CN108854591A - It is a kind of using tannic acid-titanium as composite nanometer filtering film of separating layer and preparation method thereof - Google Patents
It is a kind of using tannic acid-titanium as composite nanometer filtering film of separating layer and preparation method thereof Download PDFInfo
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- CN108854591A CN108854591A CN201810535831.7A CN201810535831A CN108854591A CN 108854591 A CN108854591 A CN 108854591A CN 201810535831 A CN201810535831 A CN 201810535831A CN 108854591 A CN108854591 A CN 108854591A
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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
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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
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
-
- 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
-
- 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
-
- 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
-
- 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
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
-
- 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
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
Abstract
The present invention provides a kind of using tannic acid-titanium as composite nanometer filtering film of separating layer and preparation method thereof, is related to technical field of membrane.It is a kind of using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, including：Basement membrane is immersed in the aqueous solution containing tannic acid；Metal titanium salt is added, in-situ preparation tannic acid-titanium crosslink functional skin layer, obtains composite nanometer filtering film on basement membrane.The method finally obtains the composite nanometer filtering film haveing excellent performance by depositing to form tannic acid-titanium separation surface layer in porous support membrane previous step.Preparation method is easy to operate, mild condition, low in cost, environmental-friendly.It is a kind of using tannic acid-titanium as the composite nanometer filtering film of separating layer, be made of the above method.The composite nanometer filtering film has outstanding separation function, antifouling property and antibacterial activity.
Description
Technical field
The present invention relates to a kind of technical field of membrane, and in particular to using tannic acid-titanium as the composite nanometer filtering film of separating layer and
Preparation method.
Background technique
The preparation of high-performance nanofiltration membrane and performance optimization are the cores of Nanofiltration Membrane Separation Technology.Composite algorithm is current using most
The preparation method of extensive most effective nanofiltration membrane.This method is usually to have nanoscale for compound one layer on porous support basement membrane
The ultra-thin surface layer in aperture.It can be made from a different material due to surface layer and supporting layer, table appropriate can be selected respectively
Layer and supporting layer, be allowed to selectivity, permeability, in terms of the performance that is optimized.Currently, interface
Polymerization is the most common method for preparing composite nanometer filtering film, it is anti-in the interface of water phase and oily phase by two kinds of activated monomers
It answers and forms ultra-thin fine and close separation surface layer on support basement membrane.But there are still some problems, for example, small point of used monomer
Son and organic solvent are harmful to environment and organism, in use vulnerable to pollution, and permeability of the membrane is smaller and operating pressure
Larger energy consumption is high.
Tannic acid is a kind of natural polyphenol derivative from plant tissue, cheap and environmental-friendly.Tannic acid
With functional groups such as catechol groups abundant, can have between a variety of substrates strongly adherent and with a variety of transition
Chelation occurs for metal ion.It is currently reported to utilize tannic acid and metal ion (Fe3+,Cu2+,Co2+,Ni+,Ag+)
Chelation forms simple tannic acid-chelate of metal ion surface functional layer.
Summary of the invention
A purpose of the present invention is that providing a kind of using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer.
By depositing to form tannic acid-titanium separation surface layer in porous support membrane previous step, final acquisition has excellent performance compound the method
Nanofiltration membrane.Preparation method is easy to operate, mild condition, low in cost, environmental-friendly.
Another object of the present invention is to provide a kind of using tannic acid-titanium as the composite nanometer filtering film of separating layer.This is compound to receive
Filter membrane includes porous support membrane and is covered on the epilamellar tannic acid-titanium functional skin layer.The tannic acid-titanium functional layer be with
Tannic acid-titanium ion chelate and titanium dioxide are the special networks structure of binary inorganic crosslinking point, and structure is uniformly and stable,
The composite nanometer filtering film has outstanding separation function, antifouling property and antibacterial activity simultaneously.
The present invention proposes a kind of using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, includes the following steps：
Basement membrane is immersed in the aqueous solution containing tannic acid by S1；
Metal titanium salt is added in S2, and in-situ preparation tannic acid-titanium crosslink functional skin layer, obtains composite nanometer filtering film on basement membrane.
The present invention proposes a kind of using tannic acid-titanium as the composite nanometer filtering film of separating layer, is made of above-mentioned preparation method.
It is provided by the invention to be by the beneficial effect of the composite nanometer filtering film of separating layer and preparation method thereof of tannic acid-titanium：
Compared with prior art, tannic acid and metal titanium salt can generate the tannin with strong adhesion in room temperature aqueous solution
Acid-titanium binary cross-linked network structure, to construct the composite nanometer filtering film of stable structure on porous basement membrane.Tannic acid has a large amount of
The functional groups such as catechol group can not only be attached on basement membrane, and can form tannic acid-titanium chelate with titanium salt.It uses
Metal titanium salt be different from other metallic salts, chelation can not only occur with tannic acid, and titanium dioxide can be formed.Cause
And tannic acid-titanium ion chelate and titanium dioxide can be obtained as the special net of binary inorganic crosslinking point by the technology
Network structure, building tannic acid-titanium function separate surface layer.The functional layer has very high hydrophily, and the parent of film surface can be improved
It is aqueous, enhance the permeability of water, is also beneficial to the antifouling property of film；Secondly, by adjust tannic acid/titanium salt feed ratio and
Sedimentation time, the surface layer of available densification, is conducive to the optimization of nanofiltration selectivity；The surface structure is stablized, between basement membrane
Also there is stronger adhesion, the performance of gained composite membrane is stablized.Whole preparation process mild condition, easy to operate, low in cost, ring
Border is friendly.Obtained Nano filtering composite membrane has very high rejection to dyestuff, such as methyl blue rejection is 96.8% and the Congo
Red rejection is 97.2%, the prospect with industrial production and business application.Particularly, which simultaneously has sodium chloride
Very high percent of pass (<12%), there is in terms of the processing of dyeing waste water and resource recycling biggish application potential.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The embodiment of the present invention is carried out specifically by the composite nanometer filtering film preparation method of separating layer of tannic acid-titanium below
Explanation.
