CN105754119A - Method for preparing nylon-6 porous polymer membrane - Google Patents

Method for preparing nylon-6 porous polymer membrane Download PDF

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Publication number
CN105754119A
CN105754119A CN201610146801.8A CN201610146801A CN105754119A CN 105754119 A CN105754119 A CN 105754119A CN 201610146801 A CN201610146801 A CN 201610146801A CN 105754119 A CN105754119 A CN 105754119A
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CN
China
Prior art keywords
nylon
acid
polymeric film
apertured polymeric
preparation
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Pending
Application number
CN201610146801.8A
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Chinese (zh)
Inventor
李耀刚
郭洋
王宏志
张青红
侯成义
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Donghua University
National Dong Hwa University
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Donghua University
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Priority to CN201610146801.8A priority Critical patent/CN105754119A/en
Publication of CN105754119A publication Critical patent/CN105754119A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/30Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by mixing gases into liquid compositions or plastisols, e.g. frothing with air
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2377/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

The invention relates to a method for preparing nylon-6 porous polymer membrane, comprising: dissolving nylon-6 slices in an acid solution, stirring at 50-80 DEG C for 2-6 h to obtain nylon-6 mixed acid solution; pushing the nylon-6 mixed acid solution through an injecting pump, dropping in deionized water in a container through a capillary tube so as to obtain the nylon-6 porous polymer membrane on a deionized water and air interface.A preparation process of the method requires no any special equipment, the technique is simple, the cost is low, and the prepared nylon-6 porous polymer membrane has uniform pore diameter and controllable thickness and is applicable to the fields such as separation, adsorption and sensing fields.

Description

A kind of preparation method of nylon 6 apertured polymeric film
Technical field
The invention belongs to the preparation field of polymer film, particularly to the preparation method of a kind of nylon 6 apertured polymeric film.
Background technology
Apertured polymeric film separating, adsorb, the field such as sensing has potential using value, thus causes researcher's Extensive concern.But traditional method preparing apertured polymeric film is mainly based on template, preparation flow length, complex process, With high costs, limit it and be widely applied.
Nylon 6 has excellent impact resistance and antilysis due to it, and has the using value of excellence under numerous environment.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of nylon 6 apertured polymeric film, the method achieves The preparation of the apertured polymeric film that size, thickness are controlled.Gained porous nylon membrane even pore distribution, film pliability is good.
A kind of preparation method of nylon 6 apertured polymeric film of the present invention, including:
(1) nylon 6 slice is dissolved in acid solution, 50-80 DEG C of stirring 2-6h, obtains nylon 6 mixed acid solution;
(2) nylon 6 mixed acid solution that stirring in step (1) obtains is advanced by syringe pump, enter capillary, in room Instill in the deionized water received in container through capillary under temperature, nylon 6 porous polymeric can be obtained in deionized water-Air Interface Thing film;Wherein, the propelling speed of syringe pump is 5~50mL/min, and the internal diameter of capillary is 0.25~5mm, deionized water Temperature is 0~80 DEG C.
In described step (1), nylon 6 slice is 1:10-1:30 with the mass ratio of acid solution.
In described step (1) acid solution be the concentrated sulfuric acid, hydrochloric acid, formic acid, nitric acid, acetic acid, propionic acid, butyric acid, octanoic acid, adipic acid, At least one in ethanedioic acid, phthalic acid and terephthalic acid (TPA).
In described step (2), capillary is polytetrafluoroethylene (PTFE) material.
In described step (2), nylon 6 apertured polymeric film can be by cellulose membrane, AAO film, PET, PS, aluminium foil, copper Paper tinsel, titanium foil or titanium net etc. are transferred to material requested surface.
In described step (2), the thickness of nylon 6 porous polymer film is 2~8 μm, and aperture is 300~1000nm.
It is desirable to provide a kind of low cost, the controlled technology of preparing of efficient nylon 6 apertured polymeric film.
The present invention regulates and controls the thickness of gained film by the propelling speed of regulation syringe pump and the caliber of selection capillary;By adjusting The temperature of joint deionized water regulates and controls the size of nylon 6 membrane pore size.
This method preparation process is without any special installation, and technique is simple, with low cost, prepared nylon 6 porous polymer Membrane aperture is uniform, and thickness is controlled, can be applicable to separate, adsorbs, the field such as sensing.
Beneficial effect
(1) present invention uses the nylon of impact resistance and good corrosion resistance as raw material, and gained film mechanical performance is excellent, can be applicable to Separate, adsorb, the field such as sensing;
(2) present invention uses solvent method pore-creating, gained even pore distribution, and pore-creating efficiency is high, and thickness is controlled;
(3) preparation process of the present invention is without template, and method is simple, and flow process is short, and technique is simple, and preparation efficiency is high, with low cost, easily In industrial popularization.
Accompanying drawing explanation
Fig. 1 is the SEM figure of nylon 6 apertured polymeric film in embodiment 1;Wherein, a) it is surface;B) it is section;
Fig. 2 is: a) embodiment 1 gained nylon 6 apertured polymeric film pliability test curve;B) embodiment 1 and 2 gained nylon 6 apertured polymeric film tensile property contrasts.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
(1) being dissolved in formic acid solution by nylon 6 slice, section and acid solution mass ratio are 1:15;Again by solution at 60 DEG C Magnetic agitation 5h under environment;
(2) nylon 6 mixed acid solution that step 1 stirring obtains is advanced by syringe pump, enter capillary, at room temperature warp Capillary instills in the deionized water received in container, can obtain nylon 6 apertured polymeric film in deionized water-Air Interface; The propelling speed of regulation syringe pump is 15mL/min, and selecting internal diameter is the capillary of 0.3mm, and gained film thickness is in 5 μm Left and right;
(3) temperature of deionized water being controlled at 50 DEG C, prepared nylon 6 porous polymer film aperture is 800-1000nm;
(4) nylon 6 porous polymer film that will be formed in deionized water-Air Interface again is transferred to material requested by titanium net Surface.
Fig. 1 is SEM (SEM) photo: a of gained nylon 6 apertured polymeric film in this embodiment) surface; B) section.
Fig. 2 a is gained nylon 6 apertured polymeric film pliability test curve in this embodiment.
Embodiment 2
(1) being dissolved in by nylon 6 slice in the concentrated sulfuric acid, adipic acid, formic acid mixed acid solution, section with acid solution mass ratio is 1:20;Again by solution magnetic agitation 4h under 60 DEG C of environment;
(2) nylon 6 mixed acid solution that step 1 stirring obtains is advanced by syringe pump, enter capillary, at room temperature warp Capillary instills in the deionized water received in container, can obtain nylon 6 apertured polymeric film in deionized water-Air Interface; The propelling speed of regulation syringe pump is 20mL/min, and selecting internal diameter is the capillary of 0.25mm, and gained film thickness is in 2 μm Left and right;
(3) temperature of deionized water being controlled at 30 DEG C, prepared nylon 6 porous polymer film aperture is 500-800nm;
(4) nylon 6 porous polymer film that will be formed in deionized water-Air Interface again is transferred to required table by AAO film Face.
Fig. 2 b is gained nylon 6 apertured polymeric film and gained nylon 6 apertured polymeric film stretching in embodiment 1 in this embodiment Performance comparison.
Embodiment 3
(1) being dissolved in by nylon 6 slice in acetic acid, formic acid, ethanedioic acid mixed acid solution, section with acid solution mass ratio is 1:25;Again by solution magnetic agitation 4h under 70 DEG C of environment;
(2) nylon 6 mixed acid solution that step 1 stirring obtains is advanced by syringe pump, enter capillary, at room temperature warp Capillary instills in the deionized water received in container, can obtain nylon 6 apertured polymeric film in deionized water-Air Interface; The propelling speed of regulation syringe pump is 10mL/min, and selecting internal diameter is the capillary of 2mm, and gained film thickness is left in 8 μm Right;
(3) temperature of deionized water being controlled at 20 DEG C, prepared nylon 6 porous polymer film aperture is 300-600nm;
(4) nylon 6 porous polymer film that will be formed in deionized water-Air Interface again is transferred to material requested by PET Surface.

