CN108187509A - A kind of cobaltous ferrocyanide PVDF hollow-fibre membranes, preparation method and its usage - Google Patents
A kind of cobaltous ferrocyanide PVDF hollow-fibre membranes, preparation method and its usage Download PDFInfo
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- CN108187509A CN108187509A CN201810072946.7A CN201810072946A CN108187509A CN 108187509 A CN108187509 A CN 108187509A CN 201810072946 A CN201810072946 A CN 201810072946A CN 108187509 A CN108187509 A CN 108187509A
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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
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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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
- B01D69/08—Hollow fibre membranes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The present invention discloses cobaltous ferrocyanide PVDF hollow-fibre membranes, preparation method and its usage.The preparation method using chemical method can will to caesium have efficient removal rate ferrocyanide cobalt nano-particle it is silicon dioxide carried in PVDF hollow fiber membrane surfaces by intermediate.Amination silica grain size used in preparation is 300nm, a concentration of 0.05% 0.5% (mass/volumes), and the cobaltous ferrocyanide load number of plies is 3 layers.Cobaltous ferrocyanide PVDF hollow-fibre membranes prepared by this method can reach the removal rate of caesium within 6 hours more than 99.5% (silica concentration 0.5%, caesium influent concentration are 100 μ g/L).Cobaltous ferrocyanide PVDF hollow-fibre membrane preparation process is simple simultaneously, of low cost, to caesium removal rate height.Therefore, it has broad application prospects in the water body processing containing caesium.
Description
Technical field
The invention belongs to technical field of water pollution control, and in particular to a kind of cobaltous ferrocyanide PVDF hollow-fibre membranes, system
Preparation Method and application thereof.
Background technology
In recent years, process of industrialization acceleration and energy demand be continuously increased so that the traditional energies such as petrochemical industry and water conservancy are
Social development demand cannot be met, this provides the foundation condition for nuclear industry fast development.Therefore, nuclear industry is in prosperities such as America and Europes
Country is rapidly developed in recent years, has built a large amount of nuclear power station and various nuclear reactors and nuclear power ships.China these
Also it greatly develops nuclear energy year, and several inland large nuclear power stations will be built in future.And as China carries forward vigorously Nuclear Power Development
Cause, the yield of radioactive wastewater will be also continuously increased.In worldwide, the radionuclide of high concentration is moving
It is detected in prestige, Greece, Spain, the U.S., Japan and Chinese water body.On the other hand, it is had occurred and that in mankind's nuclear energy uses history
A lot of serious nuclear safety accidents.Chernobyl nuclear leakage accident such as last century the eighties is the tightest so far
The nuclear safety accident of weight causes 9.3 ten thousand people dead when cancer is suffered from radiation, and about 6,000,000 people are encroached on by radiation.In March, 2011
After the nuclear leakage accident of Fukushima, Japan nuclear power station occurs, the process problem of radioactive wastewater causes global concern again.When
Radioactive wastewater enters environment, and radionuclide therein can enter human body by approach such as food chain enrichments, to environment and people
Class health constitutes a threat to, while uneasy and fear can be brought to society, is unfavorable for social harmony stabilization.Caesium in radioactive wastewater
(Cs) typical gamma-rays radioactive source is used as, content is high in waste water, and harmfulness is very big, and long half time was up to 30 years.After for many years, give up
The radioactivity of water and environment Radionuclide will be mainly based on caesium, it is therefore necessary to which the treatment technology of the caesium in waste water is ground
Study carefully.
