CN108439466A - A kind of titania nanoparticles hydrothermal synthesis method - Google Patents
A kind of titania nanoparticles hydrothermal synthesis method Download PDFInfo
- Publication number
- CN108439466A CN108439466A CN201810232209.9A CN201810232209A CN108439466A CN 108439466 A CN108439466 A CN 108439466A CN 201810232209 A CN201810232209 A CN 201810232209A CN 108439466 A CN108439466 A CN 108439466A
- Authority
- CN
- China
- Prior art keywords
- microns
- microfluidic channel
- micro
- titania nanoparticles
- reverse mould
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 16
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000839 emulsion Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012530 fluid Substances 0.000 claims abstract description 12
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims abstract description 12
- 239000011521 glass Substances 0.000 claims abstract description 11
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 10
- 229920005573 silicon-containing polymer Polymers 0.000 claims abstract description 10
- 239000006210 lotion Substances 0.000 claims abstract description 8
- 229920003023 plastic Polymers 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 239000002985 plastic film Substances 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000008236 heating water Substances 0.000 claims abstract description 4
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 8
- 239000004408 titanium dioxide Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 230000008676 import Effects 0.000 claims description 6
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 241000790917 Dioxys <bee> Species 0.000 claims 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 239000005357 flat glass Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000010409 thin film Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 description 12
- 230000008901 benefit Effects 0.000 description 5
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 5
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- -1 polydimethylsiloxanes Polymers 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000002174 soft lithography Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/50—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
A kind of titania nanoparticles hydrothermal synthesis method, includes the following steps：(1) the microfluidic channel figure of two dimensional surface is drawn；(2) pipeline template is printed on transparent plastic film, prepares reverse mould；(3) reverse mould is positioned in open culture dish or glass dish, is mixed well, is poured on reverse mould according to 10: 1 ratio using dimethyl silicone polymer and curing agent, be put into 70 degree of baking ovens and heat 1 hour；(4) microfluidic channel after break the mold must cure is bonded with glass chip bottom, obtains micro-fluid chip；(5) using the aqueous solution of titanium trichloride as water phase, dodecane carries out lotion preparation as oil phase, using micro-fluid chip；(6) it by lotion heating water bath, heats 2 hours, stirs under 70 degrees Celsius, by adjusting the size of emulsion droplet to accurately control the size of titania nanoparticles；(7) water and organic solvent washing, drying are used respectively, are finally characterized.
Description
Technical field
The present invention relates to nano-TiO2 photocatalyst preparing technical fields, specifically, being to be related to a kind of titanium dioxide to receive
Rice grain hydrothermal synthesis method.
Background technology
Titanium dioxide has special physicochemical characteristics and electronic band structure, and photocatalytic activity is high, as photocatalysis
Material is widely used in the research application field of environmental protection and pollution control.The preparation method of TiO2 affects titanium dioxide
The morphosis of catalyst, to also leverage its photocatalysis performance, thus in order to obtain the photocatalysis with high activity
The technology of preparing of agent, TiO2 is also studied extensively and in depth.
Hydro-thermal method is used for nano-powder and prepares in recent years due to having many superiority compared with other wet chemical methods
The attention of people is caused with nano materials research.It prepares with the good nano particle of specific crystalline form, particle dispersion, reaction need to
It to carry out at relatively high temperature.But the reaction time that conventional hydrothermal reaction prepares TiO2 powder is long, and uneven heating is even, obtains
TiO2 nano particle diameters are larger, wider distribution.Therefore, new hydro-thermal reaction system is studied to have great importance.
For microfluid as a kind of novel engineering technology, major advantage is embodied in the size of the microlayer model of preparation, distribution tool
There are the homogeneity of height, and the emulsion preparation method that the microlayer model prepared will be often below macroscopical.Using micro-fluidic technologies system
The precursor liquid of standby synthesis of titanium dioxide nano particle is conducive to the uniform heating of follow-up hydrothermal synthesis, accelerates reaction rate, shortens
Reaction time, raising reaction selectivity etc..Here, we develop a kind of new hydrothermal synthesis method-micro-fluidic technologies hydro-thermal
Synthetic method.This patent utilizes the advantages of micro-fluidic technologies combination hydro-thermal method, prepares nano-TiO2 photocatalyst, Study of Catalyst
Design feature and photocatalysis characteristic, it is intended to seek micro-fluidic technologies TiO2 field of nano photocatalyst preparation practical application.
