CN103881422B - Light-operated switch type TiO2 nano-particles surfactant and preparation method thereof - Google Patents
Light-operated switch type TiO2 nano-particles surfactant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a light-operated switch type TiO2 nano-particles surfactant and a preparation method thereof, and the method comprises the following steps: firstly preparing TiO2 nano-particles by using butyl titanate hydrolysis, and using alkylsilane to perform surface modification on the TiO2 nano-particles, placing the modified nano-particles in an n-hexane solution, sufficiently irradiating by using UV light under a stirring state, transforming the alkylsilane grated on the surface of the particles into the short-carbon chain, centrifuging to collect the precipitate, drying the precipitate and then sufficiently grinding to obtain the light-operated switch type TiO2 nano-particles surfactant. The method disclosed by the invention is simple and convenient, strong in operability and has no use for special instrument. The product has good UV light-operated emulsion switch and phase inversion capability, the emulsion switch function and reversible phase effect can be realized through simple non-intervention measurement in UV light/dark standing, and the method has a good application prospect in the industrial field.
Description
Technical field
The present invention relates to field of fine chemical, especially surfactant field.
Background technology
The laudatory title that tensio-active agent have " industrial monosodium glutamate ", almost penetrates into all industrial technical field, one of basic industry becoming national economy.Many commercial runs, such as crude oil recovery, soil remediation, interfacial polymerization, food-processing, medicine such as to prepare at the system all needing to use surfactants stabilize.In most of the cases, often only need it to form emulsion at certain one-phase, after end of processing, need timely break milk separation effective constituent.In addition, tensio-active agent does not participate in chemical reaction usually, uses directly to be discharged afterwards, and this is not only a kind of huge waste, and brings pollution to environment.Surfactant then can solve the problem.Under the stimulation of outside environmental elements, surfactant properties changes between Activity and inactivity, the stage stable emulsion wanted, reaction terminate after can be recovered in time again a certain mutually in, industrial application is extensive.Compared with traditional switch type tensio-active agent, nano particle surfactant relies on few, the easy recovery of its amount of particles, human body is poisoned and environmental pollution little, advantages such as stability is high and receiving much concern.The switching mode nano grain surface promoting agent reported mainly comprises pH, temperature, magnetic field, concentration-response, and pH-temperature, magnetic-temperature, pH-ionic strength double-bang firecracker should wait.
In many industrial application, often require the composition and the thermodynamic state that do not change system, the active matter of original position regulation and control table, with causing emulsion timing (time of response) quantitative (breakdown of emulsion ratio) undergoing phase transition.Now, dexterity, succinct, clean outside stimulus-light-operated are excited into as first-selection.Photoswitch type nano grain surface promoting agent possesses " non-intervention " and " original position regulation and control " born advantage, without the need to changing system environmental parameter, simple operation, and be applicable to Long-distance Control or toxic occasion, be particularly useful for emulsion preparation, sun care preparations, the micro-fluidic system of transparent channel, micro-nano reactor etc. that profit is mutually transparent.In addition, most of switching mode particle table is lived and is depended on the change of its finishing molecule, and photoactive particles table characteristic alive comes from self property, and stable performance is reproducible.But up to now, also do not have the research of photoswitch type nano grain surface promoting agent to report.Compare with the conventional surfactant of hydrophobic tail with lighting change hydrophilic head, the nano grain surface promoting agent of photic wetting property reversible transformation, will be used widely in makeup, coating, food and field of biological pharmacy by means of its inherent environmental friendliness, high stability and high returnability.
Summary of the invention
In view of the above deficiency of prior art, the present invention aims to provide a kind of photoswitch type TiO
2nano grain surface promoting agent and preparation method, make it the above shortcoming overcoming prior art.
Object of the present invention is realized by following means.
