CN102816340B - Intelligent light adjusting film based on temperature-sensitive polymer hydrogel and preparation method of intelligent light adjusting film - Google Patents
Intelligent light adjusting film based on temperature-sensitive polymer hydrogel and preparation method of intelligent light adjusting film Download PDFInfo
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- CN102816340B CN102816340B CN201210328556.4A CN201210328556A CN102816340B CN 102816340 B CN102816340 B CN 102816340B CN 201210328556 A CN201210328556 A CN 201210328556A CN 102816340 B CN102816340 B CN 102816340B
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- intelligent light
- temperature
- light adjusting
- adjusting film
- sensitive polymer
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Abstract
The invention discloses an intelligent light adjusting film and particularly discloses an intelligent light adjusting film based on a temperature-sensitive polymer hydrogel and a preparation method of the intelligent light adjusting film. A temperature-sensitive polymer and various auxiliaries are dissolved in a polymer hydrogel body without a temperature-sensitive effect to obtain the intelligent light adjusting film with a certain mechanical strength and good temperature sensitivity. The temperature-sensitive polymer, the various auxiliaries, a water-solubility monomer, a cross-linking agent and the like are prepared into an aqueous solution, an initiator is added into the aqueous solution to polymerize the solution to obtain the intelligent light adjusting film. The preparation method of the intelligent light adjusting film is simple in operation and low in cost and can be operated under room temperatures; and the obtained intelligent light adjusting film has certain strength and is good in temperature sensitivity.
Description
Technical field
The present invention relates to it is a kind of can according to variation of ambient temperature can automatically adjust transmittance intelligent light modulation film and its
Preparation method, can apply to the forms of building or the vehicles, the transparent roofs of greenhouse brooder or some construction venues and
Solar energy heat collector.
Background technology
Effective daylighting of the interior space such as building and the vehicles and solar energy heat collector is that human society is daily
One of key element of life and development green low-carbon economy.In recent years, as countries in the world are paid attention to green energy resource and low-carbon economy
The raising of degree, the effectively utilizes of solar energy and the exploitation of energy-conserving and environment-protective material receive the extensive concern of people.For building
For the vehicles, rational indoor lighting is designed with form layout and can be prevented effectively from unnecessary power consumption(Illumination
And heating);But the side effect for producing is excessively injecting and indoor temperature being caused too high for summer sunlight, needs air-conditioning system
Cold to be lowered the temperature, this undoubtedly increased power consumption again.For solar energy heat collector, sometimes also without too high temperature
Degree.In recent years, researcher develops " smart window(Smart Window)", intelligent light-control material is coated on glass pane,
Or be loaded among glass pane interlayer.Intelligent light-control material can automatically adjust transmittance according to indoor environment, to regulate and control sunlight
Inject.For example, during winter, window keeps pellucidity, and injecting for sunlight can be heating rooms;Summer, when indoor temperature height
When a certain value, window transparency reduces being injected to reduce sunlight, overheated so as to avoid indoor temperature.
The optics regulating switch of intelligent window material can induce liquid crystal aligning arrangement, particle dispersion by electric field action
Or the oxidation-reduction transformation of chromophore, to realize transparent-muddy transformation of smart window;Photochromic material is also employed
In smart window, mainly changed by light transmission caused by ultraviolet radioactive;Another kind of important intelligent window material is thermochromism
Material, transmittance, including inorganic matters such as silver, hydrargyrum, cadmium, titanium, vfanadium compound and polymer are adjusted using the change of ambient temperature
Sill.Due to its low cost and ease for operation, temperature sensing polymer hydrogel shows wide application in smart window field
Prospect.Its principle is that polymer drastically declines with the affinity of water and is separated when temperature is higher than a certain critical temperature,
The macroscopic appearance for showing is transformation of the system from clear state to muddy state, so as to cause the reduction of transmittance.Temperature sensitive type water
Soluble polymer includes hydroxypropyl cellulose(HPC), hydroxypropyl methyl cellulose(HPMC), NIPA
(PNIPA), poly- (methyl vinyl ether)(PVME), poly- (N, N- ethyl acrylamide)(PDEAM), poly- (N- vinyls acyl in oneself
Amine)(PVCL)With poly- (2- isopropyl -2- oxazolines)(PIPO), polyethylene glycol oxide-polypropylene oxide-polyethylene glycol oxide three block
Copolymer(PEO-PPO-PEO, Pluronic), these polymer show huge application potential in intellectual material field.
