CN107441955A - A kind of preparation method of titanium dioxide nano thread woven wire composite membrane - Google Patents
A kind of preparation method of titanium dioxide nano thread woven wire composite membrane Download PDFInfo
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- CN107441955A CN107441955A CN201710789756.2A CN201710789756A CN107441955A CN 107441955 A CN107441955 A CN 107441955A CN 201710789756 A CN201710789756 A CN 201710789756A CN 107441955 A CN107441955 A CN 107441955A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0069—Inorganic membrane manufacture by deposition from the liquid phase, e.g. electrochemical deposition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—Metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
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- Electrochemistry (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
A kind of preparation method of titanium dioxide nano thread woven wire composite membrane of the present invention belongs to inoranic membrane technical field of separation materials, first woven wire cleaning is dried and is placed in filter, the titanium dioxide nano thread dispersion liquid of brand-new is poured onto on woven wire, filter or natural sediment is on woven wire, after solvent all filters out, woven wire is taken out, is dried under the conditions of 25 DEG C, 90%RH constant temperature and humidity；After being kept for 1~2 hour at 100 DEG C, it is warming up to 500~1000 DEG C with 0.1~10 DEG C/min of programming rate and sinters 2~24 hours, obtain titanium dioxide nano thread woven wire composite membrane.The present invention combines woven wire and titanium dioxide nano thread, and the composite membrane of preparation can realize the separation to oil water mixture and oil emulsion, and the thickness of composite membrane is controllable, repeat usage is high, and membrane flux is big, and rejection is high, film is renewable, and industrialized production can be achieved.
Description
Technical field
The invention belongs to inoranic membrane technical field of separation materials, and in particular to be prepared using titanium dioxide nano thread acidproof resistance to
The high performance titanium dioxide of alkali-woven wire composite membrane.
Background technology
Titanium dioxide film has a very wide range of applications in fields such as photocatalysis, automatically cleaning, UF membranes, nano titania
Line has good hydrophily and underwater oleophobic property in the case where not needing any surface modification, and this causes nano titania
Line has huge application potential in water-oil separating field.With the continuous discharge of life oil-polluted water, and ocean oil leak thing
Part takes place frequently, and oily water separation technique has given play to more and more important effect in terms of sewage disposal.At present, had many forefathers'
Work, metal-ceramic composite membrane is prepared by using oxide or molecular sieve and wire netting are compound, so as to realize profit point
From.For example, Yu Jihong et al. grown one layer of molecular sieve on the net in stainless steel wire, good water-oil separationg film is prepared into, oil
Water separating effect can reach ppm levels [Chem.Sci., 2013,4,591-595]；Cailong Zhou et al. are in titanium metal net
One layer of unformed titanium dioxide nano thread of growth in situ on silk, realize the separation [Chemical of oil water mixture
Engineering Journal,301(2016),249‐256].However, metal-ceramic composite membrane also exposes problems,
As preparation technology is cumbersome, it is necessary to which surface graft modification could be realized super hydrophilic and underwater superoleophobic, this undoubtedly adds metal-pottery
The preparation cost of porcelain composite membrane.
The content of the invention
In order to solve the problems, such as to be mentioned in background technology, it is multiple that the present invention provides a kind of titanium dioxide nano thread-woven wire
Close the preparation method and purposes of film.One layer is deposited on a wire mesh very using the titanium dioxide nano thread dispersion liquid of different-diameter
Thin titanium dioxide nano thread film, is sintered at high temperature afterwards.
Specific technical scheme is as follows：
The preparation method of a kind of titanium dioxide nano thread-woven wire composite membrane, first by woven wire respectively with acetone, second
Twice, naturally dry is standby for alcohol, deionized water supersound washing；A diameter of 5~200nm titanium dioxide nano thread is taken again, is disperseed
In absolute ethyl alcohol, it is ultrasonically treated 1~5 minute, is configured to the nano titania that mass concentration is 0.01g/L~1000g/L
Line dispersion liquid；The woven wire dried is placed in filter, the titanium dioxide nano thread dispersion liquid of brand-new is poured onto gold
Belong on silk screen, filter or natural sediment is on woven wire, after solvent all filters out, take out woven wire, 25 DEG C, 90%
Dried under the conditions of RH constant temperature and humidity；After being kept for 1~2 hour at 100 DEG C, heated up with 0.1~10 DEG C/min of programming rate
Sintered 2~24 hours to 500~1000 DEG C, obtain titanium dioxide nano thread-woven wire composite membrane.