1, a kind of photoswitch type TiO
2nano grain surface promoting agent and preparation method, is characterized in that, adopts following step:
A kind of photoswitch type TiO
2nano grain surface promoting agent preparation method, is characterized in that, adopts following step:
The preparation of (a) nano particle: 1) in reaction solution, each volume components ratio is butyl (tetra) titanate: ethanol: deionized water: Glacial acetic acid=9:36:12:40, operates according to the following steps, and butyl (tetra) titanate being added drop-wise to mass ratio is in the ethanol of 95%, Keep agitation; Be added dropwise in the mixed solution of deionized water under whipped state and Glacial acetic acid again, continue to stir, till mixed solution is transparent, obtained vitreosol; 2) vitreosol is transferred to autoclave and carries out 100 ~ 150 DEG C of reacting by heating, the reaction times is 2 hours, and removing supernatant liquid, obtains white TiO
2precipitation; 3) with absolute ethanol washing white TiO
2precipitation, 15000rpm high speed centrifugation 10 ~ 20 minutes, repeats above operation 3 times, abandoning supernatant, collecting precipitation, then adds dehydrated alcohol and fully disperse, and is placed in the oven dry of 50 ~ 60 DEG C, baking oven, obtains purer TiO
2precipitation; 4) TiO of will dry
2precipitation is crushed to powder, is placed in 500 DEG C of retort furnace calcinings 30 ~ 60 minutes, the obtained TiO with photoelectric activity
2nano particle;
The modification of (b) nano particle: 1) get the TiO with photoelectric activity that (a) step obtains
2nano particle, is poured into appropriate H
2o
2in, guarantee H
2o
2the complete submergence TiO of solution
2nano particle, ultrasonic disperse 5 ~ 10 minutes; 2) dispersion liquid is sealed, be placed in dark place magnetic agitation after 4 ~ 8 hours, remove and seal and be placed in the oven dry of 45 ~ 60 DEG C, baking oven; 3) be that the trimethylchlorosilane of 1 ~ 5% or the mixed solution of dodecyltrichlorosilane or silicon fluoride and normal hexane join in the powder after oven dry by the volume ratio prepared, ultrasonic disperse 5 ~ 10 minutes, magnetic agitation, after 8 ~ 12 hours, obtains the TiO of modification
2dispersion liquid; 4) modified TiO will be left standstill
2dispersion liquid, 15000rpm high speed centrifugation 10 ~ 20 minutes, removing supernatant liquid, lower sediment is placed in the oven dry of 40 ~ 50 DEG C, baking oven; 5) oven dry powder is dispersed in normal hexane, UV rayed 24 hours (ultraviolet lamp wavelength 254nm under magnetic agitation state, power 12W, solution distance ultraviolet lamp 10 ~ 15cm), change the alkyl silane of particle surface grafting into short carbon chain, period constantly supplements normal hexane to maintain initial soln liquid level; 6) illumination terminates rear standing suspension liquid, 15000rpm high speed centrifugation 10 ~ 20 minutes, removing upper strata normal hexane, and lower sediment is placed in the oven dry of 40 ~ 50 DEG C, baking oven, and fully obtained particle after grinding, is the TiO with photoswitch function and reversible phase effect
2nano grain surface promoting agent.
The inventive method is adopted to obtain the nano-TiO of the reversible phase inversion of light-operated emulsion
2tensio-active agent invention product, has the reversible transformation ability causing emulsion coalescence, breakdown of emulsion, phase inversion.Stable W/O(water-in-oil) emulsion is in UV-light prolonged exposure coalescence gradually after about 12 hours, complete breakdown of emulsion phase-splitting after about 36 hours, emulsifying power forms stable O/W(oil-in-water again) emulsion; After dark standing O/W emulsion for some time, coalescence, until breakdown of emulsion, can revert to again stable W/O emulsion after emulsification again gradually.Above-mentioned light-operated emulsion transfer capability is still unattenuated after repeatedly UV illumination repeatedly/dark resting cycles.Under this kind of laser nano-control tensio-active agent causes emulsion switch function mainly to rely on UV rayed, the TiO of grafting short carbon chain
2nano grain surface produces great amount of hydroxy group, the hydrophilic ability of nano grain surface promoting agent is strengthened greatly, stable W/O emulsion can be made to change to stable O/W emulsion.After dark standing for some time, TiO
2the hydroxyl on surface reduces gradually, makes TiO
2the short carbon chain of the grafting in surface own is out exposed, and this group has stronger oleophylic performance, can form stable W/O emulsion, finally realizes stable W/O emulsion and changes to stable O/W emulsion.That play emulsion invertible switch transition function is TiO
2nano particle, UV rayed makes it produce both hole and electron, brings out TiO
2neighbouring H
2o molecule becomes hydroxyl.
