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Composite solid super acidic catalyst, preparation method thereof and method for catalytically synthesizing N,N-diethylaniline by using solid super acidic catalyst

A technology of solid superacid and diethylaniline, applied in the direction of catalyst activation/preparation, preparation of amino compounds, chemical instruments and methods, etc., can solve the problems of small number of acidic sites, long equilibration time, short service life, etc., to achieve High selectivity, simple preparation method, and the effect of improving the service life

Inactive Publication Date: 2019-08-23
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these common solid superacids have many advantages, there are still many deficiencies in practical applications: (1) it shows that the loaded SO 4 2- It is easy to lose and has a short service life; (2) the number of acidic sites is small, so it takes a long time for the reaction to reach equilibrium under the same conditions

Method used

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  • Composite solid super acidic catalyst, preparation method thereof and method for catalytically synthesizing N,N-diethylaniline by using solid super acidic catalyst
  • Composite solid super acidic catalyst, preparation method thereof and method for catalytically synthesizing N,N-diethylaniline by using solid super acidic catalyst
  • Composite solid super acidic catalyst, preparation method thereof and method for catalytically synthesizing N,N-diethylaniline by using solid super acidic catalyst

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Experimental program
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Embodiment 1

[0026] The composite solid superacid catalyst of this embodiment, catalyzer is made of composite carrier CeO 2 -WO 3 -ZrO 2 and surface-loaded SO 4 2- composition. Wherein, the molar ratio in the carrier n(W):n(Zr)=0.5:1, n(Ce):n(Zr)=0.1:1.

[0027] The preparation method of this catalyst comprises the steps:

[0028] (1) Preparation of CeO 2 -WO 3 -ZrO 2 Carrier precursor: ZrOCl 2·8H 2 O, (NH 4 ) 6 h 2 W 12 o 40 ·xH 2 O and Ce(NO 3 ) 3 ·6H 2 O was placed in a three-necked flask according to the above molar ratio, and water was added to dissolve it completely, and concentrated NH was added dropwise with a constant pressure dropping funnel 3 ·H 2 O (25wt%), and vigorously stirred until the pH = 9 ~ 11; continued to stir for 10 ~ 15h, ultrasonic 3-5h, and then transferred to a polytetrafluoroethylene-lined stainless steel hydrothermal synthesis kettle, at 120 ° C Aging for 22 hours; after cooling, filter with suction, dry the precipitate at 120°C for 22 hour...

Embodiment 2

[0044] The single dimension experiment of the mol ratio of embodiment 2 W and Zr

[0045] The basic steps are the same as in Example 1, except that the ratio of W and Zr in the carrier is used, and N,N-diethylaniline is catalyzed by a catalyst, and the obtained results are shown in Table 2 below.

[0046] The conversion rate of the aniline of table 2 embodiment 2 and the selectivity result of N,N-diethylaniline

[0047] serial number no W :n Zr

[0048] It can be seen from Table 2 that the present invention uses a catalyst with a molar ratio of n(W):n(Zr)=0.1~0.9:1, which can make the conversion rate of aniline reach 95.41~100%, and N,N-diethyl The selectivity of aniline can reach 53.84~70.9%.

Embodiment 3

[0049] The single dimension experiment of the molar ratio of embodiment 3 Ce and Zr

[0050] The basic steps are the same as in Example 1, except that the molar ratio of Ce and Zr is used, and the prepared catalyst is used to prepare N,N-diethylaniline, and the obtained results are shown in Table 3 below.

[0051] The conversion rate of the aniline of table 3 embodiment 3 and the selectivity result of N,N-diethylaniline

[0052] serial number no Ce :n Zr

[0053] It can be seen from Table 3 that the present invention uses a catalyst with a molar ratio n(Ce):n(Zr)=0.05~0.15:1, which can make the conversion rate of aniline reach 98.08~100%, and N,N-diethylaniline The selectivity can reach 56.34~70.9%.

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Abstract

The invention discloses a composite solid super acidic catalyst, a preparation method thereof and a method for catalytically synthesizing N,N-diethylaniline by using the solid super acidic catalyst. The composite solid super acidic catalyst is composed of a composite carrier CeO2-WO3-ZrO2 and SO4<2-> supported on the surface; the preparation comprises the following steps: preparing a precursor ofthe carrier, placing the precursor into a (NH4)2SO4 solution for immersion, performing drying, and performing calcination to obtain the super acidic catalyst; and the method for catalytically synthesizing the N,N-diethylaniline by adopting the catalyst comprises the following steps: putting the solid super acidic catalyst into a fixed bed tubular reactor, adding a mixed solution of aniline and ethanol, and performing a reaction to obtain the N,N-diethylaniline. The solid super acidic catalyst provided by the invention has strong acidity and a high acid center density, and the presence of oxygen vacancies can enhance activity of the catalyst; at the same time, the preparation method is simple and convenient, and has strong operability; and according to the N,N-diethylaniline catalytically synthesized by adopting the catalyst, the conversion rate of aniline is higher, and the selectivity of the N,N-diethylaniline is higher.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, and in particular relates to a composite solid superacid catalyst, a preparation method and a method for catalytically synthesizing N,N-diethylaniline with it. Background technique [0002] N,N-Diethylaniline is a light yellow oily liquid, mainly used in dye intermediates, latex accelerators, can be used to prepare azo dyes, triphenylmethane dyes, etc., and is also used in the pharmaceutical industry and color film developers. intermediate. There is one -NH in the aniline molecule 2 , under the action of catalyst, -NH 2 The -H on it can combine with the -OH in ethanol to remove the H 2 O molecules to generate N,N-diethylaniline. At present, the preparation method of N,N-diethylaniline mainly contains two kinds: (1) with H 2 SO 4 As a catalyst, ethanol and aniline are reacted in a batch reactor. The advantage of this method is that the technology is mature and the price of the catalyst is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053B01J37/02B01J37/08C07C209/18C07C211/48
CPCB01J27/053B01J37/0201B01J37/08C07C209/18C07C211/48
Inventor 顾正桂刘亚成曹晓艳
Owner NANJING NORMAL UNIVERSITY
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