CN108715646B - Method for preparing large amount of uniform non-spherical Janus particles - Google Patents
Method for preparing large amount of uniform non-spherical Janus particles Download PDFInfo
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- CN108715646B CN108715646B CN201810569940.0A CN201810569940A CN108715646B CN 108715646 B CN108715646 B CN 108715646B CN 201810569940 A CN201810569940 A CN 201810569940A CN 108715646 B CN108715646 B CN 108715646B
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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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
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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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/16—Chemical modification with polymerisable 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
- C08J2325/00—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 at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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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
- C08J2333/04—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 esters
- C08J2333/06—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 esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
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Abstract
The invention discloses a method for preparing a large number of uniform non-spherical Janus particles, which is based on a gas-liquid interface, adopts uniform monodisperse colloid particles as a raw material, takes a volatile solvent as an etching agent, prepares non-spherical particles with regular shapes and various shapes along with the prolonging of time, and adjusts the particle size according to the size of template particles, so that the yield can reach more than 95 percent. The non-spherical particles belong to the Janus asymmetric particles, can be used for simulating the self-assembly of colloidal particles, and are beneficial to people to know the self-assembly phenomenon of microscopic colloidal particles.
Description
Technical Field
The invention belongs to the technical field of colloid chemistry, and particularly relates to a method for preparing a large number of non-spherical particles by asymmetrically etching colloid particles by utilizing gas volatilized by a volatile organic solvent.
Background
The main method for preparing the asymmetric colloidal particles at present is as follows: phase separation, microfluidics, interfacial protection (two-dimensional, three-dimensional, etc.), block copolymer self-assembly, etc., all of which use spherical particles as templates or products, and chemically or physically distinguish the chemical components or structures of the hemispheres of the spherical microparticles from one another to obtain asymmetric particles with different functions. The method for preparing the non-spherical particles is less, and mainly comprises a solvent swelling and volatilizing method or a thermal deformation method, wherein the solvent swelling and volatilizing method firstly swells spherical particles in an organic solvent, then protects one surface of the spherical particles and enables the other surface of the spherical particles to be placed in the air, and the particles in half of the particles placed in the air can generate asymmetric deformation in the volatilizing process of the organic solvent, but the particles produced by the method have poor uniformity and serious particle agglomeration phenomenon, and cannot be produced in a large scale; in the latter, the particles are deformed by the thermal environment generated by a high-temperature high-pressure reaction kettle, but the method can destroy the structure of the particles to a certain extent, and the produced particles have rough surfaces and serious adhesion among the particles.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing non-spherical Janus particles in a large area, which is simple to operate and mild in condition and is rapid.
The technical scheme for solving the technical problems is as follows: ultrasonically dispersing spherical colloidal particles in a mixed solution of ethanol and deionized water, dropwise adding the obtained dispersion liquid onto the surface of the deionized water to enable the colloidal particles to form a single-layer colloidal crystal on a gas-liquid interface, then placing the single-layer colloidal crystal and a corresponding etching agent in a closed system, and etching the part of the colloidal particles exposed on the water surface by utilizing the volatile gas of the etching agent to obtain the non-spherical Janus particles.
The spherical colloidal particles are non-crosslinked polystyrene microspheres, non-crosslinked polymethyl methacrylate microspheres, non-crosslinked polyacrylic acid microspheres, and SiO2Any one of the microspheres. When the spherical colloidal particles are non-crosslinked polystyrene microspheres, non-crosslinked polymethyl methacrylate microspheres or non-crosslinked polyacrylic acid microspheres, the corresponding etching agent is any one or a mixture of more than two of dichloromethane, toluene and tetrahydrofuran, or a mixed solution of any one or a mixture of more than two of the dichloromethane, the toluene and the tetrahydrofuran and ethanol; when the spherical colloidal particles are crosslinked polymethyl methacrylate microspheres, the corresponding etching agent is styrene; when the spherical colloidal particles are SiO2When the microspheres are used, the corresponding etching agent is hydrogen fluoride.
