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Method for preparing 3,5-dimethyl aniline

A technology of dimethylphenol and catalyst, which is applied in 3 fields and can solve problems such as unsatisfactory 3,5-dimethylaniline technology

Active Publication Date: 2012-10-17
EAST CHINA UNIV OF SCI & TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In summary, the existing technology for preparing 3,5-dimethylaniline is not satisfactory, and there is still room for improvement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0014] Wherein said catalyst can be made by the preparation method comprising the following steps:

[0015] 1-5 g of PdCl 2 (preferably 2-3 grams of PdCl 2 ) and 5-30 grams of Ni(NO 3 ) 2 ·6H 2 O (preferably 10-20 grams of Ni(NO 3 ) 2 ·6H 2 O) be dissolved in water, obtain its saturated aqueous solution, the Al of 50-150 gram 2 o 3 (preferably 80-110g of Al 2 o 3 ) into the resulting saturated aqueous solution for at least 30 minutes to remove the Al 2 o 3 , followed by drying (drying temperature 110°C-120°C) and calcining (calcining in a muffle furnace at 500°C-600°C for 6 hours) to obtain the target catalyst.

[0016] Now implement the preparation method of the present invention as an example with the continuous reaction mode, the present invention will be further described:

[0017] The above-mentioned catalyst activated by hydrogenation (the specific activation conditions are: at 250°C to 300°C, add H 2 activated for 6 hours) into a fixed-bed tubular reactor,...

Embodiment 1

[0020] PdCl 2 2.5 g, Ni(NO 3 ) 2 ·6H 2 Dissolve 15 grams of O in water, at room temperature, Al 2 o 3 Immerse 95 grams, take it out after half an hour, drain, dry in an oven at 110-120°C, then transfer to a muffle furnace, bake at 500°C-600°C for 6 hours, and obtain Pd-Ni / Al after cooling 2 o 3 The catalyst, wherein the content of Pd is 1.1wt%, and the content of Ni is 2.3wt%. It is heated at 250 to 300°C before use, adding H 2 Activate for 6 hours.

Embodiment 2

[0022] PdCl 2 1 g, Ni(NO 3 ) 2 ·6H 2 O10 grams dissolved in water, at room temperature, the Al 2 o 3 Immerse 50 grams, take it out after half an hour, dry it in an oven at 110-120°C, then transfer it to a muffle furnace, bake it at 500-600°C for 6 hours, and get Pd-Ni / Al after cooling 2 o 3 The catalyst, wherein the content of Pd is 0.9wt%, and the content of Ni is 3wt%. It is at 250°C to 300°C before use, add H 2 Activate for 6 hours.

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PUM

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Abstract

The invention relates to a method for preparing 3,5-dimethyl aniline through an ammonification reaction of 3,5-dimethylphenol under the existence of a catalyst. The method comprises main steps that: under the existence of a catalyst, 3,5-dimethylphenol is subjected to an ammonification reaction, such that the target substance is prepared. The method is characterized in that: the catalyst is a supported catalyst, and the supported components comprising: metal palladium or / and oxide thereof, and metal nickel or / and oxide thereof. The carrier is alumina. When a total weight of the supported catalyst is considered as 100%, the metal palladium or / and the oxide thereof accounts for 0.3-5.1wt%, the metal nickel or / and the oxide thereof accounts for 0.5-10.6wt%, and the balance is the carrier. When the catalyst provided by the invention is applied in a gas-phase ammonification apparatus, the yield of 3,5-dimethyl aniline is above 80%, and the purity of 3,5-dimethyl aniline can be above 98%. The service life of the catalyst is more than two years.

Description

technical field [0001] The present invention is a preparation method of 3,5-dimethylaniline, in particular, relates to a preparation method of 3,5-dimethylaniline by ammoniation of 3,5-dimethylphenol in the presence of a catalyst. The dimethylaniline method. Background technique [0002] 3,5-Dimethylaniline is an important chemical intermediate, which is mainly used in the production of dyes, pigments, medicines, pesticides and rubber additives. Dianhydride together to synthesize perylene pigments, such as C.I. Pigment Red 149. The pigment is a high-performance red organic pigment with high light and weather fastness, as well as high thermal and chemical stability. It is widely used in the coloring of high-grade plastic products, inks and paints. [0003] So far, various methods for the preparation of 3,5-dimethylaniline have been reported. For example, CN1215720A reports a method for preparing 3,5-dimethylaniline with primary arylamine as the starting material. It uses ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/47C07C209/18
Inventor 沈永嘉张伟侯顺利张毅吉施健美
Owner EAST CHINA UNIV OF SCI & TECH
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