Invention content
For overcome the deficiencies in the prior art, the present invention provides a kind of titania nanoparticles hydrothermal synthesis methods.
In order to solve the above-mentioned technical problem, the present invention is addressed by following technical proposals：
A kind of titania nanoparticles hydrothermal synthesis method, includes the following steps：
1. drawing the microfluidic channel figure of two dimensional surface using engineering drawing software AutoCAD or Clewin5, design is most
Small feature sizes should be not less than 5 microns；
2. printing pipeline template on transparent plastic film, pipeline color is black, and rest part is still transparent plastic
Film etches photo-curable polymer SU-8 using ultraviolet light lithographic technique, it is micro- for 20-30 microns that height is prepared on silicon chip
The reverse mould of fluid line；
3. the reverse mould that step (2) obtains is positioned in open culture dish or glass dish, polydimethylsiloxanes are used
Alkane and curing agent are mixed well according to 10: 1 ratio, are carefully poured on reverse mould, and it is about 3 to 5 millis to make dimethyl silicone polymer thickness
Rice is put into 70 degree of baking ovens and heats 1 hour, cure dimethyl silicone polymer, as the raw material for making microfluidic channel；
4. break the mold cured after microfluidic channel, by the dimethyl silicone polymer microfluidic channel and glass after solidification
Piece substrate is bonded using ultraviolet plasma method, obtains micro-fluid chip；
5. using the aqueous solution of titanium trichloride as water phase, dodecane carries out lotion system as oil phase, using micro-fluid chip
It is standby；
6. lotion made from reaction is put into heating water bath in glass beaker, heated 2 hours under 70 degrees Celsius, and be added
Magnetic agitation rotor is stirred, and titanium trichloride solution can be reacted with the oxygen in air in this course, and oxidation generates two
Titanium oxide；With the continuous progress of reaction, the titanium dioxide in each emulsion droplet can gradually be nucleated, grow, ultimately forms
The uniform titania nanoparticles of particle size；Size by adjusting emulsion droplet is received to accurately control titanium dioxide
The size of rice grain；
7. by the titania nanoparticles mixed solution of gained respectively use water and organic solvent washing, drying, finally into
Row characterization.
Further, microfluidic channel described in step 4 includes two imports, one outlet；Each import includes one
Microfluid cylindrical filter, it includes the parallel integrated form micro-pipe being made of a plurality of stepped microchannel that gas-liquid/liquid-liquid, which is total at flow nozzle,
Road.
Further, micro-fluid chip whole pipeline overall height is about 25 microns in step 4, and height is about 5 at nozzle
Micron, nozzle width is about 10 microns, and nozzle rear liquid storage pool duct width is about 1 millimeter, and the interval between Filter column is about 5
Micron, remaining common pipe width is about 50 microns.
Further, oil phase contains the Span80 of 2% mass fraction as surfactant in step 5.
Further, in step 6 the big of emulsion droplet is adjusted by adjusting the flow velocity in microfluidic channel, velocity ratio
It is small.
Further, the flow velocity of water phase is about 10~50mL/hr in step 5, and the flow velocity of oil phase is about 2 times of water phase, system
Monodisperse emulsion of the titanium trichloride solution in dodecane is obtained, drop size is probably between 10 microns to 50 microns.
The titania nanoparticles hydrothermal synthesis method of the present invention prepares nano titania compared to traditional hydro-thermal method
Granule technology has the advantages that：
1. under the premise of keeping considerable production flux, the grain size of the titania nanoparticles of gained can be reduced,
And greatly improve the dimensional homogeneity of nano particle；
2, using micro-fluidic technologies for the height controlling of emulsion droplet, we can control the size of emulsion droplet,
To regulate and control the grain size of titania nanoparticles；
3, compared to traditional stirring in water bath heating means are used, it is heated more using emulsion droplet made from micro-fluidic technologies
Adding can uniformly make the growth crystallization of nano particle more controllable, and the reaction time greatly shortens；
4, the microfluidic filter device in this technology can also effectively filter solid impurity, dust in reaction dissolvent
And the precipitate particles being precipitated in solvent, make reaction that can not be filtered with the time ratio of continuous work with long-play
The micro-fluid reactor of device extends several times or even decades of times.
