CN109569324A - A kind of hydrophilic antipollution ultrafiltration membrane of CND-PVDF and the preparation method and application thereof - Google Patents
A kind of hydrophilic antipollution ultrafiltration membrane of CND-PVDF and the preparation method and application thereof Download PDFInfo
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- CN109569324A CN109569324A CN201910000472.XA CN201910000472A CN109569324A CN 109569324 A CN109569324 A CN 109569324A CN 201910000472 A CN201910000472 A CN 201910000472A CN 109569324 A CN109569324 A CN 109569324A
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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
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
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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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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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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- Dispersion Chemistry (AREA)
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- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses hydrophilic antipollution ultrafiltration membranes of a kind of CND-PVDF and the preparation method and application thereof.The present invention, using through Carboxylation Nano diamond blending and modifying polyvinylidene fluoride material, is then coated with using DMAc as solvent and forms a film and obtain the hydrophilic antipollution ultrafiltration membrane of CND-PVDF by phase inversion.Nano diamond is used among ultrafiltration membrane modifying by the present invention for the first time, and the Nano diamond after Carboxylation has the hydrophilic functional groups such as a large amount of carboxyls, so that the hydrophily of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF greatly improves, to effectively improve the resistance tocrocking function of film, prolong the service life.
Description
Technical field
The invention belongs to the technical fields of polyvinylidene fluoride (PVDF) ultrafiltration membrane, and in particular to a kind of hydrophilic antipollution of CND-PVDF is super
Filter membrane and the preparation method and application thereof.
Background technique
Kynoar (PVDF) is widely used as surpassing because it is with good chemical stability, high temperature resistant, heat resistance
Filter membrane prepares material.But since PVDF itself has strong-hydrophobicity, pollutant is easy to be deposited on film surface and film is caused to block,
Filter efficiency is seriously affected, irreversible membrane pollution occurs, to reduce the service life of ultrafiltration membrane.
Blending and modifying is a kind of common and simple and easy method for improving PVDF ultrafiltration membrane hydrophilicity.Currently, oxidation
The inorganic nano-particles such as graphene (GO), carbon nanotube (MWCNTS) have been widely used in the hydrophilic modifying of PVDF seperation film
In.PVDF ultrafiltration membrane through hydrophilic modifying is often all improved largely in terms of hydrophilicity, antifouling property.But currently,
The technical barrier of inorganic nanoparticles blending and modifying pvdf membrane is that agglomeration easily occurs for nano particle, is difficult in casting film
It is evenly dispersed in liquid.And it need in terms of pvdf membrane antifouling property made from existing inorganic nano-particle blending and modifying into one
Step improves.
Nano diamond (ND) has good chemical stability and bio-compatible as a kind of novel carbon nano-particles
Property.ND how is used to be modified PVDF ultrafiltration membrane to obtain having superior dispersibility, hydrophily and the ultrafiltration of resistance tocrocking
Film has important research significance.
Summary of the invention
To solve the shortcomings and deficiencies of the prior art, the primary purpose of the present invention is that providing a kind of Carboxylation nanometer
The preparation method of the hydrophilic antipollution ultrafiltration membrane of diamond (CND)-PVDF is mainly molten with n,N-dimethylacetamide (DMAc)
Agent is then coated with using through Carboxylation Nano diamond blending and modifying Kynoar (PVDF) material and forms a film and pass through phase
Conversion method obtains modified CND-PVDF composite hyperfiltration membrane.
Innovation of the invention is that Nano diamond is used among ultrafiltration membrane modifying for the first time, and after Carboxylation
Nano diamond has the hydrophilic functional groups such as a large amount of carboxyls, so that the hydrophily of CND-PVDF composite hyperfiltration membrane greatly improves, from
And the resistance tocrocking function of film is effectively improved, prolong the service life.
Another object of the present invention is to provide the hydrophilic antipollution ultrafiltration of a kind of CND-PVDF that the above method is prepared
Film.
