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Brominated sulfonic acid resin and preparation method thereof

A technology of bromosulfonic acid resin and sulfonic acid resin, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve pollution, resin sulfonation is difficult to occur , waste and other problems, to achieve the effect of improving catalytic activity, short end point time, and simple method

Inactive Publication Date: 2015-09-30
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is that after the brominated polystyrene resin is obtained, the resin needs to be cleaned with a variety of toxic solvents, resulting in waste and pollution. In addition, because -Br occupies the para position of the styrene ring, sulfonation can only occur in The ortho or meta position of the benzene ring, and the steric hindrance of the carbon chain of the resin and the passivation of the adjacent carbon atoms on the benzene ring by the substituent -Br, make it difficult for the sulfonation of the resin to occur

Method used

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  • Brominated sulfonic acid resin and preparation method thereof

Examples

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Comparison scheme
Effect test

Embodiment 1

[0027] The preparation method of bromosulfonic acid resin A-15-Br-1:

[0028] (1) Add 20 g of Amberlyst 15 resin and 60 mL of distilled water to the reaction bottle, then add 12 g of bromine, stir with electric power, and react in the dark at 50 °C until the solution fades, and filter to obtain modified Amberlyst 15 resin;

[0029] (2) Wash the modified Amberlyst 15 resin obtained in step (1) until neutral with distilled water, and place in 50 mLOH - In the ethanol-water solution of sodium hydroxide with a concentration of 1 mol / L (the volume ratio of ethanol to water is 1:1), heat and reflux at 90 °C for 2 h;

[0030] (3) Wash the refluxed Amberlyst 15 resin with distilled water, then rinse it with 0.8 mol / L hydrochloric acid from top to bottom at a flow rate of 1 drop / second for 4 h, until the color of the resin changes from brown to khaki completely , and finally washed with water until neutral to obtain bromosulfonic acid resin A-15-Br-1.

[0031] It was determined that ...

Embodiment 2

[0033] The preparation method of bromosulfonic acid resin A-15-Br-2:

[0034] (1) Add 20 g of Amberlyst 15 resin and 60 mL of distilled water to the reaction bottle, then add 20 g of bromine, stir electrically, and react in the dark at 60 °C until the solution fades, and filter to obtain modified Amberlyst 15 resin;

[0035] (2) Wash the modified Amberlyst 15 resin obtained in step (1) until neutral with distilled water, and place in 50 mLOH - In the ethanol-water solution of sodium hydroxide with a concentration of 1.2mol / L (the volume ratio of ethanol to water is 1.5:1), heat and reflux at 80 °C for 2.5 h;

[0036](3) Wash the refluxed Amberlyst 15 resin with distilled water, then rinse it with 1.0 mol / L hydrochloric acid from top to bottom at a flow rate of 2 drops / second for 3 h, until the color of the resin changes from brown to khaki completely , and finally washed with water until neutral to obtain bromosulfonic acid resin A-15-Br-2.

[0037] After measurement, the ma...

Embodiment 3

[0039] The preparation method of bromosulfonic acid resin D72-Br-3:

[0040] (1) Add 20 g of D72 resin and 60 mL of distilled water to the reaction bottle, then add 12 g of bromine, stir with an electric motor, and react in the dark at 55 °C until the solution fades, and filter to obtain the modified D72 resin;

[0041] (2) Wash the modified D72 resin obtained in step (1) until it is neutral with distilled water, and place it in 50 mLOH - In ethanol-water solution of sodium hydroxide with a concentration of 1.5 mol / L (the volume ratio of ethanol to water is 2:1), heat and reflux for 3 h at 75 °C;

[0042] (3) Wash the D72 resin after the reflux treatment with distilled water, and then rinse it with 1.2 mol / L hydrochloric acid from top to bottom at a flow rate of 2 drops / second for 3 h until the color of the resin changes from brown to khaki completely. Finally, wash with water until neutral to obtain bromosulfonic acid resin D72-Br-3.

[0043] After determination, the mass e...

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Abstract

The invention discloses brominated sulfonic acid resin and a preparation method thereof. The brominated sulfonic acid resin is prepared according to the method which includes the following steps: (1) adding bromine into sulfonic acid resin and water, wherein the mass ratio of bromine to sulfonic acid resin is (0.6-1):1, stirring and reacting at 50-60 DEG C under the dark environment until the color of the solution fades, and then filtering to obtain modified sulfonic acid resin; (2) washing the modified sulfonic acid resin obtained in the step (1) with water to be neutral, placing the washed modified sulfonic acid resin into a strong alkaline solution, heating, refluxing and reacting for 2-3 hours; (3) washing the sulfonic acid resin subjected to reflux treatment with water, then leaching with a strong acid solution for 3-4 hours, and finally washing to be neutral to obtain the brominated sulfonic acid resin. The brominated sulfonic acid resin is good in hydrophobicity, excellent in catalytic performance, and long in service life; the preparation method is simple and mild in reaction conditions, and is a new method for preparing a hydrophobic strong acid catalyst.

Description

Technical field [0001] The present invention involves a bromo sulfonic acid resin and its preparation method, which specifically involves a bromine sulfonic acid resin and its preparation methods with hydrophobic activity. Background technique [0002] Large hole sulfonic acid resin is a commonly used solid acid catalyst, which has the characteristics of cheap, safe and regeneration.Large holes sulfonic acid resin can be used in water or non -water media.In an environment with water, -SO 3 H will be solved, and OH is generated around the internal hole of the resin 3 + At this time, the main role to the reaction is the concentration of the reaction in the touches.However, due to the obstacles of the polymerization chain in the resin, the molecules of the reactor cannot move freely in the resin channel. The concentration of the reactant in the pores is lower than the concentration in the solution, which affects the catalytic activity of the sulfonic acid resin.In non-water media, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F12/08C08F8/22B01J31/10
Inventor 沈鹏飞徐满才
Owner HUNAN NORMAL UNIVERSITY