Radionuclide can only reduce its radioactivity by natural decay, and the processing to radioactive wastewater is substantially logical
After crossing various method concentrations, the radionuclide concentration in its processed waste water is reduced.Hollow-fibre membrane be at present it is more advanced and
Ripe membrane technology, loading density is small, at low cost, low energy consumption, can remove water part particle and larger molecular organics, but right
Waterborne radioactivity nucleic removal effect can be ignored substantially.Therefore, functional modification is carried out to film and is allowed to have selectivity to caesium
Removal, will make it during radioactive wastewater is handled, and caesium can also be effectively removed by not only removing conventional pollution beyond the region of objective existence.Polyvinylidene fluoride
Alkene (PVDF) chemistry, mechanical stability are strong, corrosion-resistant, are excellent membrane modifying materials.Ferrocyanide has caesium very high
Selective adsorption, in recent years its become removal Nuclide Cs research hotspot.Wherein cobaltous ferrocyanide (CoFC) selects to adsorb to Cs
Property is very strong.Directly by CoFC be carried on PVDF hollow fiber membrane surfaces will Severe blockage fenestra, reduce film properties.Nanometer two
Silica (SiO2) hydrophily is strong, the intermediate of link PVDF and CoFC is can not only be used for, and can weaken CoFC loads causes film to lead to
Measure the influence being greatly reduced.Therefore, CoFC is passed through into SiO2It is carried on PVDF hollow fiber membrane surfaces film will be made to have selection and go
Except the function of Cs, it is expected to for the environment remediation of extensive Spent Radioactive water pollution.
Invention content
It is an object of the invention to overcome the technical issues of being mentioned in above-mentioned background technology, a kind of cobaltous ferrocyanide is provided
PVDF hollow-fibre membranes, preparation method and its usage.Cobaltous ferrocyanide doughnut membrane stability prepared by this method is strong, load
Amount is big, can efficiently remove the Cs in water body.
The present invention first technical solution be：A kind of preparation method of cobaltous ferrocyanide PVDF hollow-fibre membranes, including
Four steps：The cleaning of PVDF hollow-fibre membranes, film surface chemical activation, intermediate SiO2Film surface fixes, cobaltous ferrocyanide
Immobilization：
1) PVDF hollow-fibre membranes clean：The both ends of PVDF hollow-fibre membranes are sealed with epoxide-resin glue, room temperature solidification
It after for 24 hours, is placed in 12h in ultra-pure water and cleans up, then be placed in 60min in ethanol solution, remove film surface excess particles and organic
Pollutant, the basement membrane cleaned up；
2) film surface chemical activation：The potassium hydroxide that the basement membrane cleaned up in step 1) is put into a concentration of 1mol/L is molten
In liquid, the tetrabutyl ammonium fluoride of 5g/L is added in, 45 DEG C of constant temperature, which stand 60min, makes film surface carry out hydroxylating；Then film is put into
In the solution of sodium bisulfite of a concentration of 1mol/L, the concentrated sulfuric acid that volume ratio is 0.06% is added in, constant temperature is stood at 45 DEG C
60min；Film is put into the hexane solution for the pyromellitic trimethylsilyl chloride that mass percent is 0.8% again, constant temperature is stood at 20 DEG C
10min, the film after being activated；
3) intermediate SiO2Film surface is fixed：In advance by amination SiO2The ultrasonic disperse 9min in ethanol solution, SiO2Second
Alcoholic solution；Film after activation in step 2) is put into SiO2In ethanol solution, under the conditions of 100rpm, 25 DEG C of constant temperature oscillation 60min,
Make SiO2Film surface is fixed on by chemical bond；SiO was loaded by above-mentioned2Film taking-up be placed in 7min in 70 DEG C of baking ovens, add
Strong SiO2In film surface solidification effect, obtain surface and fix amination SiO2The PVDF hollow-fibre membranes of layer；
4) cobaltous ferrocyanide cures：Amination SiO is fixed on surface in step 3)2The PVDF hollow-fibre membranes of layer are put into dense
It spends in the cobalt chloride solution for 0.5mol/L, under 25 DEG C of constant temperatures, 120rpm oscillations 2h；Then film is put into a concentration of
In the sodium ferrocyanide solution of 0.5mol/L, under 25 DEG C of constant temperatures, 150rpm oscillations 4h；Again film is cleaned with ultra-pure water；
Repeat more than cobaltous ferrocyanide curing schedule 2 times；
Film finally is cleaned with ultra-pure water, epoxide-resin glue sealing in composite membrane both ends is cut after being dried at 40 DEG C and is prepared into
Cobaltous ferrocyanide PVDF hollow-fibre membranes.