A further object of the present invention is to provide a kind of above-mentioned hydrophilic antipollution ultrafiltration membranes of CND-PVDF in water treatment field
Application.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of the hydrophilic antipollution ultrafiltration membrane of Carboxylation Nano diamond (CND)-PVDF, including following step
It is rapid:
(1) Nano diamond (ND) is Carboxylation, obtain Carboxylation Nano diamond (CND) powder；
(2) it disperses the CND powder that step (1) obtains in organic solvent, adds PVDF powder, casting is made after blending
Film liquid, then the hydrophilic antipollution ultrafiltration membrane of CND-PVDF is prepared in film.
The Carboxylation method of Nano diamond described in step (1) are as follows: Nano diamond is true under the conditions of 50~100 DEG C
Sky is 1~3 hour dry, then calcines 5~10 hours at 400~500 DEG C, to form the oxygen-containing hydrophilic officials such as carboxyl on the surface ND
It can group；More preferably: Nano diamond being dried in vacuo 2 hours under the conditions of 80 DEG C, is then calcined 7 hours at 450 DEG C.
The calcining carries out preferably in Muffle furnace.
Nano diamond described in step (1) is by external graphite shell or dangling bond and inside sp3Structural carbon core is constituted, and has been had
The crystal structure and the chemical stability of superelevation of beauty, hardness, biocompatibility and excellent wearability and heat conductivity are wide
It is general to be applied to the every field such as machinery, polishing, biology；But Nano diamond is due to living with biggish specific surface area and surface
Property, the agglomeration occurred between particle is more serious, and by the Carboxylation carboxyl etc. that can effectively increase its surface of Nano diamond
The content of oxygen-containing functional group so that its agglomeration in the medium be effectively relieved, while improving its hydrophily.
In casting solution described in step (2) mass content of organic solvent be 82~88%, CND powder account for CND powder with
The 0.1~1.5% of PVDF total powder quality.
Organic solvent described in step (2) is preferably N-Methyl pyrrolidone (NMP) and DMAC N,N' dimethyl acetamide
(DMAc)；More preferably DMAC N,N' dimethyl acetamide (DMAc).
Blending condition described in step (2) are as follows: stirred 10~15 hours at 30~50 DEG C, 300~400r/min；It is preferred that
To be stirred 12 hours at 40 DEG C, 350r/min.
Dispersion condition described in step (2) is preferred are as follows: first 300~400r/min is stirred 1~5 hour, then ultrasound 1~5 is small
When；More preferably: first 350r/min is stirred 3 hours, then ultrasound 3 hours.
Casting solution described in step (2) is also by following processing: standing and defoaming is handled 10~14 hours at 50~70 DEG C；
Standing and defoaming is handled 12 hours preferably at 60 DEG C.
Painting film base material described in step (2) is preferably glass plate.
A kind of hydrophilic antipollution ultrafiltration membrane of CND-PVDF that the above method is prepared.
The hydrophilic antipollution ultrafiltration membrane of the CND-PVDF with a thickness of 150~250 μm, preferably with a thickness of 200 μm.
The pure water flux of the hydrophilic antipollution ultrafiltration membrane of the CND-PVDF is 130~170L/m2H, flux after cleaning
Recovery rate is 77.2~83.3%, bovine serum albumin (BSA) rejection 93.7~96.3%.
Application of the hydrophilic antipollution ultrafiltration membrane of the CND-PVDF that the above method is prepared in water treatment field.
Compared with prior art, the present invention has the following advantages and beneficial effects:
1, for the present invention by Nano diamond through Carboxylation processing, CND has the spy that dispersion performance is excellent, hydrophily is splendid
Point overcomes Conventional nano material problem easy to reunite in organic media.
2, the Carboxylation Nano diamond amount that the present invention is added is few, and low in cost, modified effect is obvious.
3, the present invention is for the first time by Carboxylation Nano diamond in conjunction with PVDF ultrafiltration membrane, Carboxylation Nano diamond obtained
(CND) pure water flux of the hydrophilic antipollution ultrafiltration membrane of-PVDF is 130~170L/m2H, flux recovery rate is 77.2 after cleaning
~83.3%, bovine serum albumin (BSA) rejection 93.7~96.3%.
