CN113956519A - Method for temperature-sensitive miniemulsion coating surface abundance metal element - Google Patents
Method for temperature-sensitive miniemulsion coating surface abundance metal element Download PDFInfo
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- CN113956519A CN113956519A CN202111274292.4A CN202111274292A CN113956519A CN 113956519 A CN113956519 A CN 113956519A CN 202111274292 A CN202111274292 A CN 202111274292A CN 113956519 A CN113956519 A CN 113956519A
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- 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
- 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
- C08J2333/24—Homopolymers or copolymers of amides or imides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
- C08K2003/3072—Iron sulfates
Abstract
The invention relates to the fields of aqueous reversed phase colloid, photodegradation, photosensitivity, photoluminescence, photovoltaics and the like, in particular to a method for enriching metal elements on the surface of a thermosensitive miniemulsion coating. Dissolving a temperature-sensitive monomer, a cationic monomer and a water-soluble metal salt in deionized water at room temperature to form a solution A; dissolving an oil-soluble initiator in a solvent to form a solution B; and mixing the solution A and the solution B, quickly transferring the mixture into an ultrasonic biological crusher with a set temperature for crushing, and then raising the temperature to initiate polymerization to form a temperature-sensitive polymer miniemulsion colloid. Diluting the colloid, and forming a film on quartz glass at room temperature by adopting a spin coating film forming or dipping mode; the film-forming quartz glass is placed in a constant-temperature closed space, the relative humidity is kept, and the film with abundant metal ions on the surface is obtained through post-treatment. The invention realizes the migration of metal ions and prepares the film with surface abundance of certain metal ions.
Description
Technical Field
The invention relates to the fields of aqueous reversed phase colloid, photodegradation, photosensitivity, photoluminescence, photovoltaics and the like, in particular to a method for enriching metal elements on the surface of a thermosensitive miniemulsion coating.
Background
The definition of membrane may generally refer to a type of interfacial morphology material used to separate phases. Such as a protective barrier tissue in an organism; and artificially combining the separated-phase membrane material. The artificial membrane forming method can be roughly divided into: 1. volatilization of the solvent or dispersion medium forms a film: the liquid material forms a "wet film" on the article to be coated. The solvent or dispersion medium contained therein is volatilized into the atmosphere, and the viscosity of the wet film is gradually increased to a certain degree to form a solid film. 2. Polymer particles coalesce into a film: in this film formation method, polymer particle film-forming substances are aggregated under a certain condition to form a continuous solid coating film. 3. Chemical film forming method: the flowable film is heated or under other conditions, and intermolecular reaction occurs to further increase the molecular weight of the polymer or crosslink the polymer to form a tough coating film. The membrane is widely applied to the fields of bionics, separation engineering and the like.
Disclosure of Invention
The invention aims to form nanometer temperature-sensitive polymer colloidal particles with the size of 50-300 by adopting inverse miniemulsion polymerization, and pre-loading soluble metal salt. After treatment, spin coating or dipping to form a film, selecting a proper temperature to control the temperature-sensitive polymer to migrate to the surface of the film, and obtaining the film with surface abundance of certain metal elements.
The method comprises the following steps:
(1) synthesizing a thermosensitive polymer miniemulsion colloid containing metal ions:
dissolving a certain amount of temperature-sensitive monomers, cationic monomers and water-soluble metal salt in deionized water at room temperature to form a solution A; dissolving a certain amount of oil-soluble initiator in a solvent to form a solution B; weighing a certain amount of the solution A and the solution B, mixing, quickly transferring into an ultrasonic biological crusher with a preset temperature for crushing, and increasing the temperature for crushing and initiating polymerization after a certain time. Polymerizing for a certain time to form the temperature sensitive polymer miniemulsion colloid.
The temperature-sensitive monomer in the solution A in the step (1) is N-isopropyl acrylamide and the like; the cationic monomer is acryloyloxyethyl trimethyl ammonium chloride or methacryloyloxyethyl trimethyl ammonium chloride and the like; the metal salt can be a mixture of water-soluble salts of more than two different metals, such as copper sulfate, copper nitrate, nickel sulfate, nickel nitrate, ferric sulfate, cadmium nitrate or chromium sulfate;
the mass ratio of the temperature-sensitive monomer, the cationic monomer, the water-soluble metal salt and the deionized water in the solution A is 5:1-5:2: 100;
the solvent in the solution B is isoheptane, and the oil-soluble initiator can be azobisisobutyronitrile or azobisisoheptonitrile; the mass ratio of the oil-soluble initiator to the solvent in the solution B is 1: 500;
mixing a proper amount of the solution A and a proper amount of the solution B to obtain a mixture, and crushing the mixture for 15 minutes in a 90% power state by using an ultrasonic biological crusher at a high power of 500W, wherein the water bath temperature is 10 ℃; then the temperature of the water bath is increased to 60 ℃ to initiate thermal polymerization, and the polymerization time is 50 minutes.
