CN108794686A - A kind of preparation method with reversible electrochromism transparent aquagel - Google Patents
A kind of preparation method with reversible electrochromism transparent aquagel Download PDFInfo
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- CN108794686A CN108794686A CN201810722459.0A CN201810722459A CN108794686A CN 108794686 A CN108794686 A CN 108794686A CN 201810722459 A CN201810722459 A CN 201810722459A CN 108794686 A CN108794686 A CN 108794686A
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- hydrogel
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- electrochromism
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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
- C08F220/56—Acrylamide; Methacrylamide
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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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/14—Macromolecular compounds
Abstract
The present invention provides a kind of preparation methods with reversible electrochromism transparent aquagel.The hydrogel is using deionized water as solvent, acrylamide is main monomer, hexadecyl metrhacrylate is hydrophobic monomer, lauryl sodium sulfate is surfactant, lithium chloride is electrolyte, potassium tartrate is organic salt, and the hydrogel with reversible electrochromism transparent nature has been made by Raolical polymerizable.This hydrogel becomes transparent under conductive condition from opaque, and light transmittance reaches 90% or more.This hydrogel can restore original opaque state, be further continued for being powered, hydrogel can become transparent again at room temperature after stopping being powered.Therefore a kind of hydrogel that reversible electrochromism is transparent has successfully been made in the present invention.
Description
Technical field
The invention belongs to macromolecule hydrogel technical fields, and in particular to one kind having reversible electrochromism transparent aquagel
Preparation method.
Background technology
Hydrogel is the high molecular material with 3 D stereo network structure using water as decentralized medium.Hydrogel is by parent
Aqueous monomers and hydrophobic monomer are cross-linked to form network structure jointly, and interaction between the two allows hydrogel by water
Molecular Control in the network architecture, while hydrophobic grouping can hydrone effect under arrange, ultimately form polymer.Because of water-setting
Include a large amount of water in glue, so property is soft, there is certain deformability and load capacity.
Metachromatism is prevalent in nature, and such as chameleon, its body colour can change with the variation of ambient enviroment
Become.Interested people are a kind of materials with reversible color property, you can utilize certain external condition by their face
Color is changed and is restored under the conditions of another kind.Presently found metachromatism mainly has 4 classes:Electrochromism, light
Mutagens color, thermochromism and piezallochromy, wherein studying the most deep with electrochromism again.Electrochromism refers to material in electricity
The phenomenon that stablizing reversible change is generated under field action, and the reversible change of color and transparency is then shown as on appearance property.Tool
There is the material of electrochromic property to be known as electrochromic material.This material is divided into organic and inorganic two major classes, and inorganic electroluminescence becomes
The Typical Representative of color material is tungstic acid, currently, with WO3For the electrochromic device industrialization of functional material.And have
Machine electrochromic material mainly has polythiophene class and its derivative, purple sieve essence class, tetrathiafulvalene, metallo phthalocyanine
Deng.Wherein, practical application has been obtained as the electrochromic material of functional material using purple sieve essence class（Xu Na, Shen Xiaodong, Cui
Rise the progress and development prospect [J] rare metals of electrochromic materials, 2010,34 (4):000610-617.）.
Kazuhide Ueno et al. are controlled by changing the periodicity and average dielectric constant of photonic crystal in gel rubber material in PBG
Energy level, realize different colours and show, and by control conducting direction, achieved the purpose that two kinds of color phase co-conversions
（Ueno K, Matsubara K, Watanabe M, et al. An Electro‐ and Thermochromic
Hydrogel as a Full‐Color Indicator[J]. Advanced Materials, 2010, 19(19):2807-
2812.）.Since the property of this kind of material has extremely special meaning in luminosity adjusting, in electrochromism smart windows, electroluminescent
It is color changing display, very extensive without application prospect in terms of dizzy speculum and memory device, in fields such as automobile, Aeronautics and Astronautics
In be concerned, and due to the fast development of artificial intelligence bionic material, the advantage of electrochromic material is also increasingly
It is prominent.
Currently, electrochromic material is fast-developing, but still it is not achieved preferably in the performance of electrochromic material
Degree, and the cost of such material is also relatively high, greatly limit electrochromic material application range and study into
Exhibition, it is most important that report of the electrochromism property in the field of hydrogel is seldom and manufacturing process is mostly relatively complicated,
It is very restricted in each application field, so we draw electrochromic property by the method for free radical polymerization
Enter in hydrogel, to obtain the hydrogel with reversible electrochromism transparent characteristic, open hydrogel is in electrochemistry work
The application prospect of industry related field, while providing new thinking for the development of electrochromic material.
Invention content
The present invention provides a kind of preparation methods with reversible electrochromism transparent aquagel.
