CN109485882B - Preparation method of self-supporting film - Google Patents
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- CN109485882B CN109485882B CN201811156834.6A CN201811156834A CN109485882B CN 109485882 B CN109485882 B CN 109485882B CN 201811156834 A CN201811156834 A CN 201811156834A CN 109485882 B CN109485882 B CN 109485882B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- C—CHEMISTRY; METALLURGY
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- C08J2331/00—Characterised by the use of copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, or carbonic acid, or of a haloformic acid
- C08J2331/02—Characterised by the use of omopolymers or copolymers of esters of monocarboxylic acids
- C08J2331/04—Homopolymers or copolymers of vinyl acetate
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08J2431/00—Characterised by the use of copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, or carbonic acid, or of a haloformic acid
- C08J2431/02—Characterised by the use of omopolymers or copolymers of esters of monocarboxylic acids
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- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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Abstract
The invention provides a preparation method of a self-supporting film, which is prepared by dialyzing emulsion with saturated NaCl solution. The self-supporting film prepared by the method has the advantages of simplicity and convenience in operation, rapidness in film forming, environment friendliness, large-area preparation and the like, and is expected to be practically applied to the fields of preparation and application of the self-supporting film, adhesive preparation, sensors, catalytic industry and biomedical treatment.
Description
Technical Field
The invention belongs to the technical field of film making, and particularly relates to a preparation method of a self-supporting film.
Background
Along with the continuous improvement of the requirements of the membrane, the self-supporting membrane is paid more attention to by more scientists due to the advantages of high flexibility, great aspect ratio and the like, and has great application prospect in the aspects of high-strength membranes, conductive membranes, separation membranes, catalytic membranes, sensors and the like.
Hitherto, various methods for preparing self-supporting films such as a sacrificial layer method, a substrate stripping method, an interfacial method, a direct stripping method and the like have been commonly used, but the above-mentioned techniques have the disadvantages of more or less complicated preparation process, high requirements on stability, variety and assembly conditions of the films, limited preparation area and the like, so that the existing self-supporting film has the disadvantages of low preparation efficiency, narrow selectivity and larger limitation.
The technology selects a saturated NaCl solution to prepare a single-layer, double-layer and composite self-supporting film by a dialysis method. The defects of complex preparation process, high substrate selectivity, limited preparation area and the like on the basis of the prior art are overcome, and the preparation method plays an important role in the future preparation and application fields of the self-supporting film.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a self-supporting film.
The preparation method of the self-supporting film comprises the following steps and conditions:
the invention relates to abbreviated Chinese names: PVAc is polyvinyl acetate emulsion, PVA is polyvinyl alcohol, OP-10 is polyoxyethylene octyl phenol ether-10, SDS is sodium dodecyl sulfonate, KPS is potassium persulfate, VAc is vinyl acetate, and DBP is dibutyl phthalate. 906 is an acrylic tackifying emulsion.
The invention provides a method for preparing a latex film on a metal surface by electrodeposition, which comprises the following steps:
two types of emulsions are used, wherein one type is 906 emulsion, the other type is PVAc emulsion, the 906 emulsion is purchased from the market, and the PVAc emulsion is self-made emulsion of the invention, and the specific method is as follows:
(1) 906 emulsion
The 906 emulsion is purchased from four Confucius Pondelia chemical industry Co., ltd, has pH of 4.0-7.0, solid content of 52.0+ -2.0, and viscosity of 300-1000cps.
(2) Preparation of PVAc emulsion
At room temperature, 3g of PVA and 27g of deionized water were placed in a reactor, and heated to 90℃for dissolution, to prepare a PVA solution. Then 12mL of deionized water, 0.8mL of OP-10,0.25g of SDS,2mL of KPS solution with mass volume concentration of 10mg/mL, 5mL of Vac are added to the solution, and the mixture is refluxed and stirred in a water bath at 70 ℃ for 1h. Then, 27mL of VAc and 6mL of KPS having a mass-volume concentration of 10mg/mL were alternately added to the reaction solution, and the dropping time was 2 hours. Immediately after the temperature was increased to 90℃and the reaction was completed without reflux, the reaction was cooled to 50℃and the pH was adjusted to 5. Finally, 9g of DBP is put into a container to react for 30min to obtain PVAc emulsion.
