CN105601951A - Fast preparing method of gel photon crystal - Google Patents
Fast preparing method of gel photon crystal Download PDFInfo
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- 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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- 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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- 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
- C08J2429/00—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 alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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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
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
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Abstract
The invention discloses a fast preparing method of a gel photon crystal. The fast preparing method comprises the following steps: (1) dispersing a monomer in water to prepare emulsion with a mass percent of 15-30 percent, heating the emulsion to 90 DEG C, then adding an initiator with a mass percent of 0.5-2 percent, and reacting for 0.5-2h to prepare nano particle suspension; (2) adding a high molecular material into the nano particle suspension, controlling the temperature at 90 DEG C, and reflowing for 1-2h to obtain high molecular pregel; (3) adding resin exchange resin into the high molecular pregel, cooling the temperature to 50 DEG C, and performing purification for 2 to 10 hours to obtain a photon crystal pregel; (4) adding the photon crystal pregel into a syringe, injecting into a die, sealing the die, then placing in an environment of -20-0 DEG C for freezing for 2-24h, and then unfreezing in an environment of 20-25 DEG C for 0.5-1h or curing in an oven of 60 DEG C for 2h, and demoulding to obtain the gel photon crystal. The preparing method can improve the yield of the gel photon crystal and achieves economic, energy-saving and environment protecting effects.
Description
Technical field
The present invention relates to photonic crystal technical field, particularly a kind of quick preparation side of gel photonic crystalMethod.
Background technology
Photonic crystal is a kind of structure of dielectric constant periodic modulation, it is characterized in that having forbidden photon band. Work as electricityWhen magnetic wave is propagated in this periodic structure, the ripple that frequency and forbidden photon band match can be controlled; According to lightThis characteristic of sub-crystal, can design different periodic structures, thereby realizes the control to Electromagnetic Wave Propagation modeSystem, this class material has had wide range applications in fields such as optical circuit, communication sensing, optical memories; WhenThe forbidden band of photon crystal material is in visible-range time, and material can present bright-coloured schemochrome in macroscopic view,Can be applicable to the aspects such as Laser Devices, structural anti false, novel printing.
Taking the hydrogel of environmental response as matrix, the gel photon crystalline substance prepared as primitive of the photonic crystal that can develop the colorBody material, can produce volume breathing according to environmental change by hydrogel matrix, drives inner photonic crystalThe crystal lattice constant change of primitive, is moved the forbidden photon band position of material monolithic, and macroscopic view is presented as gelThe variation of photon crystal structure look. In the time that change color can be identified by naked eyes, can be applied to visualChange sensor material; Manufacture this class photonic crystal sensor material, conventionally need to first synthesize mono-dispersed nano micro-Ball, is arranged in the crystal array with periodic structure in the mode of electrostatic self-assembled, then by monomer, crosslinkedThis array of the infiltration such as agent, light trigger, utilizes the polymerization of ultraviolet light trigger monomer, is forming polyalcohol hydrogelIn time, is fixed crystal array. Selection has photon crystalline substance prepared by the polyalcohol hydrogel of different sensitivity characteristicsBody sensor can produce color response to specific environmental stimulus, such as, adopt temperature-sensitive hydrogel to buildPhotonic crystal sensors variations in temperature can be shown as to change color, in addition, gel photonic crystal sensingDevice can also be realized the response to various outside stimulus such as pH, magnetic field, stress, molecules.
At present, prepare above-mentioned gel photonic crystal material required time all very of a specified duration, this is due to photonic crystalAssembling process slower, need the impurity in long dialysis removal system, the common warp of this processGo through 14-21 days, and follow-up gel encapsulation process also must, through the purge process of certain hour, keepSystem is pure.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of can overcome the preparation time that prior art exists long,The fast preparation method of a kind of gel photonic crystal of the problems such as complex process.
For achieving the above object, technical scheme of the present invention is as follows:
A fast preparation method for gel photonic crystal, described fast preparation method comprises the steps:
(1) monomer is dispersed in water, is mixed with the emulsion that mass fraction is 15-30%, by emulsionBe warming up to 90 DEG C, then adding mass fraction is the initator of 0.5-2%, obtains through reaction in 0.5-2 hourNano granule suspension;
(2) macromolecular material is added in nano granule suspension, temperature is controlled at 90 DEG C, backflow 1-2Hour, obtain macromolecule pregel;
(3) ion exchange resin is added in macromolecule pregel, and cool to 50 DEG C, purifying 2-10 is littleTime, obtain photonic crystal pregel;
(4) photonic crystal pregel is joined in syringe, then be injected in mould, mould is sealedFreezing 2-24 hour in the environment of be placed on-20-0 DEG C, 0.5-1 then thaws in the environment of 20-25 DEG CHour, or be placed in 60 DEG C of baking ovens curing 2 hours, and get final product the demoulding, obtain gel photonic crystal.