The dosage of described titanium dioxide nano thread, it is preferably every square centimeter to use 0.2mg~5mg, herein preferred model
Outside enclosing, less than 0.2mg/cm2, silk screen can not be completely covered in nano wire；
Described natural sediment, refer to woven wire being placed in Suction filtration device, titanium dioxide nano thread ethanol is disperseed
After liquid is poured onto on woven wire, without vavuum pump vacuumizing filtration, but gravity natural subsidence is used.
Described sintering temperature, preferably 600~900 DEG C；Sintering environment is air, vacuum, argon gas, nitrogen, hydrogen gas
Atmosphere etc.；Sintering temperature is too low, and the adhesion of nano wire and stainless steel cloth is not strong；Sintering temperature is too high, nano wire can be caused to send out
Raw phase transformation.
Described programming rate, preferably 0.25~1 DEG C/min；Programming rate is too fast, nano wire can be caused to occur disconnected
Split.
Advantages of the present invention and good effect：Stainless steel cloth has the characteristics that intensity is big, flux is high, corrosion-resistant.This
The selected stainless steel cloth of invention has protective layer, can effectively prevent the damage of nano wire above silk screen.And titanium dioxide
Nano wire has many premium properties such as the big, automatically cleaning of super hydrophilic, corrosion-resistant, antibacterial, specific surface area.The present invention is organic by the two
Combine so that prepared titanium dioxide nano thread-woven wire composite membrane can be realized to oil water mixture and breast
The separation of carburetion.The thickness of the composite membrane is controllable, and repeat usage is high, and membrane flux is big, and rejection is high, and film is renewable, can be real
Existing industrialized production.
Brief description of the drawings
Fig. 1:The photo in kind of stainless steel cloth disk used in the embodiment of the present invention 3.
Fig. 2：0.2mg/cm is deposited on the net in stainless steel wire in the embodiment of the present invention 42100nm titanium dioxide nano threads
Photo.
Fig. 3:The electron scanning micrograph of stainless steel cloth disk used in the embodiment of the present invention 2.
Fig. 4：0.2mg/cm is deposited on the net in stainless steel wire in the embodiment of the present invention 42100nm titanium dioxide nano threads
Stereoscan photograph.
Fig. 5：1.4mg/cm is deposited on the net in stainless steel wire in the embodiment of the present invention 62100nm titanium dioxide nano threads
Stereoscan photograph.
Fig. 6：1.4mg/cm is deposited on the net in stainless steel wire in the embodiment of the present invention 62100nm titanium dioxide nano threads
It is amplified to 2000 times of stereoscan photograph.
Fig. 7：XRD spectrum of the 100nm titanium dioxide nano threads in 200 DEG C and 600 DEG C obtained by the embodiment of the present invention 1
Figure, wherein being TiO corresponding to 200 DEG C2(B) diffraction maximum of phase, it is the diffraction maximum of Anatase corresponding to 600 DEG C.
Fig. 8：Hexamethylene, toluene, silicone oil, soya-bean oil, the underwater contact angle figure of carbon tetrachloride in the embodiment of the present invention 8.Institute
The underwater contact angle for the various oil droplets surveyed is all higher than 150 °.It is underwater superoleophobic film to illustrate obtained composite membrane.
Fig. 9:The photo of oily-water seperating equipment used in the present invention, embodiment 10, embodiment 11, embodiment 12；
Figure 10：The pure water flux figure that the embodiment of the present invention 9 is tested.
Figure 11：The photo before oil water mixture separation process in the embodiment of the present invention 10.
Figure 12：The photo after oil water mixture separation stabilization in embodiment 10 of the present invention.
Figure 13：The photo of oil emulsion before being separated in the embodiment of the present invention 11.
Figure 14:The photo of filtrate after being separated in the embodiment of the present invention 11.
Figure 15:The microphotograph of oil emulsion before being separated in the embodiment of the present invention 11.