A concentration of 0.05%-0.5% (mass/volume) of amination silica described in the step 3), grain size are
300nm。
The present invention second technical solution be：A kind of cobaltous ferrocyanide PVDF hollow-fibre membranes, using above-mentioned preparation
Method, the PVDF hollow-fibre membranes, fibre diameter 0.3cm, membrane aperture are 0.1-1 μm.
The present invention third technical solution be：The purposes of above-mentioned cobaltous ferrocyanide PVDF hollow-fibre membranes, for efficient
Except caesium.
Advantageous effect
1st, the ferrocyanide cobalt granule for having efficient removal rate to caesium is passed through SiO by the present invention using chemical method2It is fixed
In PVDF hollow fiber membrane surfaces, it is easy to run off so as to solve ferrocyanide cobalt granule, is not easily recycled the problems such as utilization.It and will be sub-
Cobalt hexacyanoferrate PVDF hollow-fibre membranes are applied to have in wastewater treatment containing Cs efficient, convenient, stable, non-secondary pollution excellent
Point.
2nd, first by chemical bond by intermediate SiO2Be fixed on PVDF hollow fiber membrane surfaces, later using chemical bond by
CoFC is fixed on SiO by step2Particle surface, and then achieve the purpose that CoFC is indirectly secured to PVDF hollow fiber membrane surfaces.It should
Preparation method operating process is simple, and CoFC load capacity is high, and compound membrane stability is strong, and the removal rate of Cs is high, has extensive industry
Change application prospect.
Description of the drawings
Fig. 1 is cobaltous ferrocyanide PVDF hollow fiber membrane surface x-ray photoelectron spectroscopy figures；
Fig. 2 is cobaltous ferrocyanide PVDF hollow fiber membrane surface scanning electron microscope spectrograms：
(a), PVDF hollow-fibre membranes；
(b)、SiO2Layer PVDF hollow-fibre membranes；
(c), cobaltous ferrocyanide PVDF hollow-fibre membranes.
Specific embodiment
Below by specific embodiments and the drawings, the present invention is further illustrated.The embodiment of the present invention is in order to more
Those skilled in the art is made to more fully understand the present invention well, any limitation is not made to the present invention.
Embodiment 1
1) PVDF hollow-fibre membranes clean：The both ends of PVDF hollow-fibre membranes are sealed with epoxide-resin glue, room temperature solidification
It after for 24 hours, is placed in 12h in ultra-pure water and cleans up, then be placed in 60min in ethanol solution, remove film surface excess particles and organic
In pollutant, the basement membrane cleaned up, film surface x-ray photoelectron spectroscopy figure such as Fig. 1 shown in (a), film surface is swept
It retouches shown in electron microscope spectrogram such as Fig. 2 (a)；
2) film surface chemical activation：The potassium hydroxide that the basement membrane cleaned up in step 1) is put into a concentration of 1mol/L is molten
In liquid, the tetrabutyl ammonium fluoride of 5g/L is added in, 45 DEG C of constant temperature, which stand 60min, makes film surface carry out hydroxylating；Then film is put into
In the solution of sodium bisulfite of a concentration of 1mol/L, the concentrated sulfuric acid that volume ratio is 0.06% is added in, constant temperature is stood at 45 DEG C
60min；Film is put into the hexane solution for the pyromellitic trimethylsilyl chloride that mass percent is 0.8% again, constant temperature is stood at 20 DEG C
