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Preparation method and application of magnetic sulfonated polystyrene molecular brush

A technology of polystyrene and molecular brushes, which is applied in the preparation of organic compounds, chemical instruments and methods, and the preparation of aminohydroxyl compounds, etc., can solve problems such as increased production costs, low sulfonic acid group loading, and difficulty in recycling, and achieve reduction Effects of pollutant discharge, simplified post-treatment, and cost reduction

Inactive Publication Date: 2020-05-12
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the load of sulfonic acid groups is low, the amount added during the reaction increases, and the price of the monomer TMPM is expensive, which increases the production cost
In addition, because the catalyst P(TMA-co-SSS) is a random copolymer, the particle size is small, the recovery is difficult, and it is not conducive to the post-processing of the product.

Method used

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  • Preparation method and application of magnetic sulfonated polystyrene molecular brush
  • Preparation method and application of magnetic sulfonated polystyrene molecular brush
  • Preparation method and application of magnetic sulfonated polystyrene molecular brush

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. Preparation of Magnetic Sulfonated Polystyrene Molecular Brush SG-Fe 3 o 4 @PS-PSH

[0032] (1) Accurately weigh 20nm ferric oxide Fe 3 o 4 (6.0 g), vinyltriethoxysilane SG-151 (7.5 g) in a 1000 mL four-neck flask, add 240 mL of absolute ethanol and 20 mL of deionized water, and ultrasonically disperse for 30 min to disperse homogeneous, and stirred at 600 r / min for 16 h in a constant temperature water bath at 40 °C under the protection of nitrogen. After repeated washing with absolute ethanol and deionized water, and vacuum drying at 60 °C for 48 h, SG-Fe 3 o 4 .

[0033] (2) SG-Fe 3 o 4 (6 g), St (11.4168 g, 109.62 mmol), AIBN (0.6 g, 3.654 mmol), DVB (9.5448 g, 73.08 mmol), solvent acetonitrile (600 mL) were placed in a 1000 mL In a four-neck flask, under the protection of nitrogen, stir and reflux for 6 h in a constant temperature oil bath at 80 °C at a speed of 600 r / min. After repeated washing with absolute ethanol and deionized water, dry in a vacuum ...

Embodiment 2

[0041] 1. Preparation of Magnetic Sulfonated Polystyrene Molecular Brush SG-Fe 3 o 4 @PS-PSH

[0042] (1) Accurately weigh 20 nm ferric oxide Fe 3 o 4 (6.0 g), vinyltriethoxysilane SG-151 (7.5 g) in a 1000 mL four-neck flask, add 300 mL of absolute ethanol and 20 mL of deionized water, and ultrasonically disperse for 30 min to disperse homogeneous, and stirred at 600 r / min for 16 h in a constant temperature water bath at 40 °C under the protection of nitrogen. After repeated washing with absolute ethanol and deionized water, and vacuum drying at 60 °C for 48 h, SG-Fe 3 o 4 .

[0043] (2) SG-Fe 3 o 4 (6 g), St (11.4168 g, 109.62 mmol), AIBN (0.6 g, 3.654 mmol), DVB (9.5448 g, 73.08 mmol), solvent acetonitrile (600 mL) were placed in a 1000 mL In a four-neck flask, under the protection of nitrogen, stir and reflux for 6 h in a constant temperature oil bath at 80 °C at a speed of 600 r / min. After repeated washing with absolute ethanol and deionized water, dry in a vacu...

Embodiment 3

[0051] 1. Preparation of Magnetic Sulfonated Polystyrene Molecular Brush SG-Fe 3 o 4 @PS-PSH

[0052] (1) Accurately weigh 20 nm ferric oxide Fe 3 o 4Magnetic powder (6.0 g) and vinyltriethoxysilane SG-151 (7.5 g) were put into a 1000 mL four-neck flask, and 300 mL of absolute ethanol and 20 mL of deionized water were added, and ultrasonically dispersed for 30 min to make it Disperse evenly, and stir at 600 r / min for 16 h in a constant temperature water bath at 40 °C under nitrogen protection. After repeated washing with absolute ethanol and deionized water, and vacuum drying at 60 °C for 48 h, SG-Fe 3 o 4 .

[0053] (2) SG-Fe 3 o 4 (6 g), St (11.4168 g, 109.62 mmol), AIBN (0.6 g, 3.654 mmol), DVB (14.3172 g, 109.62 mmol), solvent acetonitrile (600 mL) were placed in a 1000 mL In a four-neck flask, under the protection of nitrogen, stir and reflux for 6 h in a constant temperature oil bath at 80 °C at a speed of 600 r / min. After repeated washing with absolute ethano...

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Abstract

The invention provides a preparation method, which comprises the following steps: carrying out surface modification on nano ferroferric oxide by using vinyltriethoxysilane; by taking styrene as a monomer and taking magnetic polystyrene chloride balls as a macromolecular initiator, grafting polystyrene on the surfaces of the magnetic polystyrene chloride balls to obtain a magnetic polystyrene molecular brush, and sulfonating the magnetic polystyrene molecular brush to obtain the magnetic sulfonated polystyrene molecular brush. The invention relates to a method for synthesizing N-(ethoxymethylene) aniline by using the magnetic sulfonated polystyrene molecular brush. When the magnetic sulfonated polystyrene molecular brush is used for preparing N-(ethoxymethylene) aniline through catalysis, the reaction rate is high, the N-(ethoxymethylene) aniline can be recycled, and the magnetic sulfonated polystyrene molecular brush has the advantages that pollutant emission is reduced, resources aresaved, and the cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of solid acid catalysis, and in particular relates to a preparation method of a magnetic sulfonated polystyrene molecular brush and its application in synthesizing N-(ethoxymethylene)aniline. Background technique [0002] As an important organic chemical raw material, N-(ethoxymethylene)aniline and its derivatives are widely used in pharmaceutical, pesticide, dyestuff and other industries. Currently, acid-catalyzed N-alkylation of aniline with triethyl orthoformate is the - (Ethoxymethylene)aniline main method. [0003] Conventional acid catalysts include inorganic acids (such as: sulfuric acid, hydrohalic acid, phosphoric acid, fluorosulfonic acid) and organic acids (such as: p-toluenesulfonic acid, alkylsulfonic acid, etc.). Small molecular inorganic acids can be fully mixed and contacted between the reaction system and the reactants. Generally, they have high activity and low cost, but they have disadva...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F285/00C08F292/00C08F212/08C08F212/36C08F212/14C08F8/36B01J31/10C07C213/00C07C217/08
CPCC08F285/00C08F292/00C08F8/36B01J31/10C07C213/00B01J35/33C07C217/08C08F212/08C08F212/36C08F212/14
Inventor 刘少杰王利利郝盼盼赵婷张锐褚晓萌孙玉娟
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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