CN109535691A - A kind of thermochromic thin film and preparation method thereof - Google Patents
A kind of thermochromic thin film and preparation method thereof Download PDFInfo
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/30—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with substituted triazines
- C08G12/32—Melamines
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—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
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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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
- 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
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
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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
- C08K5/05—Alcohols; Metal alcoholates
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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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
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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Abstract
The present invention provides a kind of thermochromic thin films and preparation method thereof, wherein using polyvinyl alcohol as basis material, to improve its toughness, it is blended with aqueous polyurethane, adjust the ratio of the two, it is added temperature sensing color changing Nano capsule as functional additive in film forming matrix, thermochromic thin film is prepared by casting filming therapy.The preparation method simple process consumes energy low, through film obtained by the preparation method while having high-intensitive and toughness, can keep good heat-storage thermoregulation function, also has good thermochromism and temperature indicator, use is safe, widely used.
Description
Technical field
The present invention relates to membrane preparation technology, specially it is a kind of include temperature sensing color changing Nano capsule thermochromic thin film and
Preparation method.
Background technique
Whether military project or in daily life, the important role of thermochromic material all performers.In military field
In, one of discoloration art in modern battlefield is exactly to make the color of protected target surface with back using reversible color material
The color of scape is different and changes colour, blendes together one with locating background, to achieve the purpose that vision is stealthy.In daily life, hot
Cause off-color material to can be used as the pad pasting of building glass, this film without the driving of any energy, can be used for indoor glass, every
Disconnected, wall, lampshade, mural painting, artificial flower etc., make it change colour with indoor temperature change generated in case, are also used as indicating cold and hot intelligent
Material.Energy-saving and temperature-regulating film be phase-changing energy storage material is compound with film forming matrix, obtain the smart membrane that can automatically adjust temperature.Temperature adjustment
Film is remained unchanged using release in substance phase transition process or absorption latent heat, temperature, has two-way automatic temperature-adjusting function, to cope with ring
The variation of border temperature, to achieve the purpose that film to the balance and adjusting of local microenvironment temperature.Therefore, temperature adjustment film is as a kind of
New material has a wide range of applications in fields such as clothes fabric, building, medical textiles.
Polyvinyl alcohol is due to its good biocompatibility, biological degradability, water solubility and lower bio-toxicity,
It is used in many fields such as: filtering material, film, coating, protective clothes, weaving, drug release.Aqueous polyurethane has
Excellent biocompatibility, hypotoxicity, good mechanical property, intensity, flexibility and damping and amortization, in coating, adhesive, fabric
The fields such as coating, automobile, building and biomedicine are widely used.
Capsule, which refers to, is overmolding to solid, liquid or gas with the miniature of particular geometric configuration by using filmogen
Container, this miniature vessel are widely used in the energy, drug delivery, food, doctor for protecting or controlling release capsule-core substance
The fields such as medicine, health, coating, adhesive.By leuco dye, color developing agent and discoloration temperature control solvent group at Reversible thermochromic
Microcapsules can effectively improve the stability and repeatability of such reversible temperature sensitive variable color system.
At present intensity and excellent tenacity and have thermochromism and the film of heat-storage thermoregulation and preparation method thereof seldom reported
Road.
Summary of the invention
The present invention provides a kind of thermochromic thin films and preparation method thereof, wherein using polyvinyl alcohol as basis material,
To improve its toughness, it is blended with aqueous polyurethane, adjusts the ratio of the two, add using temperature sensing color changing Nano capsule as function
Add agent to be added in film forming matrix, thermochromic thin film is prepared by casting filming therapy.The preparation method simple process, energy consumption
Low, the high mechanical strength of film obtained by the preparation method, toughness is strong, has high intensity through film obtained by the preparation method
While with toughness, good heat-storage thermoregulation function can be kept, also there is good thermochromism and temperature indicator, use peace
Entirely, widely used.
