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High-acidity solid sulfonic acid catalyst for catalyzing aromatic compound nitrification, and preparation method

A technology of aromatic compounds and sulfonic acid catalysts, applied in the direction of organic compound/hydride/coordination complex catalysts, nitro compound preparation, physical/chemical process catalysts, etc. Small, unfavorable heat and mass transfer and other problems, to achieve the effect of good cycle performance

Active Publication Date: 2020-04-14
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

TiO 2 -ZrO 2 Solid acid resistance is very good, but its fine pores have a small specific surface area, which is not conducive to the heat and mass transfer of the reaction, and it is easy to cause coke and deactivation

Method used

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  • High-acidity solid sulfonic acid catalyst for catalyzing aromatic compound nitrification, and preparation method
  • High-acidity solid sulfonic acid catalyst for catalyzing aromatic compound nitrification, and preparation method
  • High-acidity solid sulfonic acid catalyst for catalyzing aromatic compound nitrification, and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Preparation of 3D-SiO 2 : Using P123 as a template, 3-methylbutanol as a pore-expanding agent, and ethyl orthosilicate as a gel-forming agent, the gel is generated under the catalysis of concentrated hydrochloric acid. The feeding weight ratio is: ethyl orthosilicate: P123: 3-methylbutanol: concentrated hydrochloric acid: water = 100: 40: 55: 75: 1500 (wt.), and the feeding amount of ethyl orthosilicate is 85g. The gel forming operation is: add triblock polyether and 3-methylbutanol into water to dissolve, then add concentrated hydrochloric acid and stir well. Then at 40°C, ethyl orthosilicate was uniformly added dropwise within 18 hours, and then reacted at 100°C for 20 hours. After suction filtration, washing with water, and calcination in air at 500°C for 5 hours, 19.7g of 3D-SiO was obtained 2 . Specific surface area 860m 2 / g, and the average pore diameter is 6.1 nm.

[0034] (2) The method of phenyl functionalization is: in toluene, use diphenyldimethoxys...

Embodiment 2

[0044] (1) Preparation of 3D-SiO 2 : Using P123 as a template, 3-methylbutanol as a pore-expanding agent, and ethyl orthosilicate as a gel-forming agent, the gel is generated under the catalysis of concentrated hydrochloric acid. The feeding weight ratio is: ethyl orthosilicate: P123: 3-methylbutanol: concentrated hydrochloric acid: water = 100: 50: 70: 90: 1750 (wt.), and the feeding amount of ethyl orthosilicate is 85g. The gel forming operation is: add triblock polyether and 3-methylbutanol into water to dissolve, then add concentrated hydrochloric acid and stir well. Then, tetraethyl orthosilicate was uniformly added dropwise within 35 to 12 hours, and then reacted at 90°C for 22 hours. After suction filtration, washing with water, and calcination in air at 550°C for 4 hours, 20.8g of 3D-SiO was obtained 2 . The specific surface area is greater than 888m 2 / g, the average pore diameter is 7.6nm.

[0045] (2) The method of phenyl functionalization is: in toluene, use d...

Embodiment 3

[0054] (1) Preparation of 3D-SiO 2 : Using F127 as a template, 3-methylbutanol as a pore-expanding agent, and ethyl orthosilicate as a gelling agent, the gel is generated under the catalysis of concentrated hydrochloric acid. The feeding weight ratio is: ethyl orthosilicate: F127: 3-methylbutanol: concentrated hydrochloric acid: water = 100: 60: 80: 110: 2000 (wt.), and the feeding amount of ethyl orthosilicate is 85g. The gel forming operation is: add triblock polyether and 3-methylbutanol into water to dissolve, then add concentrated hydrochloric acid and stir well. Then, tetraethyl orthosilicate was uniformly added dropwise within 24 hours at 25°C, and then reacted at 80°C for 24 hours. After suction filtration, washing with water, and calcination in air at 600°C for 3 hours, 19.2g of 3D-SiO was obtained 2 . The specific surface area is greater than 804m 2 / g, and the average pore diameter is 9.0 nm.

[0055] (2) The method of phenyl functionalization is: in toluene, u...

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Abstract

The invention belongs to the field of organic synthesis, and particularly relates to a high-acidity solid sulfonic acid catalyst for catalyzing aromatic compound nitrification, and a preparation method thereof. The preparation method of the catalyst comprises the following steps: 1, preparing three-dimensional mesoporous silica (3D-SiO2); 2, carrying out complete phenylation on the surface of thethree-dimensional mesoporous silica by using phenylsilane to obtain phenylated three-dimensional mesoporous silica (3D-SiO2-Ph); 3, sulfonating the phenylated three-dimensional mesoporous silica to obtain benzenesulfonic acid functionalized three-dimensional mesoporous silica (3D-SiO2-Ph-SO3H); and 4, catalyzing aromatic compound nitrification by using the 3D-SiO2-Ph-SO3H as a catalyst so as to cleanly synthesize the nitro derivative of the aromatic compound.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a high-acidity solid sulfonic acid catalyst for catalyzing the nitration of aromatic compounds and a preparation method thereof. Background technique [0002] The nitration reaction of aromatic compounds is an important process in the synthesis of medicines, dyes, pesticides, explosives and fibers. Mixed acid (nitric acid + sulfuric acid) is commonly used as nitrating agent in nitration reaction. The amount of sulfuric acid is generally greater than that of nitric acid, so a large amount of liquid waste acid is produced in the production process, which is difficult to handle, easily causes environmental pollution, and greatly reduces production efficiency. [0003] In order to overcome the serious disadvantages of liquid mixed acid nitration, people are committed to developing solid acid instead of concentrated sulfuric acid to catalyze the nitration reaction of aroma...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J35/10C07C205/12C07C201/08C07C205/44C07C205/06
CPCB01J31/0274C07C201/08B01J35/617B01J35/647C07C205/12C07C205/44C07C205/06
Inventor 单玉华李芙蓉王维胡春洋刘入强郑梦阳高远蔡志祥黄冲
Owner CHANGZHOU UNIV
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