Accompanying drawing is described as follows:
Fig. 1 is the photoswitch type nano grain surface promoting agent principle of work schematic diagram of product of the present invention: the W/O emulsion of initial (a) nanoparticles stable, the O/W emulsion of (b) nanoparticles stable after UV illumination, c () particle surface oleophylic, (d) particle surface is hydrophilic.
Embodiment
Below in conjunction with accompanying drawing, enforcement of the present invention is further described.But it should be emphasized that embodiment is below exemplary, instead of in order to limit the scope of the invention and apply.In processing step, involved chemical feedstocks and reagent are conventional commercial technical pure.
Embodiment 1
9mL butyl (tetra) titanate being added drop-wise to 36mL mass ratio is in the ethanol of 95%, Keep agitation.Be added dropwise in the mixed solution of 12mL deionized water under whipped state and 40mL Glacial acetic acid again, continue to stir, till mixed solution is transparent, obtained vitreosol.Vitreosol is transferred to autoclave and carries out 150 DEG C of reacting by heating, the reaction times is 2 hours, and removing supernatant liquid, obtains white TiO
2precipitation.With absolute ethanol washing white TiO
2precipitation, 15000rpm high speed centrifugation 10 minutes, repeats above operation 3 times, abandoning supernatant, collecting precipitation, then adds dehydrated alcohol and fully disperse, and is placed in the oven dry of 60 DEG C, baking oven, obtains purer TiO
2precipitation.By the TiO of drying
2precipitation is crushed to powder, is placed in 500 DEG C of retort furnace calcinings 30 minutes, the obtained TiO with photoelectric activity
2nano particle.
The TiO of photoelectric activity will be had
2nano particle, is poured into appropriate H
2o
2in, guarantee H
2o
2the complete submergence TiO of solution
2nano particle, ultrasonic disperse 5 minutes.Dispersion liquid is sealed, is placed in dark place magnetic agitation after 4 hours, removes and seal and be placed in the oven dry of 45 DEG C, baking oven.Join in the powder after oven dry by the mixed solution of the 1mL dodecyltrichlorosilane prepared and 20mL normal hexane, ultrasonic disperse is after 5 minutes, then magnetic agitation 12 hours, the TiO of obtained modification
2dispersion liquid.Modified TiO will be left standstill
2dispersion liquid, 15000rpm high speed centrifugation 10 minutes, removing supernatant liquid, lower sediment is placed in the oven dry of 50 DEG C, baking oven.Be dispersed in normal hexane by oven dry powder, UV rayed 24 hours (ultraviolet lamp wavelength 254nm, power 12W, solution distance ultraviolet lamp 10 ~ 15cm) under magnetic agitation state, period constantly supplements normal hexane to maintain initial level.Illumination terminates rear standing suspension liquid, 15000rpm high speed centrifugation 10 minutes, removing upper strata normal hexane, and lower sediment is dried, and is crushed to powder, obtain stable W/O emulsion and have photoswitch function TiO
2nanometer surfactant.
W/O emulsion is stablized and the TiO with invertible switch function by obtaining
2nanometer surfactant 0.09g puts into 10mL normal hexane, after ultrasonic dispersed 5 minutes, joins in 10mL deionized water.Carry out emulsification (rotating speed is 15000rpm) with Portable high speed decollator, stable W/O emulsion can be formed, as accompanying drawing (a).With power be 12W, wavelength is the ultraviolet lamp prolonged exposure emulsion of 254nm, period keeps emulsion to be in gentle agitation state, reaches emulsion by the effect of UV-light uniform irradiation.Under the irradiation of UV-light, TiO
2react with surrounding water molecules after transition of electron and produce hydroxyl, stable W/O emulsion gradually coalescence until complete breakdown of emulsion.After about 36 hours, with Portable high speed decollator by mixed solution emulsification again (rotating speed 15000rpm), stable O/W emulsion can be formed, as accompanying drawing (b).After dark standing O/W emulsion for some time, coalescence is until breakdown of emulsion gradually, and after about 36 hours, emulsification can revert to again stable W/O emulsion again.Identical through 5 UV illumination repeatedly/dark resting cycles experimental result.Visible, the nanometer surfactant of this research preparation has the light-operated emulsion switch function of UV and reversible phase effect.