Wherein specific step is as follows for the preparation method of the thermochromic thin film:
(1) it the preparation of temperature sensing color changing Nano capsule: by mass, takes in 10~30 parts of organic phase change material solvents and is added
2~10min is stirred in 0.1~1 part of color developing agent and procrypsis agent at 120~200 DEG C, forms phase-change material solution capsule-core；By 5~
15 parts of cyst materials are dissolved in 50~90 DEG C of dispersing agents, are stirred evenly；5~20 parts of emulsifiers are dissolved in 40~50 DEG C of steaming
In distilled water, stir evenly；The pH value that above-mentioned three kinds of solution is mixed evenly, and adjusts mixed solution is 1.5~6.5, with
Carrying out shear rate to it afterwards is 450~10000rpm/min emulsification pretreatment, 5~30min.By the mixed solution after emulsification pretreatment
It is moved into three-necked flask, is warming up to 60~70 DEG C, then 5 are added dropwise into solution with 0.1 part/min~2 part/min speed~
15 parts of cyst materials, gradually heat up at 60~85 DEG C, keep the temperature 2~5h, and adjusting solution pH value is that 6.5~9 reaction was completed, by product
Solution is filtered, washed, is dried, temperature sensing color changing Nano capsule can be obtained.
(2) preparation of poly-vinyl alcohol solution: polyvinyl alcohol is dissolved in deionized water, and 60~90 DEG C of oil bath heatings are simultaneously mechanical
Certain density poly-vinyl alcohol solution is made in stirring, vacuum defoamation.
(3) by mass, polyvinyl alcohol and aqueous polyurethane are uniformly mixed into film forming matrix, by step (1) preparation
Temperature sensing color changing Nano capsule is added to according to a certain percentage in the film forming matrix, through ultrasonic disperse, after vacuum defoamation, by molten
Liquid the tape casting blade coating film forming.
The organic phase change material solvent is fatty acid, fatty alcohol, fatty ester, cod-liver oil etc. or above-mentioned organic compound
Two or more mixture, but not limited to this substance that place is listed.
The cyst material is the Lauxite in amino resins, phenolic resin, melamine resin and its alkyl
Etherified resin includes methyl etherified melamine formaldehyde resin, butyl be etherified melamine resin etc. and polyurethane and its
Performed polymer, polymethyl methacrylate, chitosan, sodium alginate, cellulose acetate, gelatin, in group composed by Arabic gum
At least one.
The emulsifier is polyvinyl alcohol, polyvinylpyrrolidone, sorbitol anhydride oleate, polyoxyethylene nonylphenol ether 10, fat
Alcohol polyethenoxy ether sodium sulfate, styrene maleic anhydride copolymer, fatty alcohol polyoxyethylene ether, turkey red oil, benzene sulfonamide
It is any or any in sour sodium, alginate propylene glycol, polyoxyethylene sorbitan monooleate, sodium alkyl sulfate or pull open powder
Several mixtures with any ratio.
The particle size range of the capsule is in 100nm~5 μm.
The polyvinyl alcohol is any in polyvinyl alcohol 1788,1792,1799,2499 or any several with any ratio
Mixture.
The polyvinyl alcohol concentration is 10%~35%.
The solid content of the aqueous polyurethane is 15%~40%.
Step (3) the temperature sensing color changing Nano capsule accounts for 3wt%~40wt% that film forming matrix is measured in a word.
The ratio of the polyvinyl alcohol and aqueous polyurethane is 2: 8~8: 2.
Detailed description of the invention
Fig. 1 and Fig. 2 is the surface of thermochromic thin film prepared by embodiment 1 and the scanning electron microscope of section respectively
Photo.
Specific embodiment
The method that the present invention describes is further illustrated below by way of specific embodiment, it is not intended that the present invention limits to
In these embodiments.