(3) Cleaning of substrates
The substrate used for preparing the support membrane is a dialysis membrane with the molecular weight cutoff of 8000-14000. Placing the dialysis membrane in a mixed solution of absolute ethyl alcohol and water in a volume ratio of 1:1, heating to 80 ℃ and boiling the solution for 40min, and then washing with deionized water for later use;
the saturated NaCl solution is added into a container, then the treated dialysis membrane is placed on the surface of the saturated NaCl solution to float, and then the container is placed in a closed device.
(4) Preparation of monolayer self-supporting films
The emulsion is coated on the surface of the dialysis membrane, and after 1-30min, the single-layer self-supporting membrane with the thickness of 68+/-8.36-568+/-60.6 mu m can be prepared.
(5) Preparation of bilayer self-supporting films
The emulsion is coated on the surface of the dialysis membrane, after 1-30min, a single-layer self-supporting membrane with the thickness of 68+/-8.36-568+/-60.6 mu m can be prepared, then another emulsion is coated on the surface of the single-layer self-supporting membrane, and after 1-30min, a double-layer self-supporting membrane with the thickness of 170+/-23-1254+/-72.3 mu m can be prepared.
(6) Preparation of composite self-supporting film
The volume ratio of the two emulsions with good compatibility is 1:1 are mixed together in proportion and stirred for 48 hours to be uniformly mixed together. And then coating the mixed emulsion on a dialysis membrane for dialysis, thus preparing the composite self-supporting membrane.
Detailed Description
The following examples further illustrate the practice and results of the present invention and are not intended to limit the invention thereto.
Example 1 a method for preparing a self-supporting film, the emulsion being PVAc, the steps and conditions for preparation being as follows:
(1) Preparation of PVAc emulsion
At room temperature, 3g of PVA and 27g of deionized water are firstly placed in a four-neck flask, heated and dissolved at 90 ℃ to obtain PVA solution, then 12mL of deionized water, 0.8mL of OP-10,0.25g of SDS,2mL of KPS solution with mass volume concentration of 10mg/mL and 5mL of VAc are sequentially added, and the mixture is refluxed and stirred in a water bath at 70 ℃ for reaction for 1h. Then, 27mL of VAc and 6mL of KPS having a mass-volume concentration of 10mg/mL were alternately added to the reaction solution, and the addition was completed within 2 hours. Then the temperature was raised to 90℃and the reaction was cooled to 50℃after no reflux. The pH was adjusted to 5. Finally, 9g of DBP was added and reacted for 30min. The PVAc emulsion is prepared.
(2) Cleaning of substrates
The substrate used for preparing the support membrane is a dialysis membrane with the molecular weight cutoff of 8000-14000. Placing the dialysis membrane in a mixed solution of absolute ethyl alcohol and water in a volume ratio of 1:1, heating to 80 ℃ and boiling the solution for 40min, and then washing with deionized water for later use;
the saturated NaCl solution is added into a container, then the treated dialysis membrane is placed on the surface of the saturated NaCl solution to float, and then the container is placed in a closed device.
(3) Preparation of monolayer self-supporting films
And (3) coating PVAc on the surface of the dialysis membrane for 1min to prepare the single-layer PVAc self-supporting membrane with the thickness of 88+/-14.83 mu m.
Example 2 a method for preparing a self-supporting film, the emulsion being PVAc with 906, the steps and conditions for preparation being as follows:
(1) Preparation of PVAc emulsion
At room temperature, 3g of PVA and 27g of deionized water are firstly placed in a four-neck flask, heated and dissolved at 90 ℃ to obtain PVA solution, then 12mL of deionized water, 0.8mL of OP-10,0.25g of SDS,2mL of KPS solution with mass volume concentration of 10mg/mL and 5mL of VAc are sequentially added, and the mixture is refluxed and stirred in a water bath at 70 ℃ for reaction for 1h. Then, 27mL of VAc and 6mL of KPS having a mass-volume concentration of 10mg/mL were alternately added to the reaction solution, and the addition was completed within 2 hours. Then the temperature was raised to 90℃and the reaction was cooled to 50℃after no reflux. The pH was adjusted to 5. Finally, 9g of DBP was added and reacted for 30min. The PVAc emulsion is prepared.