Preferably, described monomer is alkene type organic, its be styrene, methacrylate, acrylic acid withAnd one or more in acrylamide.
Preferably, described initator is ammonium persulfate or potassium peroxydisulfate.
Preferably, described initator is azodiisobutyronitrile or ABVN.
Preferably, described macromolecular material is polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, poly-ammoniaOne or more in ester and PLA.
Preferably, described ion exchange resin is mixed-bed resin, and cation and anion ratio are 1:2-1:5.
By technique scheme, the invention has the beneficial effects as follows:
(1) the present invention compared with prior art, has overcome conventional gel photonic crystal material preparation process slowShortcoming, a kind of method that can prepare fast gel photonic crystal device is provided, can improve productive rate,Play again the effect of economical and energy saving and protection of the environment;
(2) select different macromolecular materials, prepared gel photonic crystal has different mechanical strengthsAnd environmental response characteristic, as pH, temperature, stress etc.
(3) gel photonic crystal material of preparing with the present invention, can be used as mould material for further changingProperty obtains other senser elements.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the invention process process;
Implementation process comprises: synthesis of nano particle, add macromolecular material and ion exchange resin and gel.
Detailed description of the invention
For technological means, creation characteristic that the present invention is realized, reach object and effect is easy to understand,Further set forth the present invention below.
Shown in Figure 1, Fig. 1 is the schematic flow sheet of the invention process process;
Embodiment 1
The invention discloses a kind of fast preparation method of gel photonic crystal, this fast preparation method comprise asLower step:
(1) 50 grams of styrene are dispersed in 150 grams of water, are mixed with mass fraction and are 25% emulsion,Emulsion is warming up to 90 DEG C, then adds 1 gram of potassium peroxydisulfate, obtain polystyrene through reaction in 1 hour and receiveRice grain suspension;
(2) 20 grams of polyvinyl alcohol and 10 grams of polyethylene glycol are added in polystyrene nanoparticles suspension,Temperature is controlled at 90 DEG C, refluxes 1 hour, obtains polyvinyl alcohol/polyethylene glycol pregel;
(3) mixed-bed resin that is 1:2 by cation and anion ratio adds polyvinyl alcohol/polyethylene glycol pre-In gel, and cool to 50 DEG C, purifying 6 hours, obtains photonic crystal pregel;
(4) photonic crystal pregel is injected in mould with micro syringe, mould sealing is placed onIn the environment of-18 DEG C freezing 24 hours, then in the environment of 20 DEG C, thaw 1 hour, get final product the demoulding,Obtain polyvinyl alcohol/polyethylene glycol gel photonic crystal, can change and produce body temperature, concentration of alcohol and pH, there is color change in long-pending response simultaneously.
Embodiment 2
The invention discloses a kind of fast preparation method of gel photonic crystal, this fast preparation method comprise asLower step:
(1) 60 grams of methyl methacrylates are dispersed in 150 grams of water, being mixed with mass fraction is 28.5%Emulsion, emulsion is warming up to 90 DEG C, then add 1 gram of ammonium persulfate, through 1 hour reaction obtainPolymethyl methacrylate nano particle suspension liquid;
(2) 20 grams of polyvinyl alcohol and 10 grams of polyethylene glycol are added to polymethyl methacrylate nano particleIn suspension, temperature is controlled at 90 DEG C, refluxes 1 hour, obtains polyvinyl alcohol/polyethylene glycol pregel;
(3) mixed-bed resin that is 1:5 by cation and anion ratio adds polyvinyl alcohol/polyethylene glycol pre-In gel, and cool to 50 DEG C, purifying 6 hours, obtains photonic crystal pregel;
(4) photonic crystal pregel is injected in mould with micro syringe, mould sealing is placed onIn the environment of-18 DEG C freezing 24 hours, then in the environment of 20 DEG C, thaw 1 hour, get final product the demoulding,Obtain polyvinyl alcohol/polyethylene glycol gel photonic crystal, can diffracts visible light, can be to concentration of alcohol, pH andVariations in temperature produces volume response, and color change occurs simultaneously.