Figure 16:The microphotograph of filtrate after being separated in the embodiment of the present invention 11.
Embodiment
Embodiment 1
0.3g P25 are taken, are placed in 70ml 10M NaOH solution, after being sufficiently stirred 30 minutes.Load 100ml reactors
In, reacted 4 days at 200 DEG C.Taken out after being cooled to room temperature.In obtained sodium titanate add 200ml10M nitric acid carry out from
Son exchanges, magnetic agitation 2 hours.It is repeated 2 times.After obtained metatitanic acid centrifuges out, 2 times are washed with deionized, ethanol
Washing is three times, standby.The nanowire diameter being prepared under the conditions of this is in 100nm or so, and it is in 200 DEG C and 600 DEG C of XRD
Spectrum is as shown in Figure 7.
Embodiment 2
0.3g P25 are taken, are placed in 70ml 10M NaOH solution, after being sufficiently stirred 30 minutes.Load 100ml reactors
In, reacted 4 days at 150 DEG C.Taken out after being cooled to room temperature.The nitric acid that 200ml10M is added in obtained sodium titanate carries out ion
Exchange, magnetic agitation 2 hours.It is repeated 2 times.After obtained metatitanic acid centrifuges out, it is washed with deionized 2 times, ethanol is washed
Wash three times, it is standby.The nanowire diameter being prepared under the conditions of this is in 10nm or so.
Embodiment 3
The stainless steel cloth disk that specification is 30mm*2mm is taken to use acetone, ethanol, deionized water supersound washing twice respectively,
Naturally dry, standby, photo and stereoscan photograph difference in kind is as shown in Figure 1, Figure 3.
Embodiment 4
The 100nm titanium dioxide nano threads for taking 1mg embodiments 1 to prepare, 100ml absolute ethyl alcohols are added, it is ultrasonic 1 minute,
Natural sediment on stainless steel substrates described in embodiment 3, it is placed in temperature and is 25 DEG C, 12 are dried in the environment of relative humidity is 90%RH
Hour.After dried stainless steel cloth is kept for 1~2 hour at 100 DEG C, with 0.1~10 DEG C/min programming rate liter
Warm to 500 DEG C sinter 2~6 hours, obtain titanium dioxide nano thread-woven wire composite membrane, and photo and ESEM in kind shine
Respectively as shown in Figure 2, Figure 4 shows, the surface density of titanium dioxide nano thread is 0.2mg/cm to piece2。
Embodiment 5
The 100nm titanium dioxide nano threads described in 3mg embodiments 1 are taken, add 100ml absolute ethyl alcohols, it is ultrasonic 1 minute,
Natural sediment on stainless steel substrates described in embodiment 3, it is placed in the climatic chamber that temperature is 25 DEG C, relative humidity is 90%RH
In, dry 12 hours.After dried stainless steel cloth is kept for 1~2 hour at 100 DEG C, with 0.1~10 DEG C/min liter
Warm speed is warming up to 500 DEG C and sintered 2~6 hours, obtains titanium dioxide nano thread-woven wire composite membrane.
Embodiment 6
The 100nm titanium dioxide nano threads described in 10mg embodiments 1 are taken, add 100ml absolute ethyl alcohols, it is ultrasonic 1 minute,
Natural sediment on stainless steel substrates described in embodiment 3, it is placed in the climatic chamber that temperature is 25 DEG C, relative humidity is 90%RH
In, dry 12 hours.After dried stainless steel cloth is kept for 1~2 hour at 100 DEG C, with 0.1~10 DEG C/min liter
Warm speed is warming up to 500 DEG C and sintered 2~6 hours, obtains titanium dioxide nano thread-woven wire composite membrane, stereoscan photograph
Be amplified to 2000 times of stereoscan photograph as shown in Figure 5, Figure 6, the density of titanium dioxide nano thread is 1.4mg/cm2。
Embodiment 7
The 10nm titanium dioxide nano threads described in 3mg embodiments 2 are taken, add 100ml absolute ethyl alcohols, ultrasound 1 minute, in reality
Natural sediment on the stainless steel substrates described in example 3 is applied, is placed in the climatic chamber that temperature is 25 DEG C, relative humidity is 90%RH,
Dry 12 hours.After dried stainless steel cloth is kept for 1~2 hour at 100 DEG C, with 0.1~10 DEG C/min heating
Speed is warming up to 500 DEG C and sintered 2~6 hours, obtains titanium dioxide nano thread-woven wire composite membrane.