The inventive point of the present invention is：Organic salt is introduced in hydrogel, achievees the purpose that reversible electrochromism is transparent.
A kind of preparation method with reversible electrochromism transparent aquagel provided by the invention, its step are as follows：
（1）Prepare mixed solution
By deionized water, main monomer, hydrophobic monomer, surfactant, electrolyte, organic salt, Oxidizing and Reducing Agents each group
Divide in mass ratio 100：(19.35-25.8): (0.13-0.22):(0.68-1.37):(3.22-6.45):(1.61-3.87):
(0.13-0.26):(0.11-0.20) it is uniformly mixed, obtains uniform mixed solution；The main monomer is acrylamide, is dredged
Aqueous monomers are hexadecyl metrhacrylate, and surfactant is lauryl sodium sulfate, and electrolyte is lithium chloride, and organic salt is
Potassium tartrate, oxidant are potassium peroxydisulfate, and reducing agent is tetramethylethylenediamine.
（2）Uniform mixed solution obtained above is put into preparing in water-setting sealing rubber die and being placed on mold for sealing
In baking oven, 35 DEG C of constant temperature reacts 3-4 hours, and reaction terminates, reaction postcooling to room temperature, you can obtains hydrogel sample.
Advantageous effect：Organic salt is introduced into hydrogel by the present invention, makes water using the electrical heating process when being powered
Gel internal structure changes, and hydrogel is changed into pellucidity by opaque state, and this hydrogel is after stopping being powered,
It can restore original opaque state at room temperature, be once again powered up, hydrogel can become transparent again.Thus successfully by reversible electricity
The property and hydrogel for causing color changeable transparent combine, and have widened application field of the hydrogel in off-color material.
Specific implementation mode
Embodiment 1
（1）Prepare mixed solution
By deionized water, main monomer, hydrophobic monomer, surfactant, electrolyte, organic salt, Oxidizing and Reducing Agents each group
Divide by quality and is：100g, 19.35g, 0.13g, 0.68g, 3.22g, 1.61g, 0.13g and 0.11g are uniformly mixed, and are obtained uniform
Mixed solution；The main monomer is acrylamide, and hydrophobic monomer is hexadecyl metrhacrylate, surfactant ten
Sodium dialkyl sulfate, electrolyte are lithium chloride, and organic salt is potassium tartrate, and oxidant is potassium peroxydisulfate, and reducing agent is tetramethyl
Ethylenediamine.
（2）Uniform mixed solution obtained above is put into preparing in water-setting sealing rubber die and being placed on mold for sealing
In baking oven, 35 DEG C of constant temperature reacts 3-4 hours, and reaction terminates, reaction postcooling to room temperature, you can obtains hydrogel sample.
Preparation length is 50mm, and width 4mm, thickness is the hydrogel test sample of 2mm, and light is divided by UV, visible light
Degree meter is tested.
Transmitance is 50 before the reversible electrochromism transparent aquagel prepared in example 1 is not powered on, and transmitance is after energization
95, transmitance is 50 after a hour is placed at room temperature for after energization, and it is 95 to be once again powered up transmitance, and one is placed at room temperature for after being once again powered up
Transmitance is 50 after hour.
Embodiment 2
（1）Prepare mixed solution
By deionized water, main monomer, hydrophobic monomer, surfactant, electrolyte, organic salt, Oxidizing and Reducing Agents each group
Divide by quality and is：100g, 21.62g, 0.13g, 0.92g, 4.54g, 2.62g, 0.18g and 0.16g are uniformly mixed, and are obtained uniform
Mixed solution；The main monomer is acrylamide, and hydrophobic monomer is hexadecyl metrhacrylate, surfactant ten
Sodium dialkyl sulfate, electrolyte are lithium chloride, and organic salt is potassium tartrate, and oxidant is potassium peroxydisulfate, and reducing agent is tetramethyl
Ethylenediamine.
（2）Uniform mixed solution obtained above is put into preparing in water-setting sealing rubber die and being placed on mold for sealing
In baking oven, 35 DEG C of constant temperature reacts 3-4 hours, and reaction terminates, reaction postcooling to room temperature, you can obtains hydrogel sample.
With the assay method in embodiment 1, the reversible electrochromism transparent aquagel prepared in example 2 is not powered on preceding light transmission
Rate is 48, and light transmittance is 94 after energization.It is 48 that a hour transmitance is stood after energization, and it is 94 to be once again powered up transmitance.Again
Transmitance is 94 after being placed at room temperature for one hour after energization.