Embodiment 3
The invention discloses a kind of fast preparation method of gel photonic crystal, this fast preparation method comprise asLower step:
(1) 50 grams of styrene are dispersed in 150 grams of water, are mixed with mass fraction and are 25% emulsion,Emulsion is warming up to 90 DEG C, then adds 1 gram of ammonium persulfate, obtain polystyrene through reaction in 1 hour and receiveRice grain suspension;
(2) 40 grams of polyurethane are added in polystyrene nanoparticles suspension, temperature is controlled at 90 DEG C,Reflux 1 hour, obtain polyurethane pregel;
(3) mixed-bed resin that is 1:3 by cation and anion ratio adds in polyurethane pregel, andCool to 50 DEG C, purifying 6 hours, obtains photonic crystal pregel;
(4) photonic crystal pregel is injected in mould with micro syringe, mould sealing is placed onIn 60 DEG C of baking ovens, solidify 2 hours, get final product the demoulding, obtain polyurethane gle photonic crystal, energy diffracts visible light,Can produce volume response to concentration of alcohol, variations in temperature, color change occurs simultaneously.
Embodiment 4
The invention discloses a kind of fast preparation method of gel photonic crystal, this fast preparation method comprise asLower step:
(1) 50 grams of styrene are dispersed in 150 grams of water, are mixed with mass fraction and are 25% emulsion,Emulsion is warming up to 90 DEG C, then adds 1 gram of potassium peroxydisulfate, obtain polystyrene through reaction in 1 hour and receiveRice grain suspension;
(2) 35 grams of polyvinyl alcohol are added in polystyrene nanoparticles suspension, temperature is controlled at 90 DEG C,Reflux 1 hour, obtain polyvinyl alcohol pregel;
(3) mixed-bed resin that is 1:2 by cation and anion ratio adds in polyvinyl alcohol pregel,And cooling to 50 DEG C, purifying 6 hours, obtains photonic crystal pregel;
(4) photonic crystal pregel is injected in mould with micro syringe, mould sealing is placed onIn the environment of-18 DEG C freezing 24 hours, then in the environment of 20 DEG C, thaw 1 hour, get final product the demoulding,Obtain polyvinyl alcohol gel photonic crystal, energy diffracts visible light, can change and produce volume response concentration of alcohol,There is color change simultaneously.
Embodiment 5
The invention discloses a kind of fast preparation method of gel photonic crystal, this fast preparation method comprise asLower step:
(1) 50 grams of styrene are dispersed in 150 grams of water, are mixed with mass fraction and are 25% emulsion,Emulsion is warming up to 90 DEG C, then adds 1 gram of potassium peroxydisulfate, obtain polystyrene through reaction in 1 hour and receiveRice grain suspension;
(2) 40 grams of polyurethane are added in polystyrene nanoparticles suspension, temperature is controlled at 90 DEG C,Reflux 1 hour, obtain polyurethane pregel;
(3) mixed-bed resin that is 1:2 by cation and anion ratio adds in polyurethane pregel, andCool to 50 DEG C, purifying 6 hours, obtains photonic crystal pregel;
(4) photonic crystal pregel is injected in mould with micro syringe, mould sealing is placed onIn the environment of-18 DEG C freezing 24 hours, then in the environment of 20 DEG C, thaw 1 hour, get final product the demoulding,Obtain polyurethane gle photonic crystal, energy diffracts visible light, can produce concentration of alcohol, extraneous STRESS VARIATION, there is color change in volume response simultaneously.
More than show and described general principle of the present invention and principal character and advantage of the present invention. The industryTechnical staff should understand, the present invention is not restricted to the described embodiments, in above-described embodiment and descriptionThat describes just illustrates principle of the present invention, without departing from the spirit and scope of the present invention, and the present inventionAlso have various changes and modifications, these changes and improvements all fall in the claimed scope of the invention. ThisInventing claimed scope is defined by appending claims and equivalent thereof.