In the preparation method, preferably, the spherical colloidal particles are ultrasonically dispersed in a mixed solution of ethanol and deionized water in a volume ratio of 1: 9-5: 5.
The invention has the following beneficial effects:
according to the invention, no other surfactant is needed to be added, colloidal particles are only needed to be dispersed in a solution of ethanol and water, the dispersion liquid is dropwise added onto the surface of deionized water, hexagonal close-packed monolayer colloidal crystals can be formed at a gas-liquid interface, and then the hexagonal close-packed monolayer colloidal crystals are etched by using gas volatilized from an etching agent at normal temperature, so that uniform non-spherical Janus particles can be formed. The method has the advantages of simple operation, mild conditions, high yield and wide application range, can effectively etch cross-linked or non-cross-linked colloidal particles with different particle diameters, and has potential significance in the aspect of colloidal particle self-assembly.
Drawings
FIG. 1 is a FESEM photograph of non-spherical polystyrene particles obtained in example 1 when the etching time was 5 min.
FIG. 2 is a FESEM image of non-spherical polystyrene particles obtained in example 2 at an etching time of 45 min.
FIG. 3 is a FESEM photograph of non-spherical polystyrene particles obtained in example 3 when the etching time was 95 min.
FIG. 4 is an FESEM photograph of non-spherical polymethyl methacrylate particles obtained in example 4 when the etching time was 20 min.
FIG. 5 is an FESEM photograph of non-spherical polymethyl methacrylate particles obtained in example 5 when the etching time was 30 min.
Detailed Description
The invention will be further explained in more detail below with reference to the drawings and examples, but the scope of protection of the invention is not limited to these examples.
Example 1
Adding polystyrene microspheres with the particle size of 1.2 microns into a mixed solution of 2mL of ethanol and 8mL of deionized water, performing ultrasonic dispersion for 10min to uniformly mix the polystyrene microspheres, and then slowly dropwise adding the obtained dispersion into a 100mL beaker containing 80mL of deionized water to rapidly form single-layer large-area close-packed polystyrene microspheres on a gas-liquid interface. Then, the beaker is placed inside a 1000mL beaker, 20mL of dichloromethane is poured into the 1000mL beaker, the beaker is sealed and stands for 5min, and the volatile dichloromethane gas can etch the exposed part of the polystyrene microspheres on the water surface, so that the non-spherical polystyrene particles shown in FIG. 1 are obtained.
Example 2
In this example, the sealing and standing time was 45min, and the other steps were the same as in example 1, to obtain non-spherical polystyrene particles shown in FIG. 2.
Example 3
In this example, the sealing and standing time was 95min, and the other steps were the same as in example 1, to obtain non-spherical polystyrene particles shown in FIG. 3.
Example 4
Adding polymethyl methacrylate microspheres with the particle size of 1 mu m into a mixed solution of 2mL of ethanol and 8mL of deionized water, carrying out ultrasonic dispersion for 10min to uniformly mix the microspheres, and then slowly dropwise adding the obtained dispersion into a 100mL beaker containing 80mL of deionized water to rapidly form single-layer large-area close-packed polymethyl methacrylate microspheres on a gas-liquid interface. Then, the beaker is placed inside a 1000mL beaker, 10mL of dichloromethane and 10mL of anhydrous ethanol are poured into the 1000mL beaker, the beaker is sealed and stands for 20min, and the volatile dichloromethane gas can etch the part of the polymethyl methacrylate microspheres exposed on the water surface, so that the non-spherical polymethyl methacrylate particles shown in FIG. 1 are obtained.
Example 5
In this example, the sealing and standing time was 30min, and the other steps were the same as in example 4, to obtain non-spherical PMMA particles shown in fig. 5.