This technology has extensive industrialization, commercial applications foreground, can be applied in environmental protection industry remove formaldehyde material
Material, purification sewage reaction unit, light reaction catalyst etc., expanded can also be used to prepare other inorganic metals or polymer
Nano-particle material creates considerable economic benefit.
Description of the drawings
Attached drawing described herein is used to provide further understanding of the present invention, and is constituted part of this application, this hair
Bright illustrative embodiments and their description are not constituted improper limitations of the present invention for explaining the present invention.In the accompanying drawings：
Attached drawing 1 is the schematic diagram of the present invention.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of without creative work, shall fall within the protection scope of the present invention.
As shown in Figure 1, a kind of titania nanoparticles hydrothermal synthesis method of the present invention, specifically includes following steps：
1. drawing the microfluidic channel figure of two dimensional surface using engineering drawing software AutoCAD or Clewin5, design is most
Small feature sizes should be not less than 5 microns；
2. printing pipeline template on transparent plastic film, pipeline color is black, and rest part is still transparent plastic
Film can be in silicon using ultraviolet light lithographic technique (soft-lithography) etching photo-curable polymer SU-8 (2025)
On piece prepares height as the reverse mould of 20~30 microns of microfluidic channel；
3. reverse mould obtained in the previous step is positioned in open culture dish or glass dish, dimethyl silicone polymer is used
(PDMS) it mixes well according to 10: 1 ratio with curing agent, is carefully poured on reverse mould, make polydimethylsiloxane thickness about
It is 3 to 5 millimeters, is put into 70 degree of baking ovens and heats 1 hour, you can solidification polydimethylsiloxane, as making microfluid pipe
The raw material in road；
4. break the mold is the microfluidic channel after being cured, by the polydimethylsiloxane microfluidic channel after solidification
It is bonded using ultraviolet plasma (UV plasma treatment) method with glass chip bottom, has just obtained final miniflow
Body chip；
5. using the aqueous solution of titanium trichloride as water phase, dodecane (contains the Span80 conducts of 2% mass fraction as oil phase
Surfactant), carry out lotion preparation using micro-fluid chip.The flow velocity of water phase is about 10~50mL/hr, and the flow velocity of oil phase is about
It is 2 times of water phase.Monodisperse emulsion of the titanium trichloride solution in dodecane is made, drop size is probably micro- to 50 at 10 microns
Between rice, and can be by accuracy controlling.
6. lotion made from reaction is put into heating water bath in glass beaker, heated 2 hours under 70 degrees Celsius, and be added
Magnetic agitation rotor is stirred, and titanium trichloride solution can be reacted with the oxygen in air in this course, and oxidation generates two
Titanium oxide.With the continuous progress of reaction, the titanium dioxide in each emulsion droplet can gradually be nucleated, grow, ultimately forms
The uniform titania nanoparticles of particle size.By the size (flow velocity, stream i.e. in microfluidic channel that adjust emulsion droplet
Speed ratio) sizes of titania nanoparticles can also be accurately controlled.
7. by the titania nanoparticles mixed solution of gained respectively use water and organic solvent washing, drying, finally into
Row characterization.
Further, microfluidic channel described in step 4 includes two imports, one outlet；Each import includes one
Microfluid cylindrical filter, it includes the parallel integrated form micro-pipe being made of a plurality of stepped microchannel that gas-liquid/liquid-liquid, which is total at flow nozzle,
Road.
Further, micro-fluid chip whole pipeline overall height is about 25 microns in step 4, and height is about 5 at nozzle
Micron, nozzle width is about 10 microns, and nozzle rear liquid storage pool duct width is about 1 millimeter, and the interval between Filter column is about 5
Micron, remaining common pipe width is about 50 microns.