4, ultrafiltration membrane is made using phase inversion in the present invention, and technological operation used is simple and easy, and device therefor is ability
Domain conventional instrument, it is easy to operate, it is low in cost.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
The hydrophilicity of the hydrophilic antipollution ultrafiltration membrane of Carboxylation Nano diamond (CND)-PVDF prepared by the present invention passes through
Following methods evaluation:
Using the surface contact angle of the contact angle analyzer test hydrophilic antipollution ultrafiltration membrane of CND-PVDF, using contact angle point
Analyzer (Data Physics, OCA-15) tests ultra-pure deionized water in the contact angle of film surface, records contact angle values.
The permeance property of the hydrophilic antipollution ultrafiltration membrane of Carboxylation Nano diamond (CND)-PVDF prepared by the present invention and anti-
Pollutant performance is evaluated by the following method:
Pure water flux (J) is defined as: under certain operating condition (such as pressure), per membrane area is penetrated in the unit time
Water volume, unit L/m2H (is denoted as LMH).Specific formula for calculation is as follows:
Ultrafiltration membrane is as follows to the calculation formula of the rejection (R) of bovine serum albumin (BSA):
Wherein CPAnd CFThe concentration of protein respectively in permeate and feeding liquid, concentration use UV-vis spectroscopy light
Degree meter measures at wavelength 278nm.
Flux recovery rate (FRR) is generally used to the antifouling property of grading film, and specific formula for calculation is as follows:
Wherein Jw1And Jw2Respectively pure water flux and filtration protein liquid of the ultrafiltration membrane without pollution and clean after
Pure water flux.
Embodiment 1:
The preparation method of the hydrophilic antipollution ultrafiltration membrane of a kind of Carboxylation Nano diamond (CND)-PVDF, wherein casting obtained
Film liquid includes following mass percentage component: solvent (DMAC N,N' dimethyl acetamide) 85% and solute (Kynoar+carboxylic acid
Change Nano diamond) 15%, wherein Carboxylation Nano diamond accounts for the 0.5% of solute gross mass.
The following steps are included:
(1) Carboxylation Nano diamond (CND) is prepared: first by Nano diamond (ND) in 80 DEG C of vacuum oven
Vacuum drying 2 hours to remove the surface ND organic impurities；Then the ND after vacuum drying is placed in by Muffle furnace using heat treating process
Calcining 7 hours in (temperature is 450 DEG C), keep its Carboxylation, to form the oxygen-containing hydrophilic functional groups such as carboxyl on the surface ND, thus
To CND powder.
(2) it prepares the uniform mixed liquor of CND: dispersing organic solvent N, N- dimethyl second for the CND powder that step (1) obtains
In amide, re-ultrasonic dispersion 3 hours after magnetic agitation (350r/min) 3 hours, to obtain evenly dispersed CND-DMACMixing
Liquid.
(3) PVDF powder is blended with the CND-DMAc mixed liquor that step (2) obtains, then 40 DEG C of oil baths and 350r/min
Stirring 12 hours after be made casting solution, by casting solution at 60 DEG C standing and defoaming 12 hours, then apply film preparation on a glass
Obtain the hydrophilic antipollution ultrafiltration membrane of CND-PVDF with a thickness of 200 μm.
The test method of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF made from the present embodiment is as follows:
Pure water flux test: first ultrafiltration membrane is placed in ultrafiltration cup, precompressed 30min, then exists under 0.15MPa pressure
Deionized water is filtered under 0.1MPa pressure, every filtering 5min weighs the quality of filter liquor, until quality tends towards stability, record is last
Primary weighed filter liquor quality.Finally pure water flux can be calculated to obtain according to pure water flux calculation method.
The test of BSA rejection: first ultrafiltration membrane is placed in ultrafiltration cup, the precompressed 30min under 0.15MPa pressure, through precompressed
The BSA solution that the filted chroma under 0.1MPa pressure of film afterwards is 0.5g/L, is tested using ultraviolet-visible spectrophotometer and is penetrated
The concentration of protein in liquid and feeding liquid, then according to ultrafiltration membrane to the calculation formula of the rejection (R) of bovine serum albumin (BSA)
Calculate BSA rejection.