Example 6
Adding crosslinked polymethyl methacrylate with the particle size of 1 mu m into a mixed solution of 2mL of ethanol and 8mL of deionized water, performing ultrasonic dispersion for 10min to uniformly mix the crosslinked polymethyl methacrylate and the ethanol, and then slowly dropwise adding the obtained dispersion into a 100mL beaker containing 80mL of deionized water to rapidly form a single-layer large-area close-packed crosslinked polymethyl methacrylate microsphere at a gas-liquid interface. And then placing the beaker in a 1000mL beaker, pouring 20mL of styrene into the 1000mL beaker, sealing and standing for 20min, and etching the exposed part of the crosslinked polymethyl methacrylate microspheres on the water surface by the volatilized styrene gas to obtain the non-spherical crosslinked polymethyl methacrylate particles.
Example 7
In this example, methylene chloride in example 1 was replaced with toluene of the same volume, and the resultant was sealed and allowed to stand for 20min, and the other steps were the same as in example 1, to obtain non-spherical polystyrene particles.
Claims (1)
1. A method of making a plurality of uniform non-spherical Janus particles, comprising: ultrasonically dispersing spherical colloidal particles in a mixed solution of ethanol and deionized water in a volume ratio of 1: 9-5: 5, dropwise adding the obtained dispersion liquid onto the surface of the deionized water to enable the colloidal particles to form a single-layer colloidal crystal on a gas-liquid interface, then placing the single-layer colloidal crystal and a corresponding etching agent in a closed system, and etching the part, exposed on the water surface, of the colloidal particles by utilizing the volatile gas of the etching agent to obtain non-spherical Janus particles;
the spherical colloidal particles are any one of non-crosslinked polystyrene microspheres, non-crosslinked polymethyl methacrylate microspheres, crosslinked polymethyl methacrylate microspheres and non-crosslinked polyacrylic acid microspheres;
when the spherical colloidal particles are non-crosslinked polystyrene microspheres, non-crosslinked polymethyl methacrylate microspheres or non-crosslinked polyacrylic acid microspheres, the corresponding etchant is any one or a mixture of two of dichloromethane and toluene, or a mixed solution of any one or a mixture of two of dichloromethane and toluene and ethanol;
when the spherical colloidal particles are crosslinked polymethyl methacrylate microspheres, the corresponding etching agent is styrene.
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| CN201810569940.0A CN108715646B (en) | 2018-06-05 | 2018-06-05 | Method for preparing large amount of uniform non-spherical Janus particles |
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| CN201810569940.0A CN108715646B (en) | 2018-06-05 | 2018-06-05 | Method for preparing large amount of uniform non-spherical Janus particles |
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| CN108715646B true CN108715646B (en) | 2020-11-17 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102162136A (en) * | 2011-02-28 | 2011-08-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for quick preparation of large-area two-dimensional colloidal crystal |
| CN103524770A (en) * | 2013-08-28 | 2014-01-22 | 中国科学院福建物质结构研究所 | 3D (Three Dimensional) printing product surface polishing method and device thereof |
| CN105601958A (en) * | 2015-12-28 | 2016-05-25 | 江南大学 | Preparation of Janus polymer particle |
| CN107540863A (en) * | 2017-07-28 | 2018-01-05 | 昆明理工大学 | Inside is the preparation method of hollow or loose structure totally-enclosed polymer microballoon |
-
2018
- 2018-06-05 CN CN201810569940.0A patent/CN108715646B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102162136A (en) * | 2011-02-28 | 2011-08-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for quick preparation of large-area two-dimensional colloidal crystal |
| CN103524770A (en) * | 2013-08-28 | 2014-01-22 | 中国科学院福建物质结构研究所 | 3D (Three Dimensional) printing product surface polishing method and device thereof |
| CN105601958A (en) * | 2015-12-28 | 2016-05-25 | 江南大学 | Preparation of Janus polymer particle |
| CN107540863A (en) * | 2017-07-28 | 2018-01-05 | 昆明理工大学 | Inside is the preparation method of hollow or loose structure totally-enclosed polymer microballoon |
Non-Patent Citations (1)
| Title |
|---|
| Asymmetric deformation of swollen microspheres on a water surface;Likui Wang et al.;《RSC Advances》;20160518;第6卷;第50368-50372页 * |
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