CN107831164A - A kind of preparation method of the intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function - Google Patents
A kind of preparation method of the intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function Download PDFInfo
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- CN107831164A CN107831164A CN201710887322.6A CN201710887322A CN107831164A CN 107831164 A CN107831164 A CN 107831164A CN 201710887322 A CN201710887322 A CN 201710887322A CN 107831164 A CN107831164 A CN 107831164A
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Abstract
The present invention relates to a kind of preparation method of the intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function, belongs to material science and analysis detection field.Colloidal photon crystal is scattered in containing in the polymer solution that can be physical crosslinking by this method first, reached the semifixed purpose in the physics polymeric hydrogel of physical crosslinking of photonic crystal by way of freeze-thaw, then it is fixed on again in the hydrogel of another chemical crosslinking and introduces beryllium ion recognition unit by reacting simultaneously, the finally heated hydrogel for removing physical crosslinking, only deposits chemically crosslinked aquagel.Because the effect of beryllium ion and its recognition unit can cause hydrogel Volume Changes, the change of photon crystal micro-ball spacing is driven simultaneously, and photonic crystal hydrogel thin film color change is caused according to Bragg diffraction law and reflection peak is subjected to displacement and then determines contained beryllium ion concentration in solution.The method of this intelligent photonic crystal hydrogel thin film detection beryllium ion with beryllium ion Visual retrieval function has high sensitivity, high specificity, operation is simple, cost is cheap, observation is accurate.
Description
Technical field
Designing material science of the present invention, analysis detection field, more particularly, to a kind of intelligence of highly sensitive detection beryllium ion
Photonic crystal hydrogel thin film material, its preparation method and application.
Background technology
Due to the special nature of beryllium, it is widely used in nuclear power as moderator best in nuclear reactor and reflecting layer
The nuclear industry such as stand.Meanwhile beryllium is led in electronic device, aviation, X-ray tube, refractory ceramics, satellite structure part and space shuttle etc.
Domain is also widely used.But in fact, the compound of all berylliums has very strong pulmonary toxicity and is possible carcinogenic substance.Due to
It can be enriched with by food and water in skin, soft tissue, it is thus possible to serious harm is brought to the health of people,
Such as chronic berylliosis, severe pulmonary disorder etc., and A class carcinogenic substances are classified as by Environmental Protection Agency USA.
The main method of laboratory or industrial circle detection beryllium ion has AAS and AES spectrum, fluorescence spectrophotometer at present
Photometry, voltammetry, inductively coupled plasma method and gas chromatography etc., but these method sample pre-treatments are complicated, step
Rapid cumbersome and expensive equipment is heavy, can not accomplish to detect real-time.Finding one kind being capable of convenient and swift detection beryllium ion in real time
The method of concentration is significant.
Photonic crystal is a kind of periodic structure being made up of the material with different refractivity in space-alternating, due to it
Unique optical properties, it is the study hotspot in the fields such as material science in recent years.Changing the lattice parameter of photonic crystal can cause
Bragg diffraction peak changes, by the way that colloidal photon crystal is semifixed in hydrogel, with reference to the optical of photonic crystal
The sensitivity of matter and hydrogel, it is possible to achieve to the Sensitive Detection of specific compound or ion.
The content of the invention
The present invention solves the technical problem of provide a kind of intelligent photonic with beryllium ion Visual retrieval function
The preparation method of crystal hydrogel thin film and the use intelligent photonic crystal water-setting with beryllium ion Visual retrieval function
The method that glue carries out beryllium ion Visual retrieval in solution, conveniently detects the beryllium in the solution such as seawater, river, sewage
Ion concentration, it compensate for detecting the shortcomings that beryllium ion concentration needs complex instrument and can not detected in real time at present.
In order to solve the above technical problems, one aspect of the present invention is：
A kind of preparation method of the intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function is provided, wrapped
Include following steps：
(1) preparation process of the photonic crystal hydrogel of physical crosslinking：
The polymer that can be physical crosslinking is dissolved in corresponding solvent and forms gel, by colloidal photon crystal with it is upper
State that gel mixes and heating is vibrated repeatedly, to having compared with strong refraction.Then gel is injected in quartz sample pool, and carries out physics friendship
Connection, form photonic crystal-polyalcohol hydrogel of physical crosslinking.
(2) preparation process of the photonic crystal hydrogel with beryllium ion quick in situ detection function：
The physical cross-linking hydrogel that step 1 is obtained is placed in containing in the solution of aggressiveness before 9- crown ethers -3, adds initiator
After carry out chemical crosslink reaction, reaction removed after terminating obtained by chemically crosslinked aquagel, be placed in ultra-pure water and heat remover
The polyalcohol hydrogel of reason crosslinking obtains the photonic crystal hydrogel of the modification of 9- crown ethers -3.