Embodiment 1:
A kind of preparation method of thermochromic thin film, includes the following steps:
(1) it takes and 0.3 part of crystal violet lactone and 0.9 part of bisphenol-A is added in 20 parts of tetradecyl alchohols, stir 10min at 120 DEG C,
Form phase-change material solution capsule-core；10 parts of melamines and paraformaldehyde are dissolved in 75 DEG C of deionized waters, are stirred evenly；It will
5 parts of styrene-maleic anhydride copolymer solution (SMA) are dissolved in 50 DEG C of distilled water, stir evenly；By above-mentioned three kinds of solution
The pH value for being mixed evenly, and adjusting mixed solution is 4.5, carries out shear rate to it then as 5000rpm/min shearing
Emulsify 30min.Mixed solution after emulsification pretreatment is moved into three-necked flask, is warming up to 60 DEG C, then with 0.3 part/min's
10 parts of cyst materials are added dropwise into solution for speed, are warming up to 75 DEG C, keep the temperature 1h, then raise temperature to 85 DEG C, keep the temperature 1h, adjust solution
PH value is that 7 reaction was completed, and product is filtered, wash, is dried, temperature sensing color changing Nano capsule can be obtained.
(2) preparation of poly-vinyl alcohol solution: 20 part of 1788 type polyvinyl alcohol is dissolved in 100 parts of deionized waters, 80 DEG C of oil
The poly-vinyl alcohol solution that concentration is 20wt% is made in bath heating and mechanical stirring, vacuum defoamation.
(3) by mass, by concentration be 20wt% polyvinyl alcohol and solid content be 35wt% aqueous polyurethane by 6: 4
Ratio uniform be mixed into film forming matrix, by the step of 20wt% (1) prepare temperature sensing color changing Nano capsule be added to it is described at
In membrane matrix, through ultrasonic disperse, after vacuum defoamation, is scratched and formed a film by solution casting method.
Thermochromic thin film surface made from the present embodiment and cross-section morphology figure are as shown in figures 1 and 2.
Embodiment 2:
A kind of preparation method of thermochromic thin film, includes the following steps:
(1) it takes and 0.1 part of crystal violet lactone and 1 part of bisphenol-A is added in 10 parts of hexadecanols, 2min is stirred at 200 DEG C, formed
Phase-change material solution capsule-core；5 parts of melamines and paraformaldehyde are dissolved in 50 DEG C of deionized waters, are stirred evenly；By 10 parts
Styrene-maleic anhydride copolymer solution (SMA) is dissolved in 40 DEG C of distilled water, is stirred evenly；Above-mentioned three kinds of solution is mixed
Conjunction stirs evenly, and the pH value for adjusting mixed solution is 1.5, and it is 450rpm/min emulsification pretreatment that shear rate is then carried out to it
5min.Mixed solution after emulsification pretreatment is moved into three-necked flask, is warming up to 70 DEG C, then with the speed of 0.1 part/min
5 parts of cyst materials are added dropwise into solution, are warming up to 75 DEG C, keep the temperature 2h, then raise temperature to 85 DEG C, keep the temperature 3h, adjust solution pH value
For 6.5, reaction was completed, and product filters solution, washs, dry, temperature sensing color changing Nano capsule can be obtained.
(2) preparation of poly-vinyl alcohol solution: 10 part of 1799 type polyvinyl alcohol is dissolved in 100 parts of deionized waters, 90 DEG C of oil
The poly-vinyl alcohol solution that concentration is 10wt% is made in bath heating and mechanical stirring, vacuum defoamation.
(3) by mass, by concentration be 10wt% polyvinyl alcohol and solid content be 15wt% aqueous polyurethane according to 2: 8
Ratio uniform is mixed into film forming matrix, and the temperature sensing color changing Nano capsule of the 3wt% of step (1) preparation is added to the film forming base
In matter, through ultrasonic disperse, after vacuum defoamation, is scratched and formed a film by solution casting method.
