making them ideal carriers for transporting reactants and targets during reactions. Overall, this new technology allows for efficient use of expensive materials while maintaining desired properties such as enhanced performance and increased efficiency in various industries involved in producing ammonia from urea synthesis processes.

Problems solved by technology

This patented technical problem addressed in this patents relates to improving the efficiency and effectiveness of chemical syntheses involving hydroformylations between different types of molecules called phynolds (isomers). Current methods involve expensive metal catalyst systems like palladium nickels, while newer materials like iron nitroxide could be cheaper without sacrificial effects on performance.

Method used

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  • Method for preparing m-xylylenediamine from m-phthalodinitrile through hydrogenation

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Experimental program
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Embodiment 1

[0014] Using aluminum sol with a solid content of 5% alumina as the carrier precursor, keep the temperature of the sol at 40 o c. Dissolve nickel nitrate in an appropriate amount of water to obtain a 0.5 g / ml nickel salt solution. Add an appropriate amount of nickel salt solution and ammonium molybdate alkaline solution with a molybdenum content of 4 wt.% to the aluminum sol to adjust the pH of the nickel-aluminum sol to ~9. o After aging for 24 hours at C, the gel was filtered, washed and dried to obtain the corresponding catalyst precursor. catalyst precursor at 100 o C roasting for 1 hour, 200 o C roasting 2h, 450 o C was calcined for 4 hours to obtain the oxidized catalyst, which was recorded as catalyst 1~3. The physical and chemical properties of the catalysts are listed in Table 1.

[0015]

Embodiment 2

[0017] Using aluminum sol with a solid content of 5% alumina as the carrier precursor, keep the temperature of the sol at 40 o c. Add a certain amount of cerium nitrate hexahydrate directly to the aluminum sol and stir for 1 hour. Dissolve nickel nitrate in an appropriate amount of water to obtain a 0.5 g / ml nickel salt solution. Add an appropriate amount of nickel salt solution and molybdenum content of 4wt.% ammonium molybdate alkaline solution to the sol, adjust the nickel aluminum sol pH ~ 9, at 90 o After aging for 24 hours at C, the gel was filtered, washed and dried to obtain the corresponding catalyst precursor. catalyst precursor at 100 o C roasting for 1 hour, 200 o C roasting 2h, 450 o C was calcined for 4 hours to obtain an oxidized catalyst, which was designated as catalyst 4. The physical and chemical properties of the catalysts are listed in Table 1.

[0018]

[0019] Table 1 Main physicochemical properties of catalysts 1-5

[0020]

Embodiment 3

[0025] Catalyst 1 is packed in the 80ml adiabatic bed hydrogenation reactor, and the reduction process condition that adopts is: in hydrogen atmosphere, under the pressure 0.2MPa condition, with 40 o The rate of C / h raises the temperature of the bed to 250 o C and maintained for 5h, then 10 o C / h heat up to 380 o C, maintain 10h, and then use 10 o C / h heat up to 450 o C, maintained for 12h, then cooled to the reaction temperature.

[0026] The reaction process conditions are: methanol / toluene / triethylamine is used as the reaction solvent, the reaction pressure is 7MPa, the inlet temperature is 70 o C, raw material space velocity 1.5h -1 Under the condition of running 300h. The conversion rate of isophthalonitrile is 100%, and the average selectivity of m-xylylenediamine is 95%.

[0027]

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Abstract

The invention relates to a method for preparing m-xylylenediamine from m-phthalodinitrile through hydrogenation, and mainly solves the problems of high catalyst consumption, high cost, unideal product selectivity, intermittent operation of a high-pressure autoclave and the like in the prior art. The technical scheme of the method is as follows: a nickel-based catalyst with centralized pore distribution is used and comprises the following components in percentage by weight: a) 30-70 parts of nickel or oxide thereof; b) 2-8 parts of molybdenum or oxide thereof; and c) 22-68 parts of supporter aluminum oxide, wherein the specific surface area of the catalyst is 150-300 m<2>/g, the pore volume is 0.3-0.8 ml/g, and the pore volume of 5-10 nm accounts for 80-90% of the total pore volume; and the most probable pore size distribution is in the position of 6-10 nm. Thus, the problems are well solved. The method can be used for industrial production of m-xylylenediamine preparation from m-phthalodinitrile through hydrogenation.

Description

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Claims

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Application Information

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Owner CHINA PETROLEUM & CHEM CORP
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