(2) Cleaning of substrates
The substrate used for preparing the support membrane is a dialysis membrane with the molecular weight cutoff of 8000-14000. Placing the dialysis membrane in a mixed solution of absolute ethyl alcohol and water in a volume ratio of 1:1, heating to 80 ℃ and boiling the solution for 40min, and then washing with deionized water for later use;
the saturated NaCl solution is added into a container, then the treated dialysis membrane is placed on the surface of the saturated NaCl solution to float, and then the container is placed in a closed device.
(3) Preparation of bilayer self-supporting films
And (3) coating the 906 emulsion on the surface of the dialysis membrane for 1min to prepare a single-layer self-supporting membrane with the thickness of 68+/-8.36 mu m, and then coating PVAc on the surface of the single-layer self-supporting membrane for 1min to prepare the double-layer self-supporting membrane with the thickness of 176+/-11.40 mu m.
Example 3 a method for preparing a self-supporting film, the emulsion being PVAc with 906, the steps and conditions for preparation being as follows:
(1) Preparation of PVAc emulsion
At room temperature, 3g of PVA and 27g of deionized water are firstly placed in a four-neck flask, heated and dissolved at 90 ℃ to obtain PVA solution, then 12mL of deionized water, 0.8mL of OP-10,0.25g of SDS,2mL of KPS solution with mass volume concentration of 10mg/mL and 5mL of VAc are sequentially added, and the mixture is refluxed and stirred in a water bath at 70 ℃ for reaction for 1h. Then, 6mL of KPS having a mass-volume concentration of 10mg/mL and 27mL of VAc were alternately added to the reaction solution, and the addition was completed within 2 hours. Then the temperature was raised to 90℃and the reaction was cooled to 50℃after no reflux. The pH was adjusted to 5. Finally, 9g of DBP was added and reacted for 30min. The PVAc emulsion is prepared.
(2) Cleaning of substrates
The substrate used for preparing the support membrane is a dialysis membrane with the molecular weight cutoff of 8000-14000. Placing the dialysis membrane in a mixed solution of absolute ethyl alcohol and water in a volume ratio of 1:1, heating to 80 ℃ and boiling the solution for 40min, and then washing with deionized water for later use;
the saturated NaCl solution is added into a container, then the treated dialysis membrane is placed on the surface of the saturated NaCl solution to float, and then the container is placed in a closed device.
(3) Preparation of composite self-supporting film
PVAc and 906 are mixed according to the volume ratio of 1:1 are mixed together in proportion and stirred for 48 hours to be uniformly mixed together. And then the mixed emulsion is coated on a dialysis membrane for dialysis, thus preparing the composite self-supporting membrane with the thickness of 900+/-190 mu m.