The test of flux recovery rate: film filters after being cleaned up after filtering BSA solution with clear water, then under 0.1MPa pressure
Deionized water, every filtering 5min weigh the quality of filter liquor, until quality tends towards stability, the weighed filter liquor of record last time
Quality.Finally flux recovery rate can be calculated to obtain according to flux recovery rate calculation method.
It is found after test, the contact angle of the hydrophilic antipollution ultrafiltration membrane of the CND-PVDF that the present embodiment is prepared is
68.1 °, effectively improve the hydrophilicity of traditional pvdf membrane；The pure water flux of the hydrophilic antipollution ultrafiltration membrane of the CND-PVDF is
130LMH, BSA rate and protein retention are 93.7%, and flux recovery rate is 77.2%；The hydrophilic antipollution ultrafiltration membrane of the CND-PVDF
Pure water flux, excellent hydrophily and preventing membrane pollution performance with higher effectively extend the service life of pvdf membrane.
Embodiment 2:
The preparation method of the hydrophilic antipollution ultrafiltration membrane of a kind of Carboxylation Nano diamond (CND)-PVDF, wherein casting obtained
Film liquid includes following mass percentage component: solvent (DMAC N,N' dimethyl acetamide) 85% and solute (Kynoar+carboxylic acid
Change Nano diamond) 15%, wherein Carboxylation Nano diamond accounts for the 1% of solute gross mass.
The following steps are included:
(1) Carboxylation Nano diamond (CND) is prepared: first by Nano diamond (ND) in 80 DEG C of vacuum oven
Vacuum drying 2 hours to remove the surface ND organic impurities；Then the ND after vacuum drying is placed in by Muffle furnace using heat treating process
Calcining 7 hours in (temperature is 450 DEG C), keep its Carboxylation, to form the oxygen-containing hydrophilic functional groups such as carboxyl on the surface ND, thus
To CND powder.
(2) it prepares the uniform mixed liquor of CND: dispersing organic solvent DMA for the CND powder that step (1) obtainsCIn, magnetic force
(350r/min) is stirred re-ultrasonic dispersion 3 hours after 3 hours, to obtain evenly dispersed CND-DMACMixed liquor.
(3) CND-DMA for obtaining PVDF powder and step (2)CMixed liquor is blended, then 40 DEG C of oil baths and 350r/min
Stirring 12 hours after be made casting solution, by casting solution at 60 DEG C standing and defoaming 12 hours, then apply film preparation on a glass
Obtain the hydrophilic antipollution ultrafiltration membrane of CND-PVDF with a thickness of 200 μm.
The test method of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF made from the present embodiment is the same as embodiment 1.
It is found after test, the contact angle of the hydrophilic antipollution ultrafiltration membrane of the CND-PVDF that the present embodiment is prepared is
65.3 °, effectively improve the hydrophilicity of traditional pvdf membrane；The pure water flux of the hydrophilic antipollution ultrafiltration membrane of the CND-PVDF is
170LMH, BSA rate and protein retention are 95.8%, and flux recovery rate is 83.3%；The hydrophilic antipollution ultrafiltration membrane of the CND-PVDF
Pure water flux, excellent hydrophily and preventing membrane pollution performance with higher effectively extend the service life of pvdf membrane.
Embodiment 3:
The preparation method of the hydrophilic antipollution ultrafiltration membrane of a kind of Carboxylation Nano diamond (CND)-PVDF, wherein casting obtained
Film liquid includes following mass percentage component: solvent (DMAC N,N' dimethyl acetamide) 85% and solute (Kynoar+carboxylic acid
Change Nano diamond) 15%, wherein Carboxylation Nano diamond accounts for the 1.5% of solute gross mass.
The following steps are included:
(1) Carboxylation Nano diamond (CND) is prepared: first by Nano diamond (ND) in 80 DEG C of vacuum oven
Vacuum drying 2 hours to remove the surface ND organic impurities；The ND after vacuum drying is then placed in by Muffle furnace using heat treating process
Calcining 7 hours in (temperature is 450 DEG C), keep its Carboxylation, to form the oxygen-containing hydrophilic functional groups such as carboxyl on the surface ND, thus
To CND powder.