Claims (6)
1. a fast preparation method for gel photonic crystal, is characterized in that, described fast preparation methodComprise the steps:
(1) monomer is dispersed in water, is mixed with the emulsion that mass fraction is 15-30%, by emulsionBe warming up to 90 DEG C, then adding mass fraction is the initator of 0.5-2%, obtains through reaction in 0.5-2 hourNano granule suspension;
(2) macromolecular material is added in nano granule suspension, temperature is controlled at 90 DEG C, backflow 1-2Hour, obtain macromolecule pregel;
(3) ion exchange resin is added in macromolecule pregel, and cool to 50 DEG C, purifying 2-10 is littleTime, obtain photonic crystal pregel;
(4) photonic crystal pregel is joined in syringe, then be injected in mould, mould is sealedFreezing 2-24 hour in the environment of be placed on-20-0 DEG C, 0.5-1 then thaws in the environment of 20-25 DEG CHour, or be placed in 60 DEG C of baking ovens curing 2 hours, and get final product the demoulding, obtain gel photonic crystal.
2. according to the fast preparation method of a kind of gel photonic crystal described in claim 1, its featureBe, described monomer is alkene type organic, and it is styrene, methacrylate, acrylic acid and propyleneOne or more in acid amides.
3. according to the fast preparation method of a kind of gel photonic crystal described in claim 1, its featureBe, described initator is ammonium persulfate or potassium peroxydisulfate.
4. according to the fast preparation method of a kind of gel photonic crystal described in claim 1, its featureBe, described initator is azodiisobutyronitrile or ABVN.
5. according to the fast preparation method of a kind of gel photonic crystal described in claim 1, its featureBe, described macromolecular material be polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, polyurethane andOne or more in PLA.
6. according to the fast preparation method of a kind of gel photonic crystal described in claim 1, its featureBe, described ion exchange resin is mixed-bed resin, and cation and anion ratio are 1:2-1:5.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107043445A (en) * | 2017-05-09 | 2017-08-15 | 长春理工大学 | A kind of rigid brush block copolymer and synthetic method |
| CN107085249A (en) * | 2017-07-04 | 2017-08-22 | 上海第二工业大学 | A kind of preparation method of two-dimensional invisible photonic crystal |
| CN108133659A (en) * | 2017-12-25 | 2018-06-08 | 苏州善恩纳米功能材料科技有限公司 | A kind of cold chain storage and transportation monitoring label based on nanometer temperature sensing color changing material |
| CN111635596A (en) * | 2020-07-09 | 2020-09-08 | 上海第二工业大学 | Preparation method and application of gel photonic crystal with self-repairing performance |
| CN111816054A (en) * | 2020-07-21 | 2020-10-23 | 苏州善恩纳米功能材料科技有限公司 | Solid-state temperature-sensitive color-changing label |
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| US20070063208A1 (en) * | 2005-03-24 | 2007-03-22 | Klimov Victor I | Nanocrystal/photonic crystal composites |
| CN101899712A (en) * | 2010-07-27 | 2010-12-01 | 华东理工大学 | Thermoreversible physical gel photonic crystal material and preparation method thereof |
| JP2011123238A (en) * | 2009-12-10 | 2011-06-23 | Konica Minolta Holdings Inc | Display element |
| CN102193213A (en) * | 2011-05-19 | 2011-09-21 | 东南大学 | Brightly colorful contact lens and preparation method thereof |
-
2015
- 2015-12-28 CN CN201511003088.3A patent/CN105601951B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070063208A1 (en) * | 2005-03-24 | 2007-03-22 | Klimov Victor I | Nanocrystal/photonic crystal composites |
| JP2011123238A (en) * | 2009-12-10 | 2011-06-23 | Konica Minolta Holdings Inc | Display element |
| CN101899712A (en) * | 2010-07-27 | 2010-12-01 | 华东理工大学 | Thermoreversible physical gel photonic crystal material and preparation method thereof |
| CN102193213A (en) * | 2011-05-19 | 2011-09-21 | 东南大学 | Brightly colorful contact lens and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107043445A (en) * | 2017-05-09 | 2017-08-15 | 长春理工大学 | A kind of rigid brush block copolymer and synthetic method |
| CN107085249A (en) * | 2017-07-04 | 2017-08-22 | 上海第二工业大学 | A kind of preparation method of two-dimensional invisible photonic crystal |
| CN108133659A (en) * | 2017-12-25 | 2018-06-08 | 苏州善恩纳米功能材料科技有限公司 | A kind of cold chain storage and transportation monitoring label based on nanometer temperature sensing color changing material |
| CN111635596A (en) * | 2020-07-09 | 2020-09-08 | 上海第二工业大学 | Preparation method and application of gel photonic crystal with self-repairing performance |
| CN111816054A (en) * | 2020-07-21 | 2020-10-23 | 苏州善恩纳米功能材料科技有限公司 | Solid-state temperature-sensitive color-changing label |
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