The mass ratio of the solution A to the solution B in the mixture is 100: 500.
(2) Forming a film by miniemulsion:
diluting the metal ion-containing temperature-sensitive polymer miniemulsion colloid prepared in the quantitative step (1), and forming a film on the purified quartz glass by adopting a spin coating film forming or dipping mode at room temperature.
Diluting the metal ion-containing temperature-sensitive polymer miniemulsion colloid prepared in the step (1) by 3-5 volume times, wherein the diluent is isoheptane. The thickness of the spin coating or dipping film is controlled to be 150-200 microns.
(3) Post-treatment to obtain surface abundance certain metal ions:
and (3) placing the film-forming quartz glass prepared in the quantitative step (2) in a constant-temperature closed space, keeping the relative humidity, and performing post-treatment for a certain time to obtain the film with surface abundance and certain metal ions.
In the post-treatment method in the step (3), the temperature of a closed space is 60-70 ℃, the relative humidity is kept at 60%, and the post-treatment time is 4-6 hours.
The invention adopts inverse miniemulsion polymerization to form latex particles, and the latex particles are preloaded with soluble metal salt. Forming a film and obtaining the film with surface abundance of certain metal ions in the film after treatment. The method has potential application prospect in the fields of semiconductors, gas sensitivity, photodegradation, photoluminescence and the like.
The invention has the advantages that the film which transfers certain metal ions and finally has surface abundance of certain ions is realized by utilizing the temperature sensitivity of the N-isopropyl acrylamide and the cationic polymer. Has the following advantages:
1. the metal ion adsorption amount can be controlled by adjusting the proportion of N-isopropyl acrylamide and cationic monomer;
2. the synthesized thermosensitive polymer miniemulsion colloid nano particles containing metal ions have uniform particle size distribution and the size is approximately 100 nanometers;
3. the temperature-sensitive polymer is easy to form a film, and the migration of certain metal ions in the film is realized through temperature and humidity control post-treatment, so that the film with surface abundance of certain metal elements is finally obtained.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
(1) Synthesizing a thermosensitive polymer miniemulsion colloid containing metal ions:
dissolving 5 g of N-isopropylacrylamide, 1 g of acryloyloxyethyltrimethyl ammonium chloride, 1 g of copper sulfate and 1 g of nickel nitrate in 100 g of deionized water at room temperature to form a solution A; dissolving 1 g of azobisisobutyronitrile into 500 g of isoheptane to obtain a solution B; weighing 100 g of the solution A and 500 g of the solution B, mixing, quickly transferring to an ultrasonic biological crusher with a preset temperature, crushing at 90% power for 15 minutes at a high power of 500W, and heating in a water bath at 10 ℃; the temperature of the water bath is raised to 60 ℃ to initiate thermal polymerization, and the polymerization time is 50 minutes. Forming a temperature sensitive polymer miniemulsion colloid.
(2) Forming a film by miniemulsion:
diluting 10 ml of the temperature-sensitive polymer miniemulsion colloid containing the metal ions prepared in the step (1) with 30 ml of isoheptane, forming a film on the purified quartz glass by adopting a spin-coating film forming mode at room temperature, and measuring the film thickness to be 150 microns by an ultrasonic thickness meter.
(3) Post-treatment to obtain a film with surface abundance of certain metal ions:
and (3) placing the film-forming quartz glass prepared in the step (2) in a constant-temperature closed space at 60 ℃, keeping the relative humidity of 60%, and performing post-treatment for 4 hours to obtain the film with surface abundance of certain metal ions. The number percentage of copper elements and nickel elements on the surface is 4:1 through X-ray photoelectron spectroscopy; the percentage of the total copper element and nickel element in the film is about 1:1 by scanning electron microscope elemental analysis. The surface abundance copper metal element obtained by the above method is illustrated.
Example 2
(1) Synthesizing a thermosensitive polymer miniemulsion colloid containing metal ions:
dissolving 5 g of N-isopropylacrylamide, 5 g of methacryloyloxyethyl trimethylammonium chloride, 0.5 g of cadmium sulfate, 0.5 g of nickel nitrate and 1.0 g of ferric sulfate in 100 g of deionized water at room temperature to form a solution A; dissolving 1 g of azobisisobutyronitrile into 500 g of isoheptane to obtain a solution B; weighing 100 g of the solution A and 500 g of the solution B, mixing, quickly transferring to an ultrasonic biological crusher with a preset temperature, crushing at 90% power for 15 minutes at a high power of 500W, and heating in a water bath at 10 ℃; then the temperature of the water bath is increased to 60 ℃ to initiate thermal polymerization, and the polymerization time is 50 minutes. Forming a temperature sensitive polymer miniemulsion colloid.
