Preparation method of sulfonated polyethersulfone for preparing macromolecule separation films

A technology of sulfonated polyethersulfone and separation membrane, which is applied in the field of chemical synthesis of polymer materials, can solve the problems of large space, weakening of large electron cloud, unfavorable complex stability, etc., and achieve stable performance and good separation effect Effect

Inactive Publication Date: 2012-06-20
杭州北斗星膜制品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the mechanism of the sulfonation reaction, when the benzene ring has an electron-donating group, it is beneficial to the formation of the complex, which is beneficial to the sulfonation reaction; The large electron cloud of the ring is weakened, which is not conducive to the stability of the complex formed by it, so it is not conducive to the sulfonation reaction
Since part of the benzene ring of polyethersulfone is connected with the strong electroabsorbing sulfone group, the benzene ring is passivated, so electrophilic substitution is very difficult, and the space occupied by the sulfone group and the sulfonic acid group itself is large, and the sulfonation The steric effect is larger than the corresponding halogen atom, so the steric hindrance effect is very significant, so the sulfonation reaction process of polyethersulfone is relatively difficult

Method used

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  • Preparation method of sulfonated polyethersulfone for preparing macromolecule separation films
  • Preparation method of sulfonated polyethersulfone for preparing macromolecule separation films
  • Preparation method of sulfonated polyethersulfone for preparing macromolecule separation films

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The selected reagent of the present invention is: vacuum drying oven, DZF-6050, Shanghai Jinghong; Constant speed agitator, S212-90, Shanghai Shensheng; Ubbelohde viscometer, 1385 flat type; Pure, Lanxi Liudongshan Chemical Industry; 1,2-Dichloromethane (DCM), analytically pure, Chengdu Kelon Chemical; chloroform, analytically pure, Chengdu Kelon Chemical; N,N-Dimethylformamide (DMF) , analytically pure, Chengdu Kelong Chemical; polyethersulfone (PES), 3000P, GAFONE; chlorosulfonic acid, chemically pure, Tingxin Chemical Reagent Factory.

[0027] The polyethersulfone used in the present invention was vacuum-dried at 130° C. for 10 hours.

[0028] Add 10g of polyethersulfone into a three-necked flask filled with 50mL of concentrated sulfuric acid (98%) solvent, stir and dissolve at room temperature to form a homogeneous solution, measure a certain amount of chlorosulfonic acid in a constant pressure dropping funnel, in which the sulfonating agent The molar ratio to poly...

Embodiment 2-4

[0042] According to the method shown in embodiment 1, adopt different solvents to carry out comparative test:

[0043] The influence of solvent on the sulfonation reaction, as shown in the following table

[0044]

[0045]

[0046] The above reaction chlorosulfonic acid addition rate is 3s / d, stirring speed 800r / min.

[0047] It can be seen from the data in the above table that the solvent has an important influence on the sulfonation of polyethersulfone. Among the three solvents selected, 1,2-dichloromethane, chloroform and concentrated sulfuric acid, concentrated sulfuric acid is more suitable as the polyethersulfone solvent. Solvent for sulfonation. According to the reaction mechanism, as the sulfonation reaction proceeds, the polar group sulfonic acid group continuously attacks the molecular chain of polyethersulfone, making the molecular chain of polyethersulfone gradually become more polar, and the solvation effect with the solvent becomes larger and larger. , th...

Embodiment 5-12

[0049] According to the method shown in embodiment 1, adopt the different consumption of chlorosulfonic acid to give an example.

[0050] The amount of chlorosulfonic acid, that is, the molar ratio of chlorosulfonic acid and polyethersulfone is an important parameter affecting the degree of sulfonation of polyethersulfone sulfonation reaction. In this experiment, the sulfonation reaction was studied by adopting different ratios of chlorosulfonic acid / polyethersulfone, and the results are shown in the table below:

[0051] Influence of the amount of chlorosulfonic acid on the sulfonation reaction

[0052]

[0053] The above reaction chlorosulfonic acid addition rate is 3s / d, stirring speed 800r / min. The total reaction time is 360min, the reaction temperature is 10°C, and the solvent is concentrated sulfuric acid.

[0054] From the above table and attached figure 1 It can be seen that with the increasing ratio of chlorosulfonic acid / polyethersulfone, the degree of sulfonat...

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Abstract

The invention discloses a chemical synthesis method of macromolecule materials and particularly relates to a preparation method of sulfonated polyethersulfone for preparing macromolecule separation films. The preparation method includes steps of drying polyethersulfone, adding the same serving as solute into concentrated sulfuric acid to dissolve, preparing chlorosulfonic acid serving as sulfonating agent and the polyether sulfone according to a certain proportion and mixing the same to react for 2 to 8 hours, transferring materials of the mixture into ice and water mixed liquid and precipitating products from the mixed liquid after reaction is finished, washing the products to be neutral by distilled water after the products are filtered, and finally drying the products to obtain sulfonated polyethersulfone. The preparation method has the advantages that the products uniform in sulfonation degree are obtained, precipitation and the like under the action of solvent is avoided during integral reaction, the macromolecule separation film prepared by the sulfonated polyethersulfone has better separation effect, water flux capability, contamination resistance and more stable performance and the like. The sulfonated polyethersulfone prepared by the preparation method has wide application prospect in film manufacturing field.

Description

technical field [0001] The invention relates to a chemical synthesis method of polymer materials, in particular to a preparation method of sulfonated polyethersulfone used for preparing polymer separation membranes. technical background [0002] Polyethersulfone (PES for short), the structural formula is [0003] [0004] It has a rigid benzene ring and a flexible ether group in its molecule, and the sulfone group forms a large conjugated system with the entire structural unit, so the entire molecule has good stability and exhibits excellent mechanical properties and creep resistance. And its outstanding heat resistance, thermal oxidation resistance and chemical stability are widely used in the preparation of separation membranes as separation membrane materials. However, its hydrophobicity makes it easy to cause adsorption and deposition of hydrophobic solutes on the surface of the membrane during the membrane water treatment process, which causes the membrane pores to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/23B01D71/68
Inventor 戚晶云王伟刘帅潘巧明
Owner 杭州北斗星膜制品有限公司
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