Embodiment 8
Titanium dioxide nano thread obtained by embodiment 5 and embodiment 7-woven wire composite membrane is subjected to hexamethylene respectively
The underwater contact angle test of alkane, toluene, silicone oil, soya-bean oil, carbon tetrachloride.Test result is as shown in figure 8, the oil droplet of contact angle test
Volume is 5uL, and the underwater contact angle for the various oil droplets surveyed is all higher than 150 °, and it is underwater superoleophobic to illustrate obtained composite membrane
Film.
Embodiment 9
Titanium dioxide nano thread-gold obtained by stainless steel cloth, embodiment 5 and the embodiment 7 of nano wire will not be deposited
Category silk screen composite membrane carries out pure water flux test respectively, and test result is as shown in Figure 10, and the calculation formula of pure water flux is：Wherein, for V to filter out volume (L), S is membrane area (m2), t is the time (h).Filter pressure is the gravity of water.Its
100nm titanium dioxide nano threads-compound membrane flux of woven wire obtained by middle embodiment 5 is 118Lm-2·h-1, embodiment
Composite membrane 10nm titanium dioxide nano threads-compound membrane flux of woven wire obtained by 7 is 71Lm-2·h-1.Do not have in test
Apply any pressure, only rely on gravity.Titanium dioxide nano thread-woven wire the composite membrane for illustrating to prepare has very high pure water to lead to
Amount.
Embodiment 10
Made titanium dioxide nano thread-woven wire the composite membrane got ready of Example 4, is placed in the filtering shown in accompanying drawing 9
On device.By the mixture of hexamethylene and water (volume ratio 1:1) poured into after being stirred by ultrasonic in filter, water flows down rapidly
By composite membrane, hexamethylene is trapped within composite membrane.Stand place 30 minutes, without under oil droplet, illustrate the present invention prepare
Composite membrane have good separating effect to oil water mixture.Photo before and after water-oil separating is respectively as shown in Figure 11, Figure 12.
Embodiment 11
Made titanium dioxide nano thread-woven wire the composite membrane got ready of Example 7, is placed in the filtering shown in accompanying drawing 9
On device.Hexadecane, deionized water, hexadecyltrimethylammonium chloride are mixed, are prepared into oil emulsion dispersion liquid (profit body
Product ratio is 1：99).It will be poured into after the oil emulsion dispersion liquid ultrasound prepared in filter, water is flowed down rapidly by compound
Film, oil emulsion are trapped within composite membrane, are separated front and rear photo respectively as shown in Figure 13 and Figure 14, are filtered after separating oil emulsion
It is as clear as crystal in liquid, the oil emulsion before filtering and the filtrate after filtering are put and observed under the microscope, respectively such as Figure 15, Tu16Suo
Show, lower floor's filtrate is limpid after separation, can't see oil droplet under the microscope, illustrates that composite membrane has separation effect well to oil emulsion
Fruit.
Embodiment 12
Made titanium dioxide nano thread-woven wire the composite membrane got ready of Example 7, is placed in the mistake shown in accompanying drawing 9
Filter on device.Soya-bean oil, deionized water, hexadecyltrimethylammonium chloride are mixed, are prepared into oil emulsion dispersion liquid (profit volume
Ratio is 1：99).It will be poured into after the oil emulsion dispersion liquid ultrasound prepared in filter, water is flowed down rapidly by compound
Film, oil emulsion are trapped within composite membrane, and lower floor's filtrate is limpid.
Claims (5)
- A kind of 1. preparation method of titanium dioxide nano thread-woven wire composite membrane, first by woven wire respectively with acetone, second Twice, naturally dry is standby for alcohol, deionized water supersound washing；A diameter of 5~200nm titanium dioxide nano thread is taken again, is disperseed In absolute ethyl alcohol, it is ultrasonically treated 1~5 minute, is configured to the titanium dioxide nano thread point that mass concentration is 0.01~1000g/L Dispersion liquid；The woven wire dried is placed in filter, the titanium dioxide nano thread dispersion liquid of brand-new is poured onto wire On the net, filter or natural sediment is on woven wire, after solvent all filters out, take out woven wire, in 25 DEG C, 90%RH Dried under the conditions of constant temperature and humidity；After being kept for 1~2 hour at 100 DEG C, it is warming up to 0.1~10 DEG C/min of programming rate 500~1000 DEG C sinter 2~24 hours, obtain titanium dioxide nano thread-woven wire composite membrane.