Case study on implementation 2
9mL butyl (tetra) titanate being added drop-wise to 36mL mass ratio is in the ethanol of 95%, Keep agitation.Be added dropwise in the mixed solution of 12mL deionized water under whipped state and 40mL Glacial acetic acid again, continue to stir, till mixed solution is transparent, obtained vitreosol.Vitreosol is transferred to autoclave and carries out 150 DEG C of reacting by heating, the reaction times is 2 hours, and removing supernatant liquid, obtains white TiO
2precipitation.By absolute ethanol washing white TiO
2precipitation, 15000rpm high speed centrifugation 10 minutes, repeats above operation 3 times, abandoning supernatant, collecting precipitation, then adds dehydrated alcohol and fully disperse, and is placed in the oven dry of 60 DEG C, baking oven, obtains purer TiO
2precipitation.By the TiO of drying
2precipitation is crushed to powder, is placed in 500 DEG C of retort furnace calcinings 30 minutes, the obtained TiO with photoelectric activity
2nano particle.
The TiO of photoelectric activity will be had
2nano particle, is poured into appropriate H
2o
2in, guarantee H
2o
2the complete submergence TiO of solution
2nano particle, ultrasonic disperse 5 minutes.Dispersion liquid is sealed, is placed in dark place magnetic agitation after 4 hours, removes and seal and be placed in the oven dry of 45 DEG C, baking oven.Join in the powder after oven dry by the mixed solution of the 1mL trimethylchlorosilane prepared and 20mL normal hexane, ultrasonic disperse is after 5 minutes, then magnetic agitation 12 hours, the TiO of obtained modification
2dispersion liquid.Modified TiO will be left standstill
2dispersion liquid, 15000rpm high speed centrifugation 10 minutes, removing supernatant liquid, lower sediment is placed in the oven dry of 50 DEG C, baking oven.After fully pulverizing, be dispersed in by powder in normal hexane, UV rayed 24 hours (ultraviolet lamp wavelength 254nm, power 12W, solution distance ultraviolet lamp 10 ~ 15cm) under magnetic agitation state, period constantly supplements normal hexane to maintain initial soln liquid level.Illumination terminates rear standing suspension liquid, 15000rpm high speed centrifugation 10 minutes, and removing upper strata normal hexane, lower sediment is dried, and fully pulverizes rear obtained TiO
2nano particle, is stable W/O emulsion and has the TiO of photoswitch function
2nanometer surfactant.
W/O emulsion is stablized and the TiO with reversible phase inversion function by obtaining
2nanometer surfactant 0.09g puts into 10mL kerosene, after ultrasonic dispersed 5 minutes, joins (massfraction of methylene blue solution is 0.05%) in 10mL methylene blue solution.Carry out emulsification (rotating speed is 15000rpm) with Portable high speed decollator, form stable W/O emulsion, as shown in accompanying drawing (a).Power be 12W, wavelength be the ultraviolet lamp of 254nm under prolonged exposure, period keep emulsion be in gentle agitation state, reach emulsion by the effect of UV-light uniform irradiation.Under the irradiation of UV-light, TiO
2produce hydroxyl with neighbouring water molecule reaction after transition of electron, stable W/O emulsion gradually coalescence until complete breakdown of emulsion.With Portable high speed decollator by mixed solution emulsification again (rotating speed is 15000rpm), stable O/W emulsion can be formed.After dark standing O/W emulsion for some time, coalescence, until breakdown of emulsion, can revert to again stable W/O emulsion after emulsification again gradually.Identical through 5 UV illumination repeatedly/dark resting cycles experimental result.Visible, the nano grain surface promoting agent of preparation has the light-operated emulsion switch function of UV and reversible phase effect.
The photoswitch type nano grain surface promoting agent that the present invention obtains is significant in industrial production.
