One-pot catalytic synthesis method for interfacial polymerization of aliphatic polyamide sulfonamide

A polyamide sulfonamide and interfacial polymerization technology is applied in the field of one-pot catalytic synthesis of aliphatic polyamide sulfonamide interfacial polymerization, and can solve the problems of poor operability, low yield, complicated preparation steps and the like

Active Publication Date: 2020-12-11
庆阳职业技术学院
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of solution polymerization is mostly used, and the disadvantage of the polyamide sulfonamide polymer synthesized from diamine monomers containing sulfonamide groups and bisacyl chloride monomers is that the preparation steps of diamine monomers containing sulfonamide groups are cumbersome. And the reaction conditions are harsh, and at the same time, the diamine monomer containing sulfonamide group has low activity, and it is not easy to react with dichloro monomer to synthesize high molecular weight polyamide sulfonamide polymer; and fluorine-containing polyamide sulfonamide requires special reaction conditions , poor operability, low molecular weight, low yield, high cost and other defects, which limit the performance and industrial application of polyamide sulfonamide

Method used

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  • One-pot catalytic synthesis method for interfacial polymerization of aliphatic polyamide sulfonamide
  • One-pot catalytic synthesis method for interfacial polymerization of aliphatic polyamide sulfonamide
  • One-pot catalytic synthesis method for interfacial polymerization of aliphatic polyamide sulfonamide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The synthetic procedure in Example 1. A one-pot catalytic sulfonamide fatty polyamide interfacial polymerization:

[0044] At atmospheric pressure, sufficient nitrogen, dissolved completely aliphatic diamine monomer, the composite catalyst, an acid binder deionized water was added with mechanical stirring vessel, the stirring speed of 250r / min of stirring continued dissolving an organic solvent was added dropwise a slight excess molar amount of 3-chloro-sulfonyl chloride monomers; 10 ~ 15min addition was complete, the reaction 45min at 25 deg.] C for 4h and then at 0 deg.] C, until the reaction solution PH≈7.25 when the reaction stopped, the polymer solution was precipitated white. End of the reaction, the resulting product was successively boiled deionized water and washed three times with absolute ethanol alternately, dried at 100 deg.] C under vacuum for 24 hours to obtain the sulphonamide fatty polyamide polymer, a yield of 89.53%.

[0045] Wherein: a molar ratio of 3...

Embodiment 2

[0047] Embodiment 2 A catalytic one-pot synthesis a fatty polyamide-sulfonamide interfacial polymerization:

[0048] At atmospheric pressure, sufficient nitrogen, dissolved completely aliphatic diamine monomer, the composite catalyst, an acid binder deionized water was added with mechanical stirring vessel, the stirring speed of 380r / min of stirring continued dissolving an organic solvent was added dropwise a slight excess molar amount of 3-chloro-sulfonyl chloride monomers; 10 ~ 15min addition was complete, the reaction after the reaction for 2h 25min at 40 ℃ 5 ℃, the reaction solution to be PH≈7.25 when the reaction stopped, the polymer solution was precipitated white. End of the reaction, the resulting product was boiled successively with deionized water and ethanol and alternately washed five times, dried at 100 deg.] C under vacuum for 24 hours to obtain the sulphonamide fatty polyamide polymer, a yield of 90.81%.

[0049] Wherein: a molar ratio of 3-chloro-sulfonyl chlorid...

Embodiment 3

[0051] Embodiment 3 A catalytic one-pot synthesis of an aliphatic polyamide sulfonamide interfacial polymerization:

[0052] At atmospheric pressure, sufficient nitrogen, dissolved completely aliphatic diamine monomer, the composite catalyst, an acid binder deionized water was added with mechanical stirring vessel, the stirring speed of 300r / min of stirring continued dissolving an organic solvent was added dropwise a slight excess molar amount of 3-chloro-sulfonyl chloride monomers; 10 ~ 15min addition was complete, the reaction 35min at after 3h reaction at 2 ℃ 30 ℃, the reaction solution to be PH≈7.25 when the reaction stopped, the polymer solution was precipitated white. End of the reaction, the resulting product was successively boiled deionized water and absolute ethanol alternately washed 4 times, dried at 100 deg.] C under vacuum for 24 hours to obtain the sulphonamide fatty polyamide polymer, a yield of 92.78%.

[0053] Wherein: a molar ratio of 3-chloro-sulfonyl chlorid...

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Abstract

The invention relates to a one-pot catalytic synthesis method for interfacial polymerization of aliphatic polyamide sulfonamide, which comprises the steps of adding deionized water in which an aliphatic diamine monomer, a composite catalyst and an acid-binding agent are completely dissolved into a container provided with a mechanical stirring device under the protection of normal pressure and sufficient nitrogen, and dropwise adding an organic solvent for dissolving a slightly excessive amount of 3-chlorosulfonyl benzoyl chloride monomer while continuously stirring; after dropwise adding for 10-15 minutes, reacting for 25-45 minutes at the temperature of 0-5 DEG C, then reacting for 2-4 hours at the temperature of 25-40 DEG C, alternately washing a product obtained after the reaction for 3-5 times by sequentially using boiled deionized water and absolute ethyl alcohol, and drying in vacuum to obtain the aliphatic polyamide sulfonamide polymer. The method is simple in process and easy to implement, and the obtained aliphatic polyamide sulfonamide polymer has good thermal stability, friction performance and solvent resistance and can be used as a potential reverse osmosis membrane material, an ultrafiltration membrane material and other membrane materials and a solid lubrication and special engineering material.

Description

Technical field [0001] The present invention relates to the field of functional polymer materials, in particular, it relates to a method for the synthesis of fatty polyamide sulfonamide interfacial polymerization catalyst pot. Background technique [0002] Polyamide (PA), also commonly known as nylon, refers to a class of polymer material backbone repeating units containing amide groups. 1931 W.H.Carother developed by DuPont Central Research Institute and industrialization, the first polyamide apply for patents U.S.Pat.2130948. Polyamide with excellent mechanical and electrical properties, but also with abrasion resistance, solvent resistance, oil resistance, self-lubrication and good processing properties, currently is the preferred engineering materials, and therefore derived a lot of modified functional materials for automotive, electronics electronics, aerospace and weapons industry indispensable structural materials. [0003] Polysulfonamide (PAS) refers to a polymer backbon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/42
CPCC08G69/42
Inventor 刘利剑张绍印刘丽王程吴龑平郭娜曹新和王鑫
Owner 庆阳职业技术学院
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