- 2. a kind of preparation method of titanium dioxide nano thread-woven wire composite membrane according to claim 1, its feature exist In the dosage of described titanium dioxide nano thread uses 0.2~5mg titanium dioxide nano threads for woven wire every square centimeter.
- 3. a kind of preparation method of titanium dioxide nano thread-woven wire composite membrane according to claim 1, its feature exist In described natural sediment, being that woven wire is placed in Suction filtration device, titanium dioxide nano thread alcohol dispersion liquid be poured onto After on woven wire, without vavuum pump vacuumizing filtration, but gravity natural subsidence is used.
- 4. a kind of preparation method of titanium dioxide nano thread-woven wire composite membrane according to claim 1, its feature exist In sintering temperature is 600~900 DEG C；Sintering environment is air, vacuum, argon gas, nitrogen or hydrogen atmosphere etc..
- 5. according to a kind of preparation method of any described titanium dioxide nano thread-woven wire composite membrane of Claims 1 to 4, Characterized in that, described programming rate is 0.25~1 DEG C/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109046044A (en) * | 2018-09-10 | 2018-12-21 | 苏州大学 | Composite multi-layer network film and the preparation method and application thereof based on sodium titanate nano wire and cobaltosic oxide nano needle |
| CN113481717A (en) * | 2021-07-18 | 2021-10-08 | 陕西科技大学 | Preparation method of modified carbon fiber based on one-dimensional nano material |
| CN114870646A (en) * | 2022-03-28 | 2022-08-09 | 中海油天津化工研究设计院有限公司 | Preparation method of oily sewage treatment dynamic membrane based on metal mesh-ceramic composite base membrane |
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| CN102280264A (en) * | 2011-05-20 | 2011-12-14 | 常州有则科技有限公司 | Titanium/strontium covered nanocrystalline titanium dioxide film for dye-sensitized solar cell and preparation method thereof |
| CN106669431A (en) * | 2016-12-02 | 2017-05-17 | 常州大学 | Preparation method of TiO2 nanowire ultrafiltration membrane with function of simultaneous catalysis and membrane separation |
| CN107080975A (en) * | 2017-06-15 | 2017-08-22 | 河北工业大学 | The preparation method of oil-water separation mesh film with superhydrophilic superoleophobic property |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102280264A (en) * | 2011-05-20 | 2011-12-14 | 常州有则科技有限公司 | Titanium/strontium covered nanocrystalline titanium dioxide film for dye-sensitized solar cell and preparation method thereof |
| CN106669431A (en) * | 2016-12-02 | 2017-05-17 | 常州大学 | Preparation method of TiO2 nanowire ultrafiltration membrane with function of simultaneous catalysis and membrane separation |
| CN107080975A (en) * | 2017-06-15 | 2017-08-22 | 河北工业大学 | The preparation method of oil-water separation mesh film with superhydrophilic superoleophobic property |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109046044A (en) * | 2018-09-10 | 2018-12-21 | 苏州大学 | Composite multi-layer network film and the preparation method and application thereof based on sodium titanate nano wire and cobaltosic oxide nano needle |
| CN113481717A (en) * | 2021-07-18 | 2021-10-08 | 陕西科技大学 | Preparation method of modified carbon fiber based on one-dimensional nano material |
| CN114870646A (en) * | 2022-03-28 | 2022-08-09 | 中海油天津化工研究设计院有限公司 | Preparation method of oily sewage treatment dynamic membrane based on metal mesh-ceramic composite base membrane |
| CN114870646B (en) * | 2022-03-28 | 2024-04-16 | 中海油天津化工研究设计院有限公司 | Preparation method of oily sewage treatment dynamic membrane based on metal mesh-ceramic composite base membrane |
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Application publication date: 20171208 |