Claims (6)

1. a preparation method for nylon 6 apertured polymeric film, including:
(1) nylon 6 slice is dissolved in acid solution, 50-80 DEG C of stirring 2-6h, obtains nylon 6 mixed acid solution;
(2) nylon 6 mixed acid solution that stirring in step (1) obtains is advanced by syringe pump, enter capillary, in room temperature Lower in capillary instills the deionized water received in container, nylon 6 porous polymer can be obtained in deionized water-Air Interface Film;Wherein, the propelling speed of syringe pump is 5~50mL/min, and the internal diameter of capillary is 0.25~5mm, the temperature of deionized water Degree is 0~80 DEG C.
The preparation method of a kind of nylon 6 apertured polymeric film the most according to claim 1, it is characterised in that described step (1) Middle nylon 6 slice is 1:10-1:30 with the mass ratio of acid solution.
The preparation method of a kind of nylon 6 apertured polymeric film the most according to claim 1 and 2, it is characterised in that described step Suddenly in (1) acid solution be the concentrated sulfuric acid, hydrochloric acid, formic acid, nitric acid, acetic acid, propionic acid, butyric acid, octanoic acid, adipic acid, ethanedioic acid, At least one in phthalic acid and terephthalic acid (TPA).
The preparation method of a kind of nylon 6 apertured polymeric film the most according to claim 1, it is characterised in that described step (2) Middle capillary is polytetrafluoroethylene (PTFE) material.
The preparation method of a kind of nylon 6 apertured polymeric film the most according to claim 1, it is characterised in that described step (2) Middle nylon 6 apertured polymeric film is transferred to by cellulose membrane, AAO film, PET, PS, aluminium foil, Copper Foil, titanium foil or titanium net Material requested surface.
The preparation method of a kind of nylon 6 apertured polymeric film the most according to claim 1, it is characterised in that described step (2) The thickness of middle nylon 6 porous polymer film is 2~8 μm, and aperture is 300~1000nm.
CN201610146801.8A 2016-03-15 2016-03-15 Method for preparing nylon-6 porous polymer membrane Pending CN105754119A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610146801.8A CN105754119A (en) 2016-03-15 2016-03-15 Method for preparing nylon-6 porous polymer membrane

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610146801.8A CN105754119A (en) 2016-03-15 2016-03-15 Method for preparing nylon-6 porous polymer membrane

Publications (1)

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CN105754119A true CN105754119A (en) 2016-07-13

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103270086A (en) * 2010-12-24 2013-08-28 富士胶片株式会社 Polyamide polymer, method for producing same, resin composition, molded product, fiber, film, and porous film
CN104629066A (en) * 2014-05-09 2015-05-20 中国科学院宁波材料技术与工程研究所 Film self-assembling preparation method and device thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103270086A (en) * 2010-12-24 2013-08-28 富士胶片株式会社 Polyamide polymer, method for producing same, resin composition, molded product, fiber, film, and porous film
CN104629066A (en) * 2014-05-09 2015-05-20 中国科学院宁波材料技术与工程研究所 Film self-assembling preparation method and device thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王纯 等: ""对位芳香族聚酰胺多孔膜制备及性能研究"", 《天津工业大学学报》 *

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Application publication date: 20160713