This achievement in research has very wide application prospect in makeup, food, health care, type material, medicament slow release, field of petrochemical industry.
Claims (2)
1. a photoswitch type TiO
2nano grain surface promoting agent preparation method, is characterized in that, adopts following step:
The preparation of (a) nano particle: 1) in reaction solution, each volume components ratio is butyl (tetra) titanate: ethanol: deionized water: Glacial acetic acid=9:36:12:40, operates according to the following steps, and butyl (tetra) titanate being added drop-wise to mass ratio is in the ethanol of 95%, Keep agitation; Be added dropwise in the mixed solution of deionized water under whipped state and Glacial acetic acid again, continue to stir, till mixed solution is transparent, obtained vitreosol; 2) vitreosol is transferred to autoclave and carries out 100 ~ 150 DEG C of reacting by heating, the reaction times is 2 hours, and removing supernatant liquid, obtains white TiO
2precipitation; 3) with absolute ethanol washing white TiO
2precipitation, 15000rpm high speed centrifugation 10 ~ 20 minutes, repeats above operation 3 times, abandoning supernatant, collecting precipitation, then adds dehydrated alcohol and fully disperse, and is placed in the oven dry of 50 ~ 60 DEG C, baking oven, obtains purer TiO
2precipitation; 4) TiO of will dry
2precipitation is crushed to powder, is placed in 500 DEG C of retort furnace calcinings 30 ~ 60 minutes, the obtained TiO with photoelectric activity
2nano particle;
The modification of (b) nano particle: 1) get the TiO with photoelectric activity that (a) step obtains
2nano particle, is poured into appropriate H
2o
2in, guarantee H
2o
2the complete submergence TiO of solution
2nano particle, ultrasonic disperse 5 ~ 10 minutes; 2) dispersion liquid is sealed, be placed in dark place magnetic agitation after 4 ~ 8 hours, remove and seal and be placed in the oven dry of 45 ~ 60 DEG C, baking oven; 3) be that the trimethylchlorosilane of 1 ~ 5% or the mixed solution of dodecyltrichlorosilane or silicon fluoride and normal hexane join in the powder after oven dry by the volume ratio prepared, ultrasonic disperse 5 ~ 10 minutes, magnetic agitation, after 8 ~ 12 hours, obtains the TiO of modification
2dispersion liquid; 4) modified TiO will be left standstill
2dispersion liquid, 15000rpm high speed centrifugation 10 ~ 20 minutes, removing supernatant liquid, lower sediment is placed in the oven dry of 40 ~ 50 DEG C, baking oven; 5) oven dry powder is dispersed in normal hexane, UV rayed 24 hours under magnetic agitation state; Ultraviolet lamp wavelength 254nm, power 12W used, solution distance ultraviolet lamp 10 ~ 15cm; Change the alkyl silane of particle surface grafting into short carbon chain, period constantly supplements normal hexane to maintain initial soln liquid level; 6) illumination terminates rear standing suspension liquid, 15000rpm high speed centrifugation 10 ~ 20 minutes, removing upper strata normal hexane, and lower sediment is placed in the oven dry of 40 ~ 50 DEG C, baking oven, and fully obtained particle after grinding, is the TiO with photoswitch function and reversible phase effect
2nano grain surface promoting agent.
2. a photoswitch type TiO
2nano grain surface promoting agent, is characterized in that, adopts photoswitch type TiO described in claim 1
2nano grain surface promoting agent preparation method obtains.
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| CN104127335B (en) * | 2014-08-05 | 2016-08-17 | 西南交通大学 | A kind of UV controlled release medicinal ingredient and the preparation technology of easy cleaning Pickering emulsion-type sunscreen cream |
| CN104841345B (en) * | 2015-04-21 | 2017-05-17 | 西南交通大学 | Photomagnetic dual-response Pickering emulsion coalescence reaction system and application thereof |
| CN108398395B (en) * | 2018-01-09 | 2021-06-22 | 华南师范大学 | Light-operated reversible color changing method and device |
| CN109233366B (en) * | 2018-07-09 | 2020-09-11 | 西南交通大学 | Method for preparing nano titanium dioxide coating with gradient wettability |
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