(3) visualization measure of the intelligent photonic crystal hydrogel to beryllium ion
The photonic crystal hydrogel that step 2 prepares is put into the solution containing beryllium ion, it is in situ after saturation to carry out
The measurement of reflectance spectrum and the observation of color change.
The polymer that can be physical crosslinking in step 1 is including but not limited to polyvinyl alcohol, polyurethane, polyethylene glycol and spreads out
Biology, NIPA, chitosan etc..Nanoparticle used in colloidal photon crystal is silica dioxide nano particle
Son, polystyrene nanoparticle, polymethyl methacrylate nano particle, zinc oxide nano-particle, carbosphere, yittrium oxide etc. are single
The one or more of microballoon of being uniformly dispersed assemble, and its mass fraction is can be adjusted according to detection actual requirement.
Preceding oligomer solution described in step 2 is including but not limited to acrylamide, methyl methacrylate, methacrylic acid
Hydroxyl ethyl ester, acetylbutyrylcellulose, siloxanes methacrylate, fluorine silicon methacrylate, perfluoroether or dimethyl allene
Any one or more in sour ethylene glycol mixes.
Chemical crosslink reaction method described in step 2 is specially that ultra violet lamp photochemical reaction or temperature control carry out heat
Solidification.
Another purpose of the present invention is to provide a kind of method of beryllium ion Visual retrieval：
Manufactured hydrogel may specifically bound in the solution containing beryllium ion, basis after reaction finishes
Hydrogel thin film color change or the reflectance spectrum by fiber spectrometer in-site detecting hydrogel in the solution, determine beryllium ion
Content.
The solution that possibility described in step 3 contains beryllium ion can be the aqueous solution or organic solution.
Examined by the intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function of the invention prepared
Survey beryllium ion concentration has advantages below compared with the method for existing detection beryllium ion concentration：
(1) present invention carries out the Visual retrieval of beryllium ion using intelligent photonic crystal hydrogel thin film as carrier, passes through
Visually observe beryllium ion concentration in solution, without gather sample take back laboratory can effectively judge in solution whether containing beryllium from
Son pollution, it is convenient and swift and there is real-time, by the use of fiber spectrometer, the presence of trace beryllium ion can be detected.
(2) beryllium ion recognition unit is combined by the present invention with intelligent photonic crystal hydrogel thin film, is known using beryllium ion
The change of volume causes the band gap variation of photonic crystal to be detected after other molecule combination beryllium ion, the change of the photon band gap
The change of the intelligent photonic crystal hydrogel thin film color can be brought by changing, while the movement of wavelength, energy occur for its reflectance spectrum
Differentiated easily by human eye so that detection instrument greatly simplifies, and testing cost substantially reduces.
(3) the invention provides a kind of universality method, change the species of recognition unit, can carry out multiple compounds and
The detection of ion.
Brief description of the drawings
Fig. 1 is photon crystal micro-ball scanning electron microscope (SEM) photograph.
Fig. 2 is intelligent photonic crystal hydrogel thin film scanning electron microscope (SEM) photograph.
Embodiment
Such scheme is described further below in conjunction with specific embodiment.It should be understood that these embodiments are to be used to illustrate
The present invention and be not limited to limit the scope of the present invention.The implementation condition used in embodiment can be done according to the condition specifically detected
Further adjustment, unreceipted implementation condition is usually the condition in normal experiment.Any those skilled in the art, do not taking off
In the case of from the spirit and scope of the present invention, it be able to should make various changes and modifications, therefore protection scope of the present invention
Appended claims limited range should be considered as.
Embodiment 1
(1) preparation process of the photonic crystal hydrogel of physical crosslinking：
Polyvinyl alcohol is added in dimethyl sulfoxide (DMSO) and dissolved by heating at 100 DEG C, then adds ultra-pure water mixing simultaneously
It is standby to be cooled to room temperature.Monodispersed 100nm polystyrene nanoparticle is scattered in ultra-pure water, makes its mass fraction be
5%, the colloidal photon crystal that mass fraction is 5% is mixed with above-mentioned polyvinyl alcohol gel, then heats and vibrates, is added repeatedly
Heat simultaneously vibrates multiple.Then 0.5ml mixed gels are injected in quartz sample pool, superfreeze 1h, is then placed in normal-temperature water
Middle defrosting 5h, form photonic crystal-polyvinyl alcohol hydrogel of physical crosslinking.
