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Novel N-methyl aniline catalyst synthesized through chromium-free gas phase method

A methylaniline and catalyst technology, applied in the field of new catalysts, can solve the problems of chromium pollution, chromium pollution of downstream products, etc., and achieve the effect of high conversion rate, selectivity and high strength

Active Publication Date: 2013-04-10
NANJING ZUNLONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chromium pollution not only exists in catalyst production, but also in catalyst use process and downstream products

Method used

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  • Novel N-methyl aniline catalyst synthesized through chromium-free gas phase method
  • Novel N-methyl aniline catalyst synthesized through chromium-free gas phase method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: 365g of copper nitrate, 392g of zinc nitrate, 47.8g of magnesium nitrate, 21.3g of barium nitrate and 6.3g of cerium nitrate were dissolved in 1L of water, heated to 50°C, 650g of sodium bicarbonate was dissolved in 3L of water, and heated to 70°C, then slowly drop the sodium bicarbonate solution into the mixed solution of nitrate, and stir rapidly at the same time until pH = 7.5. Raise the temperature to 80°C and stir for 1 hour, then filter and wash, and dry the solid material at 120°C 6 hours, bake at 300°C for 2 hours, then add 2% graphite and 4% water and mix evenly, and press it into a tablet of Ф5×(4.5-5.5) mm with a tablet machine. Points (calculated as oxides) 48% copper, 43% zinc, 3% magnesium, 5% barium, 1.% cerium.

Embodiment 2

[0019] Dissolve 350g of copper nitrate, 338g of zinc nitrate, 143g of magnesium nitrate, 27.7g of barium nitrate and 9.5g of cerium nitrate in 1L of water, heat to 50°C, dissolve 500g of sodium carbonate in 3L of water, and heat to 70°C, then dissolve the sodium carbonate Slowly add dropwise to the mixed solution of nitrate, and stir rapidly at the same time until pH = 7.5. Heat up to 80°C and stir for 1 hour, then filter and wash, dry the solid material at 120°C for 6 hours, and roast at 300°C for 2 hours hours, then add 1% graphite and 4% water and mix evenly, and press it into a tablet of Ф5×(4.5-5.5) mm with a tablet machine, so that the components in the catalyst (calculated as oxides) are 46% Copper, 37% zinc, 9% magnesium, 6.5% barium, 1.5% cerium.

Embodiment 3

[0020] Example 3: Dissolve 289g copper nitrate, 401g zinc nitrate, 95.5g magnesium nitrate, 44.7g barium nitrate, 9.5g cerium nitrate in 1L water, heat to 50°C, dissolve 500g sodium carbonate in 3L water, and heat to 70°C , then slowly add the sodium carbonate solution dropwise into the mixed solution of nitrates, and at the same time stir rapidly until the pH=7.5. Raise the temperature to 80°C and stir for 1 hour, then filter and wash, and dry the solid material at 120°C for 6 hours. Calcined at 300°C for 2 hours, then added graphite and 2% water, mixed evenly, and pressed into a tablet of Ф5×(4.5-5.5) mm with a tablet machine, the components in the catalyst (calculated as oxides) ) 38% copper, 44% zinc, 6% magnesium, 10.5% barium, 1.5% cerium.

[0021] The performance comparison of embodiment catalyst and comparative example catalyst:

[0022] Evaluation method: The laboratory device completely simulates the large-scale industrial production device. The reactor is a Ф32 sta...

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Abstract

The invention belongs to the technical field of catalyst, and relates to a novel catalyst used for producing N-methyl aniline through the stationary bed reaction of aniline and methyl alcohol in gas phase method. The catalyst does not contain chrome, and the catalyst contains the following components by weight (accounted by oxide): 30 to 70 percent of copper, 10 to 50 percent of zinc, 5 to 20 percent of alkaline-earth metals, and 0.2 to 2 percent of rare earth element cerium or lanthanum. According to the invention, the catalyst does not contain chrome, so that not only the chrome pollution in the production process of the catalyst is reduced, but also the chrome pollution in the use process of the catalyst and down-stream products is reduced; and when N-methyl aniline is produced by using the catalyst, N,N-methyl toluidine generated in the reaction is rather low in content. The property of the catalyst can reach or surpass that of the products used in current industrial devices, the strength is high, and the conversion ratio as well as the selectivity is high. The working condition of the catalyst is that the pressure is normal pressure, the mole ratio of methyl alcohol and aniline is 1.5 to 1, and the liquid hourly space velocity is 0.6 h<-1>.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and relates to a novel catalyst used for producing N-methylaniline by gas-phase fixed-bed reaction of aniline and methanol. The catalyst does not contain chromium, which not only reduces the chromium pollution in the production of the catalyst, but also reduces the chromium pollution in the catalyst use process and downstream products; when using this catalyst to produce N-methylaniline, the N,N-2 The content of methylaniline is extremely low. Background technique [0002] It is a mature and advanced process to produce N-methylaniline by the gas phase method of a tubular fixed bed reactor. It has a history of nearly 30 years in China. At present, the catalysts used in domestic industrial devices are copper, zinc, and chromium cylinders. Tablet catalyst, stable performance, widely used models include CNW-1 and QC-5, etc. [0003] [0004] The chromium element in copper zinc chromium acts as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83C07C209/60C07C211/48
Inventor 郝云青邹运湖
Owner NANJING ZUNLONG CHEM
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