Claims (3)
1. A method for preparing a self-supporting film, characterized by the following steps and conditions:
chinese name of the abbreviation: PVAc is polyvinyl acetate emulsion, PVA is polyvinyl alcohol, OP-10 is polyoxyethylene octyl phenol ether-10, SDS is sodium dodecyl sulfonate, KPS is potassium persulfate, VAc is vinyl acetate, DBP is dibutyl phthalate, 906 is acrylic acid tackifying emulsion;
a method for preparing a latex film by electrodeposition on a metal surface, comprising the following steps and conditions: two emulsions are used, wherein one is 906 emulsion and the other is PVAc emulsion, the 906 emulsion is purchased from the market, and the PVAc emulsion is self-made emulsion, and the specific method is as follows:
(1) 906 emulsion
906 emulsion is purchased from four-conference Pondelia chemical industry Co., ltd, and has pH value of 4.0-7.0, solid content of 52.0 s 2.0, and viscosity of 300-1000cps;
(2) Preparation of PVAc emulsion
At room temperature, 3g of PVA and 27g of deionized water are put into a reactor, and heated to 90 ℃ for dissolution, so as to prepare PVA solution; then adding 12mL of deionized water, 0.8mL of OP-10,0.25g of SDS,2mL of KPS solution with the mass volume concentration of 10mg/mL and 5mL of VAc into the solution, and refluxing and stirring in a water bath at 70 ℃ for 1h; then, 27mL of VAc and 6mL of KPS with the mass volume concentration of 10mg/mL are alternately added into the reaction solution, and the dropping time is 2h; immediately raising the temperature to 90 ℃, ending the reaction when no reflux exists, cooling to 50 ℃, and adjusting the pH to 5; finally, 9g of DBP is put into a container to react for 30min to obtain PVAc emulsion;
(3) Cleaning of substrates
The substrate used for preparing the self-supporting membrane is a dialysis membrane with molecular weight cutoff of 8000-14000; the dialysis membrane was placed in a volume ratio of 1:1, heating the mixture of absolute ethyl alcohol and water to 80 ℃ to boil the solution for 40min, and then washing the solution with deionized water for later use;
adding saturated NaCl solution into a container, placing the treated dialysis membrane on the surface of the saturated NaCl solution to float the membrane, and placing the container into a closed device;
(4) Preparation of monolayer self-supporting films
Coating the emulsion on the surface of a dialysis membrane, and preparing a single-layer self-supporting membrane with the thickness of 68+/-8.36-568+/-60.6 mu m after 1-30 min;
(5) Preparation of bilayer self-supporting films
Coating the emulsion on the surface of a dialysis membrane, preparing a single-layer self-supporting membrane with the thickness of 68+/-8.36-568+/-60.6 mu m after 1-30min, coating another emulsion on the surface of the single-layer self-supporting membrane, and preparing a double-layer self-supporting membrane with the thickness of 170+/-23-1254+/-72.3 mu m after 1-30 min;
(6) Preparation of composite self-supporting film
The volume ratio of 906 to PVAc emulsion is 1:1, stirring for 48 hours to uniformly mix the materials together; and then coating the mixed emulsion on a dialysis membrane for dialysis, thus preparing the composite self-supporting membrane.
2. The method of claim 1, wherein the self-supporting film is prepared in a closed apparatus.
3. The method of claim 1, wherein the number of layers of the self-supporting film is a single layer, a multi-layer or a composite single layer self-supporting film.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101091945A (en) * | 2007-07-26 | 2007-12-26 | 吉林大学 | Method for preparing laminar assembled self-supporting membrane by using ion lift-off technology |
| CN101381429A (en) * | 2008-07-18 | 2009-03-11 | 华南师范大学 | Self-supporting lithium ionic cell gel polymer electrolyte, special polymer and preparation method and application thereof |
| CN103212310A (en) * | 2013-03-29 | 2013-07-24 | 北京工业大学 | Modified polyvinyl chloride acetate flat micro filtration membrane preparation method |
| WO2017071267A1 (en) * | 2015-10-30 | 2017-05-04 | 广州市电纺生物科技有限公司 | Double layer-structured anti-adhesion film and manufacturing method therefor |
| CN108504302A (en) * | 2018-04-08 | 2018-09-07 | 长春理工大学 | A kind of high molecular bonding film with water-proof function |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101091945A (en) * | 2007-07-26 | 2007-12-26 | 吉林大学 | Method for preparing laminar assembled self-supporting membrane by using ion lift-off technology |
| CN101381429A (en) * | 2008-07-18 | 2009-03-11 | 华南师范大学 | Self-supporting lithium ionic cell gel polymer electrolyte, special polymer and preparation method and application thereof |
| CN103212310A (en) * | 2013-03-29 | 2013-07-24 | 北京工业大学 | Modified polyvinyl chloride acetate flat micro filtration membrane preparation method |
| WO2017071267A1 (en) * | 2015-10-30 | 2017-05-04 | 广州市电纺生物科技有限公司 | Double layer-structured anti-adhesion film and manufacturing method therefor |
| CN108504302A (en) * | 2018-04-08 | 2018-09-07 | 长春理工大学 | A kind of high molecular bonding film with water-proof function |
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