(2) preparation process of the photonic crystal hydrogel with beryllium ion quick in situ detection function：
The physical cross-linking hydrogel that step 1 is obtained is cut into 1 × 1cm2Fritter it is standby.It is 10% to prepare mass fraction
Acrylamide solution 5ml, add aggressiveness 0.002g before N ' N- methylene-bisacrylamides 0.01g, 9- crown ether -3, light trigger
15 microlitres, then the hydrogel of well cutting is placed in in the preceding oligomer solution configured dark placement a period of time, then taken out
It is placed in quartz sample pool, and adds remaining preceding oligomer solution, quartz sample pool is put under uviol lamp and carries out reaction 1h, instead
Gel mould is taken off after should terminating, and 5 minutes polyvinyl alcohol for removing physical crosslinking are heated in 55 DEG C of ultra-pure waters and obtain 9- crown ethers -3
The photonic crystal hydrogel of modification.
(3) visualization measure of the intelligent photonic crystal hydrogel to beryllium ion
The photonic crystal hydrogel that step 2 prepares is put into the seawater containing beryllium ion, to the end of 30 minutes react
The observation of the measurement and color change in situ for carrying out reflectance spectrum afterwards, determine the concentration of beryllium ion.
Embodiment 2
(1) preparation process of the photonic crystal hydrogel of physical crosslinking：
Polyurethane is added in ultra-pure water and dissolved by heating at 60 DEG C, it is standby to be subsequently cooled to room temperature.By single dispersing
300nm Nano particles of silicon dioxide be scattered in ultra-pure water, it is 15% to make its mass fraction, is 15% by mass fraction
Colloidal photon crystal mixes with above-mentioned polyvinyl alcohol gel, then heats and vibrates, and heats and is vibrated repeatedly repeatedly.Then will
In 0.5ml mixed gels injection quartz sample pool, superfreeze 5h, the 24h that thaws is then placed in normal-temperature water, forms physics and hand over
Photonic crystal-polyvinyl alcohol hydrogel of connection.
(2) preparation process of the photonic crystal hydrogel with beryllium ion quick in situ detection function：
The physical cross-linking hydrogel that step 1 is obtained is cut into 1 × 1cm2Fritter it is standby.It is 3% to prepare mass fraction
Acrylamide solution 5ml, add aggressiveness 0.005g before N ' N- methylene-bisacrylamides 0.05g, 9- crown ether -3, light trigger
15 microlitres, then the hydrogel of well cutting is placed in in the preceding oligomer solution configured dark placement a period of time, then taken out
It is placed in quartz sample pool, and adds remaining preceding oligomer solution, quartz sample pool is put under uviol lamp and carries out reaction 1h, instead
Gel mould is taken off after should terminating, and 15 minutes polyvinyl alcohol for removing physical crosslinking are heated in 55 DEG C of ultra-pure waters and obtain 9- crown ethers -3
The photonic crystal hydrogel of modification.
(3) visualization measure of the intelligent photonic crystal hydrogel to beryllium ion
The photonic crystal hydrogel that step 2 prepares is put into the river containing beryllium ion, to the end of 30 minutes react
The observation of the measurement and color change in situ for carrying out reflectance spectrum afterwards, determine the concentration of beryllium ion.
Embodiment 3
(1) preparation process of the photonic crystal hydrogel of physical crosslinking：
Add chitosan into dimethyl sulfoxide (DMSO) and dissolved by heating at 80 DEG C, then add ultra-pure water and mix and cool down
It is standby to room temperature.Monodispersed 500nm polymethyl methacrylate and silica mix nanoparticles are scattered in ultrapure
In water, it is 25% to make its mass fraction, and the colloidal photon crystal that mass fraction is 25% is mixed with above-mentioned polyvinyl alcohol gel,
Then heat and vibrate, heat and vibrated repeatedly repeatedly.Then 0.5ml mixed gels are injected in quartz sample pool, ultralow temperature
1h is freezed, the 45h that thaws is then placed in normal-temperature water, forms photonic crystal-polyvinyl alcohol hydrogel of physical crosslinking.
(2) preparation process of the photonic crystal hydrogel with beryllium ion quick in situ detection function：
The physical cross-linking hydrogel that step 1 is obtained is cut into 1 × 1cm2Fritter it is standby.It is 20% to prepare mass fraction
Acrylamide solution 5ml, add aggressiveness 0.002g before N ' N- methylene-bisacrylamides 0.01g, 9- crown ether -3, light trigger
15 microlitres, then the hydrogel of well cutting is placed in in the preceding oligomer solution configured dark placement a period of time, then taken out
It is placed in quartz sample pool, and adds remaining preceding oligomer solution, quartz sample pool is put under uviol lamp and carries out reaction 1h, instead
Gel mould is taken off after should terminating, and 30 minutes polyvinyl alcohol for removing physical crosslinking are heated in 55 DEG C of ultra-pure waters and obtain 9- crown ethers -3
The photonic crystal hydrogel of modification.
