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Hierarchical pore Hbeta molecular sieve catalyst for preparing diphenylamine by condensing aniline as well as preparation method and application thereof

A technology of β molecular sieve and microporous molecular sieve, which is applied in the field of multi-level porous Hβ molecular sieve catalysts, can solve the problems of unfavorable catalyst activity, service life, product selectivity, catalyst activity decline, and loss of activity, so as to improve reaction rate and product selection High degree, high selectivity, good stability

Active Publication Date: 2016-06-01
NANJING UNIV OF TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0006] It can be seen from the above-mentioned patents that in the process of continuous preparation of diphenylamine in liquid phase from aniline, the catalyst with Hβ molecular sieve and alumina as the main components has good catalytic activity and high selectivity, but this type of catalyst loses its strength after being used for less than half a year. activity, must be regenerated or replaced with a new catalyst
Catalyst deactivation is mainly caused by carbon deposits. With the prolongation of operation time, the by-product compounds are pyrolyzed and condensed to form carbon deposits and viscous high-molecular nitrogen-containing polymers, which are deposited on the surface of the catalyst and block the micropores of the catalyst. , covering the acid active center of the catalyst, leading to a gradual decline in catalyst activity
[0007] The Hβ molecular sieves used in the above inventions all have a microporous structure, and the pore size of the molecular sieve is generally about 0.65nm. Since the pore size of the Hβ molecular sieve is similar to the molecular size of the reactants and products, the molecules diffuse slowly in the pores and easily cause carbon deposition. It is not conducive to improving the activity, service life and product selectivity of the catalyst

Method used

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  • Hierarchical pore Hbeta molecular sieve catalyst for preparing diphenylamine by condensing aniline as well as preparation method and application thereof
  • Hierarchical pore Hbeta molecular sieve catalyst for preparing diphenylamine by condensing aniline as well as preparation method and application thereof
  • Hierarchical pore Hbeta molecular sieve catalyst for preparing diphenylamine by condensing aniline as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Dissolve 0.05g of NaCl and 0.15g of KCl in 20mL of water, add 14.4g of tetraethylammonium hydroxide aqueous solution (25% by mass) and 3.9g of silicic acid, stir at 40℃ for 4~5h, then add 0.547g of NaAlO 2 And 0.145g NaOH, the measured pH value is 12.2, continue to stir for 4-5h, then add 0.5g cetyltrimethylammonium bromide to it, and stir for 8-10h at 80°C. Put the formed white turbid liquid into the crystallization kettle, under the autogenous pressure, crystallize at 150°C for 120h, after the crystallization is finished, cool to room temperature naturally. The solid-liquid mixture was filtered to remove the liquid, washed to neutrality, and dried in an oven at 100°C for 12 hours. Then it was calcined at 550°C for 6 hours to obtain a multi-porous β molecular sieve. Take 4g of hierarchical pore β molecular sieve and 80mL of 1mol / L NH 4 The Cl solution was ion-exchanged 3 times, 4h each time, filtered, washed, dried, and calcined at 550°C for 6h to obtain a multi-porous ...

Embodiment 2

[0052] Dissolve 0.05g of NaCl and 0.15g of KCl in 20mL of water, add 14.4g of tetraethylammonium hydroxide aqueous solution (25% by mass) and 3.9g of silicic acid, stir at 40℃ for 4~5h, then add 0.164g of NaAlO 2 And 0.066g of NaOH, the measured pH value is 11.2, continue to stir for 4 to 5h, then add 0.5g of hexadecyltrimethylammonium bromide to it, and stir for 8 to 10h at 80°C. Put the formed white turbid liquid into the crystallization kettle, under the autogenous pressure, crystallize at 150°C for 120h, after the crystallization is finished, cool to room temperature naturally. The solid-liquid mixture was filtered to remove the liquid, washed to neutrality, and dried in an oven at 100°C for 12 hours. Then it was calcined at 550°C for 6 hours to obtain a multi-porous β molecular sieve. Take 4g of hierarchical pore β molecular sieve and 80mL of 1mol / L NH 4 The Cl solution was ion-exchanged 3 times, 4h each time, filtered, washed, dried, and calcined at 550°C for 6h to obtain...

Embodiment 3

[0054] Dissolve 0.05g of NaCl and 0.15g of KCl in 20mL of water, add 14.4g of tetraethylammonium hydroxide aqueous solution (25% by mass) and 3.9g of silicic acid, stir at 40°C for 4~5h, then add 0.055g of NaAlO 2 And 0.066g NaOH, the measured pH value is 10.9, continue to stir for 4-5h, then add 0.5g of hexadecyltrimethylammonium bromide to it, and stir for 8-10h at 80°C. Put the formed white turbid liquid into the crystallization kettle, under the autogenous pressure, crystallize at 150°C for 120h, after the crystallization is finished, cool to room temperature naturally. The solid-liquid mixture was filtered to remove the liquid, washed to neutrality, and dried in an oven at 100°C for 12 hours. Then it was calcined at 550°C for 6 hours to obtain a multi-porous β molecular sieve. Take 4g of hierarchical pore β molecular sieve and 80mL of 1mol / L NH 4 The Cl solution was ion-exchanged 3 times, 4h each time, filtered, washed, dried, and calcined at 550°C for 6h to obtain a multi...

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Abstract

The invention discloses a hierarchical pore Hbeta molecular sieve catalyst for preparing diphenylamine by condensing aniline. The hierarchical pore Hbeta molecular sieve catalyst is prepared by virtue of a direct synthetic method or a micropore molecular sieve modification indirect synthetic method. The invention also discloses a preparation method of the hierarchical pore Hbeta molecular sieve catalyst as well as an application in preparing diphenylamine by catalyzing the condensation of the aniline. Under the effect of a formed catalyst prepared by the hierarchical pore Hbeta molecular sieve catalyst, the aniline has a self-condensation reaction to prepare diphenylamine, the reaction temperature is 290 to 370 DEG C, the reaction pressure is 1.5MPa to 5MPa, and the airspeed is 0.1 to 0.7 / h. The molecular sieve catalyst has the advantages of good catalytic activity, good stability and high diphenylamine selectivity. Compared with the corresponding ordinary micropore Hbeta molecular sieve, the conversion rate of the aniline is at least increased by 23%, the selectivity of the diphenylamine is at least increased by 1%, and the service life of the catalyst can reach more than 7000 hours.

Description

Technical field [0001] The invention belongs to the field of chemical industry, and relates to a multistage porous Hβ molecular sieve catalyst for preparing diphenylamine by condensation of aniline, and preparation and application thereof. Background technique [0002] Diphenylamine is an important fine organic chemical raw material with a wide range of uses, mainly used in rubber additives, explosive stabilizers, medicine, dyes and other industries. The traditional production method of aniline to synthesize diphenylamine is a batch-type liquid-phase catalytic synthesis method. Due to the use of aluminum trichloride as a catalyst, the equipment is corroded seriously in the production, the environment is polluted, the reaction selectivity is low, and the separation of the catalyst and the product is difficult. The process route is long, the unit consumption of raw materials is high, and the product cost is high. [0003] In order to overcome the shortcomings of the above synthesis ...

Claims

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Application Information

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IPC IPC(8): B01J29/06B01J35/10B01J35/08C07C209/60C07C211/55
CPCC07C209/60B01J29/06B01J2229/14B01J35/50B01J35/51B01J35/617B01J35/643B01J35/615B01J35/647C07C211/55
Inventor 乔旭费兆阳郭海纬汤吉海陈献崔咪芬
Owner NANJING UNIV OF TECH
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