Substrate of glass involved by this method is normal microscope slide, and dimethyl silicone polymer is (No. CAS：
9016-00-6) commerical grade, the aqueous solution of titanium trichloride (No. CAS：7705-07-9, pH=0.5, mass fraction 20~30%),
Span 80 (No. CAS：1338-43-8), dodecane (No. CAS：112-40-3).
It should be understood that although with reference to its illustrative embodiment, particularly shown and description is carried out to the present invention,
It should be understood by those skilled in the art that without departing substantially from the spirit and model by the present invention as defined in the claims
Under conditions of enclosing, the variation of various forms and details can be carried out wherein, can carry out the arbitrary combination of various embodiments.
Claims (6)
1. a kind of titania nanoparticles hydrothermal synthesis method, it is characterised in that：Include the following steps：
(1) engineering drawing software AutoCAD or Clewin5 is used to draw the microfluidic channel figure of two dimensional surface, the minimum of design
Part dimension should be not less than 5 microns；
(2) pipeline template is printed on transparent plastic film, pipeline color is black, and rest part is still that transparent plastic is thin
Film etches photo-curable polymer SU-8 using ultraviolet light lithographic technique, and the miniflow that height is 20-30 microns is prepared on silicon chip
The reverse mould of body pipeline；
(3) reverse mould that step (2) obtains is positioned in open culture dish or glass dish, using dimethyl silicone polymer and
Curing agent is mixed well according to 10: 1 ratio, is carefully poured on reverse mould, and it is about 3 to 5 millimeters to make dimethyl silicone polymer thickness, is put
Enter 70 degree of baking ovens to heat 1 hour, cure dimethyl silicone polymer, as the raw material for making microfluidic channel；
(4) microfluidic channel after break the mold is cured, by the dimethyl silicone polymer microfluidic channel and sheet glass after solidification
Substrate is bonded using ultraviolet plasma method, obtains micro-fluid chip；
(5) using the aqueous solution of titanium trichloride as water phase, dodecane carries out lotion preparation as oil phase, using micro-fluid chip；
(6) lotion made from reaction is put into heating water bath in glass beaker, is heated 2 hours under 70 degrees Celsius, and magnetic is added
Power stirring rotator is stirred, and titanium trichloride solution can be reacted with the oxygen in air in this course, and oxidation generates dioxy
Change titanium；With the continuous progress of reaction, the titanium dioxide in each emulsion droplet can gradually be nucleated, grow, and ultimately form grain
The uniform titania nanoparticles of diameter；By adjusting the size of emulsion droplet to accurately control nano titania
The size of particle；
(7) the titania nanoparticles mixed solution of gained is used into water and organic solvent washing, drying respectively, finally carries out table
Sign.
2. according to the method described in claim 1, it is characterized in that：Microfluidic channel described in step (4) includes two imports,
One outlet；Each import includes a microfluid cylindrical filter, and it includes micro- by a plurality of step type that gas-liquid/liquid-liquid, which is total at flow nozzle,
The parallel integrated form microchannel of pipeline composition.
3. according to the method described in claim 2, it is characterized in that：Micro-fluid chip whole pipeline overall height in step (4)
About 25 microns, height is about 5 microns at nozzle, and nozzle width is about 10 microns, and nozzle rear liquid storage pool duct width is about 1
Millimeter, the interval between Filter column is about 5 microns, remaining common pipe width is about 50 microns.
4. according to the method described in claim 1, it is characterized in that：Span80 of the oil phase containing 2% mass fraction makees in step (5)
For surfactant.
5. according to the method described in claim 1, it is characterized in that：In step (6) by adjust microfluidic channel in flow velocity,
Velocity ratio adjusts the size of emulsion droplet.