(3) visualization measure of the intelligent photonic crystal hydrogel to beryllium ion
The photonic crystal hydrogel that step 2 prepares is put into the urine containing beryllium ion, to the end of 30 minutes react
The observation of the measurement and color change in situ for carrying out reflectance spectrum afterwards, determine the concentration of beryllium ion.
Claims (8)
1. a kind of preparation method of the intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function, its feature exist
In its preparation method comprises the following steps：
(1) preparation process of the photonic crystal hydrogel of physical crosslinking：
The polymer that can be physical crosslinking is dissolved in corresponding solvent and forms gel, colloidal photon crystal is coagulated with above-mentioned
Glue mixes and heating is vibrated repeatedly, to having compared with strong refraction.Then gel is injected in quartz sample pool, and is physical crosslinking,
Form photonic crystal-polyalcohol hydrogel of physical crosslinking.
(2) preparation process of the photonic crystal hydrogel with beryllium ion quick in situ detection function：
The physical cross-linking hydrogel that step 1 is obtained is placed in containing in the solution of aggressiveness before 9- crown ethers -3, and it is laggard to add initiator
Gained chemically crosslinked aquagel is removed in row chemical crosslink reaction, reaction after terminating, be placed in heating in ultra-pure water and removed physics friendship
The polyalcohol hydrogel of connection obtains the photonic crystal hydrogel of the modification of 9- crown ethers -3.
(3) visualization measure of the intelligent photonic crystal hydrogel to beryllium ion
The photonic crystal hydrogel that step 2 prepares is put into the solution containing beryllium ion, original position is reflected after saturation
The measurement of spectrum and the observation of color change.
A kind of 2. intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function according to claim 1
Preparation method, it is characterised in that the polymer being physical crosslinking including but not limited to polyvinyl alcohol, polyurethane,
Polyethylene glycol and derivative, NIPA, chitosan etc..
A kind of 3. intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function according to claim 1
Preparation method, it is characterised in that the colloidal photon crystal is received including but not limited to Nano particles of silicon dioxide, polystyrene
The single dispersing uniform microspheres such as rice corpuscles, polymethyl methacrylate nano particle, zinc oxide nano-particle, carbosphere, yittrium oxide
One or more assemble.
A kind of 4. intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function according to claim 1
Preparation method, it is characterised in that preceding oligomer solution described in step 2 be can be formed transparent polymer film organic molecule it is molten
Liquid, including but not limited to acrylamide, methyl methacrylate, hydroxyethyl methacrylate, acetylbutyrylcellulose, siloxanes
Any one or more in methacrylate, fluorine silicon methacrylate, perfluoroether or ethylene glycol dimethacrylate is mixed
Conjunction forms.
A kind of 5. intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function according to claim 1
Preparation method, it is characterised in that the mass fraction of nano particle can will according to specific detection in the colloidal photon crystal
Ask and be adjusted.
A kind of 6. intelligent photonic crystal hydrogel thin film with beryllium ion Visual retrieval function according to claim 1
Preparation method, it is characterised in that chemical crosslink reaction method described in step 2 be specially ultra violet lamp photochemical reaction or
Temperature control carries out heat cure.
A kind of 7. method of beryllium ion Visual retrieval, it is characterised in that
The hydrogel according to made of claim 1 to 6 preparation method may be subjected to spy in the solution containing beryllium ion
The opposite sex combines, reaction finish after according to hydrogel thin film color change or by fiber spectrometer in-site detecting water in the solution
The reflectance spectrum of gel, determine the content of beryllium ion.
8. the method for Visual retrieval beryllium ion according to claim 7, it is characterised in that described possibility contain beryllium from
The solution of son can be the aqueous solution or organic solution arbitrarily containing beryllium ion.
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| CN110437471A (en) * | 2019-07-11 | 2019-11-12 | 郑州轻工业学院 | A kind of viscosity composite hydrogel and its preparation method and application |
| CN110836858A (en) * | 2019-12-05 | 2020-02-25 | 中国科学院化学研究所 | Method for nondestructive real-time detection of chemical reaction process based on photonic crystal |
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| CN110437471A (en) * | 2019-07-11 | 2019-11-12 | 郑州轻工业学院 | A kind of viscosity composite hydrogel and its preparation method and application |
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| CN110836858A (en) * | 2019-12-05 | 2020-02-25 | 中国科学院化学研究所 | Method for nondestructive real-time detection of chemical reaction process based on photonic crystal |
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