Embodiment 3
（1）Prepare mixed solution
By deionized water, main monomer, hydrophobic monomer, surfactant, electrolyte, organic salt, Oxidizing and Reducing Agents each group
Divide by quality and is：100g, 23.50g, 0.21g, 1.25g, 4.95g, 3.00g, 0.24g and 0.18g are uniformly mixed, and are obtained uniform
Mixed solution；The main monomer is acrylamide, and hydrophobic monomer is hexadecyl metrhacrylate, surfactant ten
Sodium dialkyl sulfate, electrolyte are lithium chloride, and organic salt is potassium tartrate, and oxidant is potassium peroxydisulfate, and reducing agent is tetramethyl
Ethylenediamine.
（2）Uniform mixed solution obtained above is put into preparing in water-setting sealing rubber die and being placed on mold for sealing
In baking oven, 35 DEG C of constant temperature reacts 3-4 hours, and reaction terminates, reaction postcooling to room temperature, you can obtains hydrogel sample.
With the assay method in embodiment 1, the reversible electrochromism transparent aquagel prepared in example 3 is not powered on preceding transmission
Rate is 34, and transmitance is 93 after energization.It is 34 that a hour transmitance is stood after energization, and it is 93 to be once again powered up transmitance.Again
Transmitance is 34 after being placed at room temperature for one hour after energization.
Embodiment 4
（1）Prepare mixed solution
By deionized water, main monomer, hydrophobic monomer, surfactant, electrolyte, organic salt, Oxidizing and Reducing Agents each group
Divide by quality and is：100g, 24.32g, 0.15g, 1.32g, 5.85g, 3.20g, 0.24g and 0.18g are uniformly mixed, and are obtained uniform
Mixed solution；The main monomer is acrylamide, and hydrophobic monomer is hexadecyl metrhacrylate, surfactant ten
Sodium dialkyl sulfate, electrolyte are lithium chloride, and organic salt is potassium tartrate, and oxidant is potassium peroxydisulfate, and reducing agent is tetramethyl
Ethylenediamine.
（2）Uniform mixed solution obtained above is put into preparing in water-setting sealing rubber die and being placed on mold for sealing
In baking oven, 35 DEG C of constant temperature reacts 3-4 hours, and reaction terminates, reaction postcooling to room temperature, you can obtains hydrogel sample.
With the assay method in embodiment 1, the reversible electrochromism transparent aquagel prepared in example 4 is not powered on preceding transmission
Rate is 32, and transmitance is 93 after energization.It is 32 that a hour transmitance is stood after energization, and it is 93 to be once again powered up transmitance.Again
Transmitance is 32 after being placed at room temperature for one hour after energization.
Embodiment 5
（1）Prepare mixed solution
By deionized water, main monomer, hydrophobic monomer, surfactant, electrolyte, organic salt, Oxidizing and Reducing Agents each group
Divide by quality and is：100g, 25.80g, 0.22g, 1.37g, 6.45g, 3.87g, 0.26g and 0.20g are uniformly mixed, and are obtained uniform
Mixed solution；The main monomer is acrylamide, and hydrophobic monomer is hexadecyl metrhacrylate, surfactant ten
Sodium dialkyl sulfate, electrolyte are lithium chloride, and organic salt is potassium tartrate, and oxidant is potassium peroxydisulfate, and reducing agent is tetramethyl
Ethylenediamine.
（2）Uniform mixed solution obtained above is put into preparing in water-setting sealing rubber die and being placed on mold for sealing
In baking oven, 35 DEG C of constant temperature reacts 3-4 hours, and reaction terminates, reaction postcooling to room temperature, you can obtains hydrogel sample.
With the assay method in embodiment 1, the reversible electrochromism transparent aquagel prepared in example 5 is not powered on preceding transmission
Rate is 16, and transmitance is 92 after energization.It is 16 that a hour transmitance is stood after energization, and it is 92 to be once again powered up transmitance.Again
Transmitance is 16 after being placed at room temperature for one hour after energization.
Embodiment 6
（1）Prepare mixed solution
By deionized water, main monomer, hydrophobic monomer, surfactant, electrolyte, organic salt, Oxidizing and Reducing Agents each group
Divide by quality and is：100g, 25.80g, 0.22g, 0.68g, 6.45g, 3.25g, 0.13g and 0.11g are uniformly mixed, and are obtained uniform
Mixed solution；The main monomer is acrylamide, and hydrophobic monomer is hexadecyl metrhacrylate, surfactant ten
Sodium dialkyl sulfate, electrolyte are lithium chloride, and organic salt is potassium tartrate, and oxidant is potassium peroxydisulfate, and reducing agent is tetramethyl
Ethylenediamine.
（2）Uniform mixed solution obtained above is put into preparing in water-setting sealing rubber die and being placed on mold for sealing
In baking oven, 35 DEG C of constant temperature reacts 3-4 hours, and reaction terminates, reaction postcooling to room temperature, you can obtains hydrogel sample.