6. according to the method described in claim 1, it is characterized in that：The flow velocity of water phase is about 10~50mL/hr in step (5),
The flow velocity of oil phase is about 2 times of water phase, and monodisperse emulsion of the titanium trichloride solution in dodecane is made, and drop size probably exists
Between 10 microns to 50 microns.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810232209.9A CN108439466A (en) | 2018-03-21 | 2018-03-21 | A kind of titania nanoparticles hydrothermal synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810232209.9A CN108439466A (en) | 2018-03-21 | 2018-03-21 | A kind of titania nanoparticles hydrothermal synthesis method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108439466A true CN108439466A (en) | 2018-08-24 |
Family
ID=63195592
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810232209.9A Pending CN108439466A (en) | 2018-03-21 | 2018-03-21 | A kind of titania nanoparticles hydrothermal synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108439466A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110559198A (en) * | 2019-09-04 | 2019-12-13 | 扬州博科文化发展有限公司 | Method for preparing polypeptide-wrapped anthocyanin microspheres based on microfluidics technology and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504010A (en) * | 2011-11-03 | 2012-06-20 | 厦门大学 | Preparation method of micro-fluidic chip interface for two-dimensional protein electrophoretic separation |
| US20150196913A1 (en) * | 2012-11-08 | 2015-07-16 | Wuhan Yzy Biopharma Co., Ltd. | Microfluidic chip for capturing cells and preparing method thereof |
-
2018
- 2018-03-21 CN CN201810232209.9A patent/CN108439466A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504010A (en) * | 2011-11-03 | 2012-06-20 | 厦门大学 | Preparation method of micro-fluidic chip interface for two-dimensional protein electrophoretic separation |
| US20150196913A1 (en) * | 2012-11-08 | 2015-07-16 | Wuhan Yzy Biopharma Co., Ltd. | Microfluidic chip for capturing cells and preparing method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 汪洋: "《气体的吸附及薄膜材料的应用》", 31 December 2016 * |
| 马静云等: ""微流控液滴软模板制备二氧化钛中空微球"", 《色谱》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110559198A (en) * | 2019-09-04 | 2019-12-13 | 扬州博科文化发展有限公司 | Method for preparing polypeptide-wrapped anthocyanin microspheres based on microfluidics technology and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhao et al. | Nanoparticle synthesis in microreactors | |
| Meng et al. | A high efficiency microfluidic-based photocatalytic microreactor using electrospun nanofibrous TiO2 as a photocatalyst | |
| CN106270543A (en) | The method preparing the controlled Triangular nanoplates of arrangement mode continuously | |
| CN103276439A (en) | Preparation method of molecular colloidal photonic crystal beads | |
| Amreen et al. | Miniaturized and microfluidic devices for automated nanoparticle synthesis | |
| Charcosset et al. | Coupling between membrane processes and crystallization operations | |
| CN110237787B (en) | Cellular carbon nanotube porous microsphere and preparation method and application thereof | |
| Peng et al. | A review of microreactors based on slurry Taylor (segmented) flow | |
| WO2005020659A2 (en) | Microchemical method and apparatus for synthesis and coating of colloidal nanoparticles | |
| Stolzenburg et al. | Microfluidic synthesis of metal oxide nanoparticles via the nonaqueous method | |
| Ling et al. | Synthesis and characteristics of silica nano-particles using modified sol–gel method in microreactor | |
| CN104370289A (en) | Micro-channel preparation method of nano silicon dioxide with uniform particle size | |
| CN104386746A (en) | Method for preparing small-size bismuth oxychloride wafer by use of hydrothermal method | |
| Dincau et al. | Capillary sorting of particles by dip coating | |
| CN108439466A (en) | A kind of titania nanoparticles hydrothermal synthesis method | |
| CN211586547U (en) | Micro-reactor | |
| CN108726554A (en) | One kind efficiently preparing evengranular nano barium sulfate method | |
| CN110560188B (en) | Preparation method of multi-stage sample injection micro-fluidic chip for synthesizing Ag/Ag2S/CdS heterojunction | |
| Rambabu et al. | Optofluidic microreactor for the photocatalytic water splitting to produce green hydrogen | |
| Xia et al. | Recent progress in preparation of functional microparticles based on microfluidic technique | |
| CN108525622A (en) | A kind of reaction of high order micro fluidic device and its prepare applications to nanostructures | |
| CN108246187A (en) | A kind of method of micro-fluid chip production lotion or bubble | |
| CN110215942A (en) | Special infiltration surface drop directed transport method based on Gradient Effect | |
| Liang et al. | Rapid preparation of hierarchically porous ceramic microspheres based on UV-curing-assisted molding | |
| Martin et al. | High flow rate microreactors integrating in situ grown ZnO nanowires for photocatalytic degradation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180824 |