The temperature sensitive type water-soluble polymer solution or gel base smart window for appearing in the newspapers includes:HPC or HPMC adds additive as main material
It is configured to aqueous solution or gelinite(Sol.Energ.Mat.Sol.Cells 1998,54:203-211;Door and window 2009,4:42-
44;CN1621458A;CN1986630A), PVME based sols or gel(New Building Materials 2007,34:32-34;
US5404245), PNIPA base gels(Polym.Adv.Technol.2003,14:757–762)It is placed in glass sandwich or is made
Film.One important feature of temperature sensitive polymer can be separated on critical temperature LCST, is changed into by clear state muddy
Turbid state, there may come a time when that precipitation can be generated;But if making body gel, its disadvantage is accompanied by the change of transparency and can also
The obvious volume contraction of generation.When being applied to smart window, liquid system cannot film forming, can only be used as Sandwich filling material, for a long time
Easily there is layering during use with flocculation;Solid gel system can be prevented effectively from the generation of the problems referred to above, except as interlayer
Material can also be used individually with membrane material, but must assure that gel film itself does not occur Volume-phase transition and epidermis corrugation.Therefore,
It is contemplated that by temperature sensitive polymer uniform dissolution in other aquogel systems that split-phase will not occur.Document [New Building Materials
2007,34:32-34] and patent(CN101608021B)PVME or NIPA based polyalcohols are mutually through at into cross-linking polyvinyl alcohol(PVA)
Based aquagel system, obtains the intelligent light modulation film with certain elasticity and toughness.Patent CN1986630A is then special
Profit(CN1621458A)On the basic components of technology, a kind of gel such as xanthan gum, carrageenan or gellan gum are added again, obtain
Obtained the solid film under room temperature.Document [Smart Mater Struct.2011,20:075005] then by the polyoxygenated of Thermo-sensitive
Ethylene-polypropylene oxide-polyethylene glycol oxide/OPEO(PEO-PPO-PEO/TX-100)Mixed system is aided with it
Its additive is embedded in agarose gel, is prepared for intelligent light modulation film.The above-mentioned solid-state as temperature sensitive polymer carrier reported
Although hydrogel overcomes liquid polymer solution shortcoming inherently, but there is also some shortcomings:If PVA systems are although can
To give high resiliency and toughness, but the author have proven to PVA macromole be particularly at low ambient temperatures winter be easy to crystallization separate out and
Cause the irreversible muddiness of film;Although xanthan gum, carrageenan or gellan gum can be by temperature sensitive polymer solution solid states, it is only
It is crosslinked by physical action, its mechanical performance is difficult to reach the requirement being used alone as film;Although agarose aquogel has
There is certain intensity, but need in preparation process in high temperature environments by all film forming raw material mix homogeneously, in proceeding to mould
Cooling film forming, because temperature sensitive polymer is assembled under high temperature, need to ensure that its is dispersed using ultrasonic vibration, and entirely grasp
Need to be completed under high temperature, this undoubtedly increased the triviality of energy resource consumption and operation.
The content of the invention
For some shortcomings that current smart window exists with temperature-sensitive hydrogel light control material, the present invention is intended to provide a kind of tool
There are certain mechanical performance, the water-setting gum base intelligent light modulation film containing temperature sensitive polymer and preparation method thereof.