With the assay method in embodiment 1, the reversible electrochromism transparent aquagel prepared in example 6 is not powered on preceding transmission
Rate is 16, and transmitance is 92 after energization.It is 16 that a hour transmitance is stood after energization, and it is 92 to be once again powered up transmitance.Again
Transmitance is 16 after being placed at room temperature for one hour after energization.
Claims (2)
1. a kind of preparation method with reversible electrochromism transparent aquagel provided by the invention, step and condition are as follows：
（1）Prepare mixed solution
By deionized water, main monomer, hydrophobic monomer, surfactant, electrolyte, organic salt, Oxidizing and Reducing Agents each group
Divide in mass ratio 100：(19.35-25.8): (0.13-0.22):(0.68-1.37):(3.22-6.45):(1.61-3.87):
(0.13-0.26):(0.11-0.20) it is uniformly mixed, obtains uniform mixed solution；The main monomer is acrylamide, is dredged
Aqueous monomers are hexadecyl metrhacrylate, and surfactant is lauryl sodium sulfate, and electrolyte is lithium chloride, and organic salt is
Potassium tartrate, oxidant are potassium peroxydisulfate, and reducing agent is tetramethylethylenediamine;
（2）Uniform mixed solution obtained above is put into preparing in water-setting sealing rubber die and mold being placed on baking oven for sealing
In, 35 DEG C of constant temperature reacts 3-4 hours, and reaction terminates, reaction postcooling to room temperature, you can obtains hydrogel sample.
2. reversible electrochromism transparent aquagel described in, main monomer acrylamide and hydrophobic monomer hexadecyl metrhacrylate are total
Gather, the formation hydrophobic association crosslinking points formation hydrogel under emulsifier effect of the hydrophobic monomer in copolymer, it is organic in hydrogel
Electrochromism clearing process is realized in the variation of salt potassium tartrate state of aggregation in energization power process.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112107089A (en) * | 2020-09-16 | 2020-12-22 | 浙江理工大学 | Preparation method of healthy bracelet capable of displaying safe sun exposure time based on ionic liquid hydrogel |
| CN112300309A (en) * | 2020-10-30 | 2021-02-02 | 江南大学 | Preparation method of stretchable flexible electrochromic film |
| CN113568235A (en) * | 2021-06-28 | 2021-10-29 | 浙江工业大学 | Electrochromic device based on multifunctional hydrogel electrolyte and preparation method thereof |
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| WO2006056550A1 (en) * | 2004-11-24 | 2006-06-01 | Siemens Aktiengesellschaft | Electrochromic component comprising an electrolyte-filled hydrogel |
| CN1934212A (en) * | 2004-04-19 | 2007-03-21 | Lg化学株式会社 | Gel polymer electrolyte containing ionic liquid and electrochromic device using the same |
| CN105085791A (en) * | 2015-09-13 | 2015-11-25 | 长春工业大学 | Preparation method of hydrophobic microsphere toughened and reinforced physical crosslinking double-network hydrogel |
| CN106496394A (en) * | 2016-11-01 | 2017-03-15 | 长春工业大学 | A kind of cation emulsion particle toughening hydrophobic association hydrogel and preparation method |
-
2018
- 2018-07-04 CN CN201810722459.0A patent/CN108794686A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1934212A (en) * | 2004-04-19 | 2007-03-21 | Lg化学株式会社 | Gel polymer electrolyte containing ionic liquid and electrochromic device using the same |
| WO2006056550A1 (en) * | 2004-11-24 | 2006-06-01 | Siemens Aktiengesellschaft | Electrochromic component comprising an electrolyte-filled hydrogel |
| CN105085791A (en) * | 2015-09-13 | 2015-11-25 | 长春工业大学 | Preparation method of hydrophobic microsphere toughened and reinforced physical crosslinking double-network hydrogel |
| CN106496394A (en) * | 2016-11-01 | 2017-03-15 | 长春工业大学 | A kind of cation emulsion particle toughening hydrophobic association hydrogel and preparation method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112107089A (en) * | 2020-09-16 | 2020-12-22 | 浙江理工大学 | Preparation method of healthy bracelet capable of displaying safe sun exposure time based on ionic liquid hydrogel |
| CN112107089B (en) * | 2020-09-16 | 2023-01-03 | 浙江理工大学 | Preparation method of healthy bracelet capable of displaying safe sun exposure time based on ionic liquid hydrogel |
| CN112300309A (en) * | 2020-10-30 | 2021-02-02 | 江南大学 | Preparation method of stretchable flexible electrochromic film |
| CN113568235A (en) * | 2021-06-28 | 2021-10-29 | 浙江工业大学 | Electrochromic device based on multifunctional hydrogel electrolyte and preparation method thereof |
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Application publication date: 20181113 |