(2) it prepares the uniform mixed liquor of CND: dispersing organic solvent DMA for the CND powder that step (1) obtainsCIn, magnetic force
(350r/min) is stirred re-ultrasonic dispersion 3 hours after 3 hours, to obtain evenly dispersed CND-DMACMixed liquor.
(3) CND-DMA for obtaining PVDF powder and step (2)CMixed liquor is blended, then 40 DEG C of oil baths and 350r/min
Stirring 12 hours after be made casting solution, by casting solution at 60 DEG C standing and defoaming 12 hours, then apply film preparation on a glass
Obtain the hydrophilic antipollution ultrafiltration membrane of CND-PVDF with a thickness of 200 μm.
The test method of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF made from the present embodiment is the same as embodiment 1.
It is found after test, the contact angle of the hydrophilic antipollution ultrafiltration membrane of the CND-PVDF that the present embodiment is prepared is
67.7 °, effectively improve the hydrophilicity of traditional pvdf membrane；The pure water flux of the hydrophilic antipollution ultrafiltration membrane of the CND-PVDF is
154LMH, BSA rate and protein retention are 96.3%, and flux recovery rate is 82.5%；The hydrophilic antipollution ultrafiltration membrane of the CND-PVDF
Pure water flux, excellent hydrophily and preventing membrane pollution performance with higher effectively extend the service life of pvdf membrane.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF, which comprises the steps of:
(1) Nano diamond is Carboxylation, obtain CND powder；
(2) it disperses the CND powder that step (1) obtains in organic solvent, adds PVDF powder, casting film is made after blending
Liquid, then the hydrophilic antipollution ultrafiltration membrane of CND-PVDF is prepared in film.
2. a kind of preparation method of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF according to claim 1, which is characterized in that step
Suddenly the mass content of organic solvent is that 82~88%, CND powder accounts for CND powder and PVDF powder is total in casting solution described in (2)
The 0.1~1.5% of quality.
3. a kind of preparation method of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF according to claim 1 or 2, feature exist
In blending condition described in step (2) are as follows: stirred 10~15 hours at 30~50 DEG C, 300~400r/min.
4. a kind of preparation method of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF according to claim 3, which is characterized in that step
Suddenly blending condition described in (2) are as follows: stirred 12 hours at 40 DEG C, 350r/min.
5. a kind of preparation method of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF according to claim 1 or 2, feature exist
In dispersion condition described in step (2) are as follows: first 300~400r/min is stirred 1~5 hour, then ultrasound 1~5 hour.
6. a kind of preparation method of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF according to claim 1 or 2, feature exist
In casting solution described in step (2) is also by following processing: standing and defoaming is handled 10~14 hours at 50~70 DEG C.
7. a kind of preparation method of the hydrophilic antipollution ultrafiltration membrane of CND-PVDF according to claim 3, which is characterized in that step
Suddenly the Carboxylation method of Nano diamond described in (1) are as follows: Nano diamond is dried in vacuo 1~3 under the conditions of 50~100 DEG C
Hour, then calcined 5~10 hours at 400~500 DEG C.
8. the hydrophilic antipollution ultrafiltration membrane of a kind of CND-PVDF that any one of claim 1~7 the method is prepared.
9. the hydrophilic antipollution ultrafiltration membrane of a kind of CND-PVDF according to claim 8, which is characterized in that the ultrafiltration membrane
With a thickness of 150~250 μm.
10. a kind of described in any item hydrophilic antipollution ultrafiltration membrane the answering in water treatment field of CND-PVDF of claim 8~9
With.
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Cited By (1)
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| CN117282283A (en) * | 2023-11-09 | 2023-12-26 | 常州大学 | Biomass blend membrane material and preparation method and application thereof |
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| CN117282283A (en) * | 2023-11-09 | 2023-12-26 | 常州大学 | Biomass blend membrane material and preparation method and application thereof |
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