10min, the film after being activated；
3) intermediate SiO2Film surface is fixed：In advance by the amination SiO of a concentration of 0.5% (mass/volume)2Ultrasound point
The 9min in ethanol solution is dissipated, the film after activation in step 2) is put into SiO2In ethanol solution, under 25 DEG C of constant temperatures,
100rpm shakes 60min, makes SiO2Film surface is fixed on by chemical bond；SiO will be loaded2Film taking-up be placed in 70 DEG C
7min in baking oven strengthens SiO2In film surface solidification effect, obtain surface and fix amination SiO2The PVDF hollow-fibre membranes of layer,
Shown in its film surface scanning electron microscope spectrogram such as Fig. 2 (b)；
4) cobaltous ferrocyanide cures：Amination SiO is fixed on surface in step 3)2The PVDF hollow-fibre membranes of layer are put into dense
It spends in the cobalt chloride solution for 0.5mol/L, under 25 DEG C of constant temperatures, 120rpm oscillations 2h；Then film is put into a concentration of
In the sodium ferrocyanide solution of 0.5mol/L, under 25 DEG C of constant temperatures, 150rpm oscillations 4h；Again film is cleaned with ultra-pure water；It repeats
Cobaltous ferrocyanide curing above step 2 times；Film finally is cleaned with ultra-pure water, by composite membrane both ends epoxy resin after being dried at 40 DEG C
Glue sealing, which is cut, is prepared into cobaltous ferrocyanide PVDF hollow-fibre membranes, is denoted as cobaltous ferrocyanide PVDF hollow-fibre membranes 1, film
Shown in surface Scanning Electron microscope spectrogram such as Fig. 2 (c).
Embodiment 2
The cleaning of PVDF hollow-fibre membranes, film surface chemical activation, intermediate SiO in the present embodiment2Film surface is fixed and Asia
Cobalt hexacyanoferrate curing schedule is with embodiment 1, except that amination SiO in step 3)2A concentration of 0.1% (mass/volume),
It is film-made and is denoted as cobaltous ferrocyanide PVDF hollow-fibre membranes 2.
Embodiment 3
The cleaning of PVDF hollow-fibre membranes, film surface chemical activation, intermediate SiO in the present embodiment2Film surface is fixed and Asia
Cobalt hexacyanoferrate curing schedule is with embodiment 1, except that amination SiO in step 3)2A concentration of 0.05% (quality/body
Product), it is film-made and is denoted as cobaltous ferrocyanide PVDF hollow-fibre membranes 3.
Embodiment 4
The cobaltous ferrocyanide PVDF hollow-fibre membranes prepared in embodiment 1,2 and 3 are respectively used to following caesium removal experiment,
The caesium for investigating different films goes efficiency (as shown in table 1).Experimentation：It is 12.5cm to take effective area2Film, taken using cesium nitrate
Cold experiment is carried out for radionuclide caesium, passes through aqueous solution of the tunica fibrosa negative pressure filter filtering containing 100 μ g/L caesiums, solution ph
It is 7.0, system pressure is -0.9bar, and inlet and permeate sample, the concentration of caesium are taken respectively after filtering 60,180,360min
It is measured by icp ms.
The caesium removal rate of 1 cobaltous ferrocyanide PVDF tunica fibrosas of table
It should be understood that embodiment and example discussed herein simply to illustrate that, to those skilled in the art
For, it can be improved or converted, and all these modifications and variations should all belong to the protection of appended claims of the present invention
Range.