(2) Forming a film by miniemulsion:
diluting 10 ml of the metal ion-containing temperature-sensitive polymer fine emulsion colloid prepared in the step (1) with 50 ml of isoheptane, forming a film on the purified quartz glass by adopting a dipping film forming mode at room temperature, and measuring the film thickness to be 200 microns by using an ultrasonic thickness meter.
(3) Post-treatment to obtain a film with surface abundance of certain metal ions:
and (3) placing the film-forming quartz glass prepared in the step (2) in a constant-temperature closed space at 70 ℃, keeping the relative humidity of 60%, and performing post-treatment for 6 hours to obtain the film with surface abundance of certain metal ions. Measuring the number percentage of cadmium, nickel and iron on the surface to be 10:2:1 by X-ray photoelectron spectroscopy; the number percentage of cadmium element, nickel element and iron element of the whole element analysis film of the scanning electron microscope is 5:5: 10. The surface abundance cadmium metal element obtained by the method is explained.
Example 3
(1) Synthesizing a thermosensitive polymer miniemulsion colloid containing metal ions:
dissolving 5 g of N-isopropylacrylamide, 3 g of methacryloyloxyethyl trimethylammonium chloride, 0.5 g of lead nitrate, 0.5 g of nickel nitrate and 1.0 g of chromium sulfate in 100 g of deionized water at room temperature to form a solution A; dissolving 1 g of azobisisobutyronitrile into 500 g of isoheptane to obtain a solution B; weighing 100 g of the solution A and 500 g of the solution B, mixing, quickly transferring to an ultrasonic biological crusher with a preset temperature, crushing at 90% power for 15 minutes at a high power of 500W, and heating in a water bath at 10 ℃; then the temperature of the water bath is increased to 60 ℃ to initiate thermal polymerization, and the polymerization time is 50 minutes. Forming a temperature sensitive polymer miniemulsion colloid.
(2) Forming a film by miniemulsion:
diluting 10 ml of the metal ion-containing temperature-sensitive polymer fine emulsion colloid prepared in the step (1) with 40 ml of isoheptane, forming a film on the purified quartz glass by adopting a dipping film-forming mode at room temperature, and measuring the film thickness to be 180 microns by using an ultrasonic thickness meter.
(3) Post-treatment to obtain a film with surface abundance of certain metal ions:
and (3) placing the film-forming quartz glass prepared in the step (2) in a constant-temperature closed space at 65 ℃, keeping the relative humidity of 60%, and performing post-treatment for 5 hours to obtain the film with surface abundance of certain metal ions. Measuring the number percentage of lead element, nickel element and chromium on the surface to be 8:2:1 by X-ray photoelectron spectroscopy; the number percentage of the copper element, the nickel element and the chromium element of the whole element analysis film of the scanning electron microscope is 5:4: 10. The surface abundance lead metal element obtained by the above method is illustrated.
The embodiments described above are presented to enable those skilled in the art to make and use the invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and modifications to the present invention by those skilled in the art according to the present disclosure should be within the scope of the present invention.
Claims (8)
1. A method for preparing abundant metal elements on the surface of a thermosensitive miniemulsion coating film is characterized by comprising the following steps:
(1) synthesizing a thermosensitive polymer miniemulsion colloid containing metal ions:
dissolving a temperature-sensitive monomer, a cationic monomer and a water-soluble metal salt in deionized water at room temperature to form a solution A; dissolving an oil-soluble initiator in a solvent to form a solution B; weighing solution A and solution B, mixing, quickly transferring into an ultrasonic biological crusher with preset temperature for crushing, then increasing the temperature for crushing and initiating polymerization to form a temperature-sensitive polymer miniemulsion colloid;
(2) forming a film by miniemulsion:
diluting the temperature-sensitive polymer miniemulsion colloid containing the metal ions prepared in the step (1), and forming a film on the purified quartz glass by adopting a spin coating film forming or dipping mode at room temperature;
(3) post-treatment to obtain a film with surface abundance of certain metal ions:
and (3) placing the film-forming quartz glass prepared in the step (2) in a constant-temperature closed space, keeping the relative humidity, and performing post-treatment to obtain the film with surface abundance and certain metal ions.