Embodiment 3:
(1) it takes and 1 part of crystal violet lactone and 0.1 part of bisphenol-A is added in 30 parts of n-butyl stearates, stirred at 200 DEG C
2min forms phase-change material solution capsule-core；15 parts of melamines and paraformaldehyde are dissolved in 90 DEG C of deionized waters, stirring is equal
It is even；10 parts of styrene-maleic anhydride copolymer solution (SMA) are dissolved in 50 DEG C of distilled water, are stirred evenly；By above-mentioned three
Kind solution is mixed evenly, and the pH value for adjusting mixed solution is 1.5, and it is 10000rpm/ that shear rate is then carried out to it
Min emulsification pretreatment 30min.Mixed solution after emulsification pretreatment is moved into three-necked flask, is warming up to 70 DEG C, then with 2 parts/
15 parts of cyst materials are added dropwise into solution for the speed of min, are warming up to 75 DEG C, keep the temperature 1h, then raise temperature to 85 DEG C, keep the temperature 1h, adjust
Saving solution pH value is that 9 reaction was completed, and product is filtered, wash, is dried, temperature sensing color changing Nano capsule can be obtained.
(2) preparation of poly-vinyl alcohol solution: 35 part of 1792 type polyvinyl alcohol is dissolved in 100 parts of deionized waters, 60 DEG C of oil
The poly-vinyl alcohol solution that concentration is 35wt% is made in bath heating and mechanical stirring, vacuum defoamation.
(3) by mass, by concentration be 35wt% polyvinyl alcohol and solid content be 40wt% aqueous polyurethane by 8: 2
Ratio uniform is mixed into film forming matrix, and the temperature sensing color changing Nano capsule of the 40wt% of step (1) preparation is described according to being added to
In film forming matrix, through ultrasonic disperse, after vacuum defoamation, is scratched and formed a film by solution casting method.
The thermochromic thin film preparation method simple process, various ways are implementable, product thermochromic properties, heat accumulation tune
Warm nature can be stablized, low in cost, be suitable for industrial applications.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not limited to this hair the foregoing is merely a specific embodiment of the invention
Bright, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection scope within.
Claims (9)
1. a kind of thermochromic thin film containing temperature sensing color changing Nano capsule, it is characterised in that the following steps are included:
(1) it the preparation of temperature sensing color changing Nano capsule: by mass, takes and 0.1~1 is added in 10~30 parts of organic phase change material solvents
2~10min is stirred in part color developing agent and procrypsis agent at 120~200 DEG C, forms phase-change material solution capsule-core；By 5~15 parts of capsules
Wall material is dissolved in 50~90 DEG C of dispersing agents, is stirred evenly；5~20 parts of emulsifiers are dissolved in 40~50 DEG C of distilled water
In, it stirs evenly；The pH value that above-mentioned three kinds of solution is mixed evenly, and adjusts mixed solution is 1.5~6.5, then right
It is 450~10000rpm/min emulsification pretreatment, 5~30min that it, which carries out shear rate,.Mixed solution after emulsification pretreatment is moved into
Into three-necked flask, 60~70 DEG C are warming up to, 5~15 parts are then added dropwise into solution with 0.1 part/min~2 part/min speed
Cyst material gradually heats up at 60~85 DEG C, keeps the temperature 2~5h, and adjusting solution pH value is that 6.5~9 reaction was completed, and product is carried out
It filters, washing, drying, temperature sensing color changing Nano capsule can be obtained.
(2) preparation of poly-vinyl alcohol solution: polyvinyl alcohol is dissolved in deionized water, and simultaneously machinery stirs 60~90 DEG C of oil bath heatings
It mixes, vacuum defoamation, certain density poly-vinyl alcohol solution is made.
(3) by mass, polyvinyl alcohol and aqueous polyurethane are uniformly mixed into film forming matrix, by the temperature sensitive of step (1) preparation
Discoloration Nano capsule is added to according to a certain percentage in the film forming matrix, through ultrasonic disperse, after vacuum defoamation, passes through solution stream
Prolong method blade coating film forming.
2. preparation method as described in claim 1, it is characterised in that: the organic phase change material solvent is fatty acid, fat
Two or more mixture of alcohol, fatty ester, cod-liver oil etc. or above-mentioned organic compound, but not limited to this it lists in place
Substance.