To reach the above-mentioned purpose of the present invention, can be realized by following technical scheme:
The present invention provides a kind of preparation method of intelligent light modulation film, and the method is comprised the following steps:Temperature sensitive polymer is molten
Xie Yu does not have among the polyalcohol hydrogel main body of temperature sensitive effect, wherein the polyalcohol hydrogel main body passes through water-soluble mono
Body carries out radical polymerization in the presence of cross-linking agent, first will
Temperature sensitive polymer 0.25-5wt%;
Water-soluble monomer 2-30wt%;
Cross-linking agent 0.1-5wt%;
Transition temperature regulator 0-5wt%;With
Reinforcing agent 0-5wt%
Under stirring, it is dissolved in the water of 50-97.65wt%, all components total amount is 100wt%, after mix homogeneously,
If necessary letting nitrogen in and deoxidizing, adds initiator, then proceeds to mould, stands polymerization, obtains final product the intelligent light modulation film.
In order that intelligent light-control material has the high grade of transparency and certain mechanical strength, and ensure using temperature range
Inside there is no obvious volume contraction or expansion, need temperature sensitive polymer(Such as HPC, HPMC, PVME and PNIPA)It is dissolved in
With good transparency and mechanical strength, and in the main body aquogel system stable using temperature range inner volume.In order that
Polymer is uniformly dissolved in bulk gel system, needs first in aqueous to dissolve temperature sensitive polymer and water-soluble monomer
Even, then carrying out crosslinking to system makes its gelation, to obtain intelligent dimming membrane material.
Present invention employing is bulk gel as the carrier of temperature sensitive polymer without phase transformation hydrogel.First by temperature sensitive polymer
HPC, HPMC, PNIPA or PVME, water-soluble monomer, cross-linking agent and other additives such as critical transition temperature regulator and/or increasing
Strong agent is dissolved in aqueous solution, obtains the solution of homogeneous transparent.Radical polymerization initiator is subsequently adding, and polymerization system is fallen
In entering film die, in room temperature under airtight condition(≤30℃)Cause polymerization, you can varied with temperature and clear state occurs
The intelligent light-control material of ← → muddy state reversible transition.
Water-soluble monomer include acrylamide, N, N- DMAAs, acrylic acid and its salt,(Methyl)Acrylic acid hydroxyl
Ethyl ester etc..Cross-linking agent is characterized in that on individual molecule containing two or more double bonds, including but N, N- methylene bisacrylamide acyl
The water solublity polyfunctional monomers such as double (methyl) acrylate of amine, double (methyl) acrylic acid glycol esters, Polyethylene Glycol.The present invention
Selected monomer and cross-linking agent is all that this area scientific research personnel is familiar with and conventional material.In order to adjust phase transition temperature to adapt to
Different applied environment, it is sometimes desirable to add transition temperature regulator such as inorganic salt and/or surfactant.Selected inorganic salt bag
Include one or more in lithium, sodium, potassium, calcium, magnesium, the chloride of ammonium plasma, sulfate, nitrate, rhodanate etc..Surface
Activating agent includes anionic surfactant such as long chain alkyl sulfates, sulfonate or benzene sulfonate, cation surface activating
The agent such as chloride of chain alkyl trimethyl or triethyl ammonium salt, bromide, nonionic surfactant such as long chain alkylphenol gathers
Oxygen vinyl Ether OP or TX class surfactant.In order to reach the mechanical strength of needs, some packing type reinforcing agents can also be added,
Selected filler must in aqueous can be dispersed with the guarantee system transparency with nano-scale dimension, but while and can not be to temperature
The Thermo-sensitive of photosensitive polymerization thing produces impact;Selected filler includes but nano-sized clay and nanosized silica particles.