Claims (4)
1. a kind of preparation method of cobaltous ferrocyanide PVDF hollow-fibre membranes, which is characterized in that include the following steps：
1) PVDF hollow-fibre membranes clean：The both ends of PVDF hollow-fibre membranes are sealed with epoxide-resin glue, room temperature solidifies for 24 hours
Afterwards, it is placed in 12h in ultra-pure water to clean up, then be placed in 60min in ethanol solution, removes film surface excess particles and organic contamination
Object, the basement membrane cleaned up；
2) film surface chemical activation：The basement membrane cleaned up in step 1) is put into the potassium hydroxide solution of a concentration of 1mol/L
In, the tetrabutyl ammonium fluoride of 5g/L is added in, 45 DEG C of constant temperature, which stand 60min, makes film surface carry out hydroxylating；Then film is put into dense
It spends in the solution of sodium bisulfite for 1mol/L, adds in the concentrated sulfuric acid that volume ratio is 0.06%, constant temperature stands 60min at 45 DEG C；
Film being put into the hexane solution for the pyromellitic trimethylsilyl chloride that mass percent is 0.8% again, constant temperature stands 10min at 20 DEG C,
Film after being activated；
3) intermediate SiO2Film surface is fixed：In advance by amination SiO2Ultrasonic disperse 9min in ethanol solution obtains SiO2Second
Alcoholic solution；Film after activation in step 2) is put into SiO2In ethanol solution, under the conditions of 100rpm, 25 DEG C of constant temperature oscillation 60min；
SiO was loaded by above-mentioned2Film taking-up be placed in 7min in 70 DEG C of baking ovens, obtain surface and fix amination SiO2The PVDF of layer is hollow
Tunica fibrosa；
4) cobaltous ferrocyanide cures：Amination SiO is fixed on surface in step 3)2The PVDF hollow-fibre membranes of layer are put into a concentration of
In the cobalt chloride solution of 0.5mol/L, under 25 DEG C of constant temperatures, 120rpm oscillations 2h；Then film is put into a concentration of 0.5mol/L
Sodium ferrocyanide solution in, under 25 DEG C of constant temperatures, 150rpm oscillation 4h；Ultra-pure water cleaning film again；
Repeat more than cobaltous ferrocyanide curing schedule 2 times；
Film finally is cleaned with ultra-pure water, epoxide-resin glue sealing in composite membrane both ends is cut after being dried at 40 DEG C and is prepared into ferrous iron
Cobaltous cyanide PVDF hollow-fibre membranes.
2. according to the preparation method described in claim 1, which is characterized in that amination silica described in the step 3)
A concentration of 0.05%-0.5% (mass/volume), grain size 300nm.
A kind of 3. cobaltous ferrocyanide PVDF hollow-fibre membranes, using preparation method described in claim 1, which is characterized in that institute
PVDF hollow-fibre membranes, fibre diameter 0.3cm are stated, membrane aperture is 0.1-1 μm.
4. the purposes of cobaltous ferrocyanide PVDF hollow-fibre membranes according to claim 3, which is characterized in that for efficiently removing
Caesium.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108538419A (en) * | 2018-01-25 | 2018-09-14 | 天津大学 | A kind of method that cobaltous ferrocyanide composite membrane-reverse osmosis membrane joint removes caesium in water |
| CN111111621A (en) * | 2018-11-01 | 2020-05-08 | 四川德天合盛环保科技有限公司 | Method for fixing copper ferrocyanide on PVDF hollow fiber membrane |
| CN112387131A (en) * | 2019-08-12 | 2021-02-23 | 中国科学院宁波材料技术与工程研究所 | Polymer microporous membrane, preparation method and application thereof |
| CN113952845A (en) * | 2021-11-05 | 2022-01-21 | 岭东核电有限公司 | Membrane filter material, preparation method thereof and application of membrane filter material in treating aerosol |
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| CN111111621A (en) * | 2018-11-01 | 2020-05-08 | 四川德天合盛环保科技有限公司 | Method for fixing copper ferrocyanide on PVDF hollow fiber membrane |
| CN112387131A (en) * | 2019-08-12 | 2021-02-23 | 中国科学院宁波材料技术与工程研究所 | Polymer microporous membrane, preparation method and application thereof |
| CN112387131B (en) * | 2019-08-12 | 2022-04-08 | 中国科学院宁波材料技术与工程研究所 | Polymer microporous membrane, preparation method and application thereof |
| CN113952845A (en) * | 2021-11-05 | 2022-01-21 | 岭东核电有限公司 | Membrane filter material, preparation method thereof and application of membrane filter material in treating aerosol |
| CN113952845B (en) * | 2021-11-05 | 2022-07-15 | 岭东核电有限公司 | Membrane filter material, preparation method thereof and application of membrane filter material in treating aerosol |
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