3. preparation method as described in claim 1, it is characterised in that: the cyst material is the ureaformaldehyde tree in amino resins
Rouge, phenolic resin, melamine resin and its alkyl etherified resin include methyl etherified melamine formaldehyde resin, butyl
Etherified melamine amine-formaldehyde resins etc. and polyurethane and its performed polymer, polymethyl methacrylate, chitosan, sodium alginate, vinegar
Acid cellulose, gelatin, at least one of composed group of Arabic gum.
4. preparation method as described in claim 1, it is characterised in that: the emulsifier is polyvinyl alcohol, polyvinylpyrrolidine
Ketone, sorbitol anhydride oleate, polyoxyethylene nonylphenol ether 10, sodium sulfate of polyethenoxy ether of fatty alcohol, styrene maleic anhydride copolymer, rouge
Fat alcohol polyoxyethylene ether, turkey red oil, sodium alkyl benzene sulfonate, alginate propylene glycol, polyoxyethylene sorbitol acid anhydride list oleic acid
Any or any several mixtures with any ratio in ester, sodium alkyl sulfate or pull open powder.
5. preparation method as described in claim 1, it is characterised in that: the polyvinyl alcohol is polyvinyl alcohol 1788,1792,
Any or any several mixtures with any ratio in 1799,2499.
6. preparation method as described in claim 1, it is characterised in that: the polyvinyl alcohol concentration is 10wt%~35wt%.
7. preparation method as described in claim 1, it is characterised in that: the solid content of the aqueous polyurethane be 15wt%~
40wt%.
8. preparation method as described in claim 1, it is characterised in that: step (3) the temperature sensing color changing Nano capsule accounts for film forming
3wt%~40wt% that matrix is measured in a word.
9. preparation method as described in claim 1, it is characterised in that: the ratio of the polyvinyl alcohol and aqueous polyurethane is 2:
8~8: 2.
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Cited By (8)
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|---|---|---|---|---|
| CN110204751A (en) * | 2019-05-23 | 2019-09-06 | 北京工商大学 | A kind of preparation method of phase-change material flexible membrane |
| CN111592822A (en) * | 2020-04-23 | 2020-08-28 | 中新国际联合研究院 | Quick-response thermotropic dimming material and quick-response intelligent dimming film |
| CN112898992A (en) * | 2019-12-04 | 2021-06-04 | 江苏集萃智能液晶科技有限公司 | Temperature-sensitive chromogenic liquid crystal microcapsule and preparation and application methods thereof |
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| CN115450055A (en) * | 2022-05-14 | 2022-12-09 | 苏州烯之韵科技有限公司 | Preparation and application of colorful reversible electrochromism film based on graphene |
| CN115785599A (en) * | 2023-01-09 | 2023-03-14 | 中国科学技术大学 | Preparation method of bionic thermochromic material for hyperspectral camouflage |
| CN116925589A (en) * | 2023-06-06 | 2023-10-24 | 湖州乐通新材料科技有限公司 | Preparation method of thermochromic ink |
| CN118219638A (en) * | 2024-03-12 | 2024-06-21 | 科顺防水科技股份有限公司 | Color-changeable asphalt waterproof coiled material and preparation method thereof |
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| CN110204751A (en) * | 2019-05-23 | 2019-09-06 | 北京工商大学 | A kind of preparation method of phase-change material flexible membrane |
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| CN115450055A (en) * | 2022-05-14 | 2022-12-09 | 苏州烯之韵科技有限公司 | Preparation and application of colorful reversible electrochromism film based on graphene |
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| CN115785599B (en) * | 2023-01-09 | 2023-11-17 | 中国科学技术大学 | Preparation method of bionic thermochromic material for hyperspectral camouflage |
| CN116925589A (en) * | 2023-06-06 | 2023-10-24 | 湖州乐通新材料科技有限公司 | Preparation method of thermochromic ink |
| CN116925589B (en) * | 2023-06-06 | 2024-07-19 | 湖州乐通新材料科技有限公司 | Preparation method of thermochromic ink |
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