The formula of synthesis hydrogel base intelligent light-control material is as follows:
Temperature sensitive polymer 0.25-5wt%;
Water-soluble monomer 2-30wt%;
Cross-linking agent 0.1-5wt%;
Transition temperature regulator 0-5wt%;
Reinforcing agent 0-5wt%;
Water 50-97.65wt%
Optimization formula is as follows:
Temperature sensitive polymer 0.3-2wt%;
Water-soluble monomer 5-25wt%;
Cross-linking agent 0.1-2wt%;
Transition temperature regulator 0-3wt%;
Reinforcing agent 0-5wt%;
Water 63-94.6wt%
Above-mentioned raw materials are used to prepare polymerization system, to obtain gel, it is necessary to caused poly- using suitable initiator
Close.Initiator system typically adopts oxidation-reduction initiator, thermal initiator or ultraviolet radioactive initiator, and initiator used is high score
Known to subdomains research worker.Oxidation-reduction system include persulfate-thiosulfate, persulfate-(It is burnt)Sulfurous
Hydrochlorate, persulfate-aminated compoundss, Cericammoniumsulfate -ol class or ammonium ceric nitrate -ol class, hydrogen peroxide and derivant-ferrous ironization
Compound etc.;Thermal initiator includes persulfate, azo-compound etc.;Ultraviolet initiator include water miscible azo-compound, two
Benzene ketone compounds, alkyl ketone compound etc..Suitable initiator system is selected according to the gelation process for being adopted, to protect
Demonstrate,prove the high conversion of homogeneity, the transparency, stability and the monomer of gel.
It is an advantage of the current invention that the intelligent light modulation film for being obtained has certain intensity, temperature sensitivity is good;Prepare
Method is simple, with low cost.Can be used for the glass sandwich of smart window, it can also be used to make adhering film to glass.Under so as to reach low temperature
Ensure sunshading and heat-insulating under indoor fully daylighting, high temperature and reduce the purpose of energy consumption for cooling.Prior can be to avoid PVA systems
Low temperature is easily crystallized and causes irreversible muddy, agarose gel system to need the shortcoming of high-temperature heating mixing and ultrasonic disperse.
Specific embodiment
Further describe how the present invention realizes below by specific embodiment:
Embodiment
According to following formula, the preparation of gel rubber system is carried out, listed numerical value is that percentage of the various materials in total system contains
Amount.
Temperature sensitive polymer PNIPA 1.0wt%;
Acrylamide AM 10wt%;
N, N '-methylene-bisacrylamide BIS 0.4wt%;
Nano-sized clay 1.0wt%;
Water 87.6wt%
10wt% ammonium persulfate solution 260ppm(Relative to above-mentioned solution system gross weight)
10wt% sodium sulfite solution 260ppm(Relative to above-mentioned solution system gross weight)
Under room temperature PNIPA, AM, BIS, nano-sized clay are dissolved in the water by above-mentioned formula, are configured to transparent homogeneous
Solution, after letting nitrogen in and deoxidizing, to system the sodium sulfite solution that concentration is 10wt% is added, and after mix homogeneously, adding concentration is
The ammonium persulfate solution of 10wt%, proceeds to mould after mix homogeneously, sealing, and polymerization is stood under room temperature.Final acquisition has necessarily by force
The viscoelasticity transparent gel material of degree.The gel room temperature(25℃)Under, transmittance is up to 90%;The system starts to become at 33 DEG C
Muddiness, 40 DEG C bleach completely, and transmittance is only 10%;And due to this clear state ← → muddy state turn caused by temperature change
Change is reversible.
Claims (2)
1. a kind of intelligent dimming membrane preparation method, methods described includes:Temperature sensitive polymer is dissolved in and do not have temperature sensitive effect
Among polyalcohol hydrogel main body, wherein the polyalcohol hydrogel main body is carried out by water-soluble monomer in the presence of cross-linking agent
Radical polymerization, first will
Temperature sensitive polymer PNIPA 1.0wt%;
Acrylamide AM 10wt%;
N, N '-methylene-bisacrylamide BIS 0.4wt%;
Nano-sized clay 1.0wt%;
Under stirring, it is dissolved in the water of 87.6wt%, all components total amount is 100wt%, after system mix homogeneously, must
Letting nitrogen in and deoxidizing when wanting, adds the sodium sulfite solution that concentration is 10wt%, after mix homogeneously, adds concentration for 10wt%'s
Ammonium persulfate solution, proceeds to again mould after mix homogeneously, stand polymerization, obtains final product the intelligent light modulation film.
2. it is prepared by a kind of intelligent light modulation film, its method according to claim 1.
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