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Catalyst for synthesis of acetonitrile by ammoniation of acetic acid and preparation method thereof

A catalyst, a technology for chemical synthesis, which is applied in physical/chemical process catalysts, chemical instruments and methods, and ammonia-carboxylic acid reaction preparation, etc., can solve the problems of increasing the cost of ammonia gas recovery, large amount of ammonia gas, and high reaction temperature, and achieves The effect of improving coking, catalyst activity and selectivity, and stability

Pending Publication Date: 2021-10-01
CHINA TIANCHEN ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] However, the reaction conditions used in the above patents are generally above 350°C, the reaction temperature is high, and the amount of ammonia gas is large, which increases the cost of subsequent ammonia gas recovery, and some patents do not describe the impurities in the reaction in detail

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Mix the powder obtained by neutralizing aluminum sulfate and sodium metaaluminate with pseudo-boehmite at a mass ratio of 80:20 to make glue, and then mix it with a certain amount of zinc nitrate, lanthanum nitrate and Tianqing powder , and then use the oily ammonia column to form pellets with a diameter of 3 mm, and activate the pellets at 400 ° C for 8 hours in an air atmosphere to obtain porous spherical alumina containing zinc oxide and lanthanum oxide. The above-mentioned alumina was subjected to hydration treatment, the hydration treatment temperature was 70° C., and the treatment time was 10 hours. After the treatment was completed, it was dried at 200° C. for 5 hours to obtain the finished catalyst. The mass ratio of alumina to zinc oxide and lanthanum oxide is 100:5:5, and the mass ratio of alumina to Tianqing powder is 100:10. The specific surface area of ​​the obtained catalyst is 310m 2 / g, the bulk density is 0.6g / ml, the pore volume is 0.65cc / g, the pore ...

Embodiment 2

[0049] Mix the powder obtained by neutralizing aluminum sulfate and sodium metaaluminate with pseudo-boehmite at a mass ratio of 70:30 to make gel, and then mix it with a certain amount of manganese nitrate, ferrous nitrate and polyethylene glycol Mix evenly, and then use the oily ammonia column to form pellets with a diameter of 3mm, activate and roast the pellets in an air atmosphere at 450°C for 6 hours to obtain porous spherical alumina containing manganese oxide and ferrous oxide. The above-mentioned alumina was subjected to hydration treatment, the hydration treatment temperature was 50°C, the treatment time was 2h, and after the treatment was completed, it was dried at 300°C for 2h to obtain the finished catalyst. Wherein the mass ratio of aluminum oxide to manganese oxide and ferrous oxide is 100:1:10, and the mass ratio of aluminum oxide to polyethylene glycol is 100:5. The specific surface area of ​​the obtained catalyst is 350m 2 / g, the bulk density is 0.55g / ml, t...

Embodiment 3

[0052] Mix the powder obtained by neutralizing aluminum sulfate and sodium metaaluminate with pseudo-boehmite at a mass ratio of 90:10 to make glue, and then mix it with a certain amount of chromium nitrate, cerium nitrate and polyvinyl alcohol evenly , and then use the oily ammonia column balling method to make small balls with a diameter of 2 mm, activate and roast the small balls in an air atmosphere at 500 ° C for 2 hours, and obtain porous spherical alumina containing chromium oxide and cerium oxide. The above-mentioned alumina was subjected to hydration treatment, the hydration treatment temperature was 70° C., and the treatment time was 10 hours. After the treatment was completed, it was dried at 200° C. for 5 hours to obtain the finished catalyst. The mass ratio of alumina to zinc oxide and lanthanum oxide is 100:2:8, and the mass ratio of alumina to polyvinyl alcohol is 100:7. The specific surface area of ​​the obtained catalyst is 380m 2 / g, the bulk density is 0.5g...

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Abstract

The invention provides a catalyst for synthesis of acetonitrile by ammoniation of acetic acid and a preparation method thereof. The catalyst is porous spherical alumina containing transition metal or rare earth metal oxide, and the crystal form of alumina is a mixed crystal phase of one or two of gamma type or delta type. The preparation method comprises the following steps of: mixing powder prepared by neutralizing aluminum sulfate and sodium metaaluminate with pseudo-boehmite, then mixing the obtained mixture with transition metal, rare earth metal salts and a pore-enlarging agent, preparing small balls by using an oil ammonia column balling method, activating and roasting to obtain porous spherical aluminum oxide containing transition metal and rare earth metal oxide, and then hydrating the obtained aluminum oxide and drying to obtain the catalyst. A small amount of transition metal, rare earth metal and other auxiliaries are added in the preparation process of the catalyst, so that the stability of the catalyst is improved, the catalytic reaction temperature is greatly reduced, the coking condition of the catalyst is improved, the service life of the catalyst is prolonged, and the activity and selectivity of the catalyst are improved.

Description

technical field [0001] The invention belongs to the field of catalysts, in particular to a catalyst for ammoniating acetic acid to synthesize acetonitrile and a preparation method thereof. Background technique [0002] Acetonitrile, also known as methyl nitrile, is an important chemical raw material. Because acetonitrile has a special functional group nitrile group, as a solvent, it not only has the characteristics of ethanol, methanol and other solvents, but also has better distribution ratio and desorption ability than alcohols, and has high dielectric strength and dipole moment. , so it can be an excellent solvent for inorganic and organic compounds. Since high-purity acetonitrile does not absorb ultraviolet rays at 200nm-400nm, it can be used as a solvent for high-performance liquid chromatography (HPLC), and the analytical sensitivity can be as high as 10 -9 class. With the popularization of this testing technology, the demand for high-purity acetonitrile of chromato...

Claims

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Application Information

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IPC IPC(8): B01J23/10B01J23/755B01J23/889B01J35/10C07C253/22C07C255/03B01J35/08
CPCB01J23/002B01J23/10B01J23/8892B01J23/755C07C253/22B01J2523/00B01J35/51B01J35/615B01J35/635B01J35/647B01J2523/27B01J2523/31B01J2523/3706B01J2523/72B01J2523/842C07C255/03
Inventor 史文涛王聪刘新伟庄大为崔艳杰曹立杨琦武刘大李崔志国
Owner CHINA TIANCHEN ENG
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