2. The method for enriching the metal element on the surface of the temperature-sensitive miniemulsion coating film according to claim 1, wherein the temperature-sensitive monomer in the solution A in the step (1) is N-isopropylacrylamide; the cationic monomer is acryloyloxyethyl trimethyl ammonium chloride or methacryloyloxyethyl trimethyl ammonium chloride; the metal salt is a mixture of more than two different metal water-soluble salts of copper sulfate, copper nitrate, nickel sulfate, nickel nitrate, ferric sulfate, cadmium nitrate or chromium sulfate.
3. The method for coating surface abundance metal elements with temperature-sensitive miniemulsion according to claim 1, wherein the mass ratio of the temperature-sensitive monomer, the cationic monomer, the water-soluble metal salt and the deionized water in the solution A in the step (1) is 5:1-5:2: 100.
4. The method for preparing abundant metal elements on the surface of the temperature-sensitive miniemulsion coating according to claim 1, wherein the solvent in the solution B in the step (1) is isoheptane, and the oil-soluble initiator is azobisisobutyronitrile or azobisisoheptonitrile; the mass ratio of the oil-soluble initiator to the solvent in the solution B is 1: 500.
5. The method for measuring the abundance of metal elements on the surface of a temperature-sensitive miniemulsion coating film according to claim 1, wherein the mass ratio of the solution A to the solution B in the mixture in the step (1) is 100: 500.
6. The method for coating the abundant metal elements on the surface of the temperature-sensitive miniemulsion according to claim 1, wherein the mixture obtained by mixing the solution A and the solution B in the step (1) is pulverized in a 90% power state for 15 minutes by an ultrasonic biological pulverizer with high power of 500W, the preset temperature is 10 ℃, the temperature is 60 ℃ after temperature rise, and the polymerization time is 50 minutes.
7. The method for detecting the abundance metal elements on the surface of the temperature-sensitive miniemulsion coating film according to claim 1, wherein the colloid of the temperature-sensitive polymer miniemulsion prepared in the step (1) in the step (2) is diluted by 3-5 times by volume, the diluent is isoheptane, and the thickness of the spin-coating or dipping film is controlled to be 150-200 microns.
8. The method for measuring the abundance of metal elements on the surface of the temperature-sensitive miniemulsion coating film according to claim 1, wherein the temperature of the closed space in the post-treatment method in the step (3) is 60-70 ℃, the relative humidity is kept at 60%, and the post-treatment time is 4-6 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114957902A (en) * | 2022-06-22 | 2022-08-30 | 常州大学 | Method for self-assembling functional film by inverse miniemulsion |
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| US20050239957A1 (en) * | 2004-04-21 | 2005-10-27 | Pillsbury Irving W | Composition and method of preparing high solid emulsions |
| CN108948246A (en) * | 2018-06-12 | 2018-12-07 | 常州大学 | The modified phase inversion of solid particle and the method for stablizing Pickering reverse phase miniemulsion |
| CN109233173A (en) * | 2018-08-30 | 2019-01-18 | 成都华点知享知识产权运营有限公司 | A kind of amphipathic particle of hydrogel-solid of stable emulsion and preparation method thereof |
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Patent Citations (4)
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| JP2001049128A (en) * | 1999-08-05 | 2001-02-20 | Mitsubishi Rayon Co Ltd | Metal-containing polymer emulsion, metal-containing high polymer and their production |
| US20050239957A1 (en) * | 2004-04-21 | 2005-10-27 | Pillsbury Irving W | Composition and method of preparing high solid emulsions |
| CN108948246A (en) * | 2018-06-12 | 2018-12-07 | 常州大学 | The modified phase inversion of solid particle and the method for stablizing Pickering reverse phase miniemulsion |
| CN109233173A (en) * | 2018-08-30 | 2019-01-18 | 成都华点知享知识产权运营有限公司 | A kind of amphipathic particle of hydrogel-solid of stable emulsion and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| ZHANG ZHENQIAN等: "Preparation of CdFe2O4-polymeric nanoparticles by inverseminiemulsion and its film properties", 《COLLOIDS AND SURFACES A: PHYSICOCHEMICAL AND ENGINEERING ASPECTS》, vol. 495, pages 100 - 109, XP029453447, DOI: 10.1016/j.colsurfa.2016.02.010 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114957902A (en) * | 2022-06-22 | 2022-08-30 | 常州大学 | Method for self-assembling functional film by inverse miniemulsion |
| CN114957902B (en) * | 2022-06-22 | 2023-09-26 | 常州大学 | Method for self-assembling functional film by reverse miniemulsion |
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