The embodiment of the present invention propose it is a kind of using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, including with
Lower step：
Basement membrane is immersed in the aqueous solution containing tannic acid by S1；
Metal titanium salt is added in S2, and in-situ preparation tannic acid-titanium crosslink functional skin layer, obtains composite nanometer filtering film on basement membrane.
Further, in a preferred embodiment of the present invention, basement membrane is selected from polysulfone porous membrane, polyethersulfone porous membrane, polypropylene
One of nitrile perforated membrane, polyvinylidene fluoride porous film.The adhesion of the functional group of tannic acid makes that it is suitable for a variety of basement membranes.
Further, in a preferred embodiment of the present invention, in tannin aqueous acid, the concentration of tannic acid is 0.1~
50mmol/L。
Further, in a preferred embodiment of the present invention, metal titanium salt is selected from titanium tetrachloride, titanium trichloride, four fourth of metatitanic acid
Ester, tetraethyl titanate, tetraisopropyl titanate, four n-butyl titaniums, isopropyl titanate, isopropoxy titanium chloride, in isopropyl titanate
It is a kind of.
Further, in a preferred embodiment of the present invention, the molar ratio of tannic acid and titanium salt ratio is 50/1~1/30.
By regulating and controlling tannic acid/titanium salt molar ratio, the consistency of cross-linked network can be regulated and controled, improve the separation property of composite membrane
Energy.
Further, in a preferred embodiment of the present invention, in S2 step, sedimentation time is 0.1~48h.Further, it sinks
The product time is 1~15h, and reaction temperature is≤100 DEG C.Preferably, reaction temperature is room temperature~100 DEG C.It should be noted that room
Temperature is 15~25 DEG C.Suitable sedimentation time and reaction temperature, can enhance tannic acid-titanium surface layer compactness and stability.
The embodiment of the present invention also propose it is a kind of using tannic acid-titanium as the composite nanometer filtering film of separating layer, by above-mentioned preparation method
It is made.The composite nanometer filtering film includes porous support membrane and is covered on the epilamellar tannic acid-titanium functional skin layer.The tannin
Acid-titanium functional layer be using tannic acid-titanium ion chelate and titanium dioxide as the special networks structure of binary inorganic crosslinking point,
Structure is uniformly and stable, while the composite nanometer filtering film has outstanding separation function, antifouling property and antibacterial activity.
Feature and performance of the invention are described in further detail below in conjunction with specific embodiment.
Embodiment 1
Polysulfones basement membrane is directly immersed in containing in 10.5mmol/L tannin aqueous acid first；10.5mmol/L tetra- is added
Titanium chloride (i.e. tannic acid/titanium salt molar ratio is 1/1), reacts 9h, finally the in-situ deposition on polysulfones basement membrane at room temperature
Tannic acid-titanium functional skin layer is generated, composite nanometer filtering film is obtained.After deionized water rinsing for several times, composite membrane obtained is stored in
In water.
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, the difference is that, reaction time 1h.
Embodiment 3
Embodiment 3 is substantially the same manner as Example 1, the difference is that, reaction time 5h.
Embodiment 4
Embodiment 4 is substantially the same manner as Example 1, the difference is that, 1.05mmol/L titanium tetrachloride, i.e. tannin is added
Acid/titanium salt molar ratio is 10/1.
Comparative example 1
Polysulfones basement membrane
Test example 1
Composite membrane made from Examples 1 to 4 and comparative example 1 are saved in water, in the aqueous sodium sulfate of 5mmol/L
Liquid, operating pressure test its cutoff performance under the conditions of being 0.2MPa.The results are shown in Table 1.
Test example 2
Composite membrane made from Examples 1 to 4 and comparative example 1 are cleaned, drying, measures film table using contact angle tester
Face static contact angle, to analyze its hydrophily.The results are shown in Table 1.
Test example 3
Measure embodiment 1 made from composite nanometer filtering film to methyl blue and Congo red cutoff performance.It can be seen that compound
Film is up to 96.8% and 97.2% to methyl blue rejection and Congo red rejection respectively, filtering front and back significant effect.
The performance test table of 1 sample of table
Under 0.2MPa low operating pressure, the water flux of the composite membrane of embodiment 1 is 19L/m2H, sodium sulphate rejection are
70.3%.Referring to the performance of comparative example 1, tannic acid-titanium functional skin layer is constructed on basement membrane by step sedimentation success, it is compound
The separation function of film realization nanofiltration.The contact angle of film is only 39.1o, illustrates that surface hydrophilicity is good, be conducive to permeability of the membrane and
Resistance tocrocking.
Under identical feed ratio, with the extension of deposition reaction time, obtained tannic acid-titanium functional skin layer is more next
More finer and close, thicker, water flux gradually decreases, and sodium sulphate cutoff performance significantly improves, and film surface hydrophily is also improved.In phase
Under same sedimentation time, with the increase of tannic acid/titanium salt molar ratio, obtained tannic acid-titanium functional skin layer becomes
Must be finer and close, cutoff performance increases.Using suitable feed ratio and sedimentation time, it is capable of Effective Regulation composite nanometer filtering film
The performance of performance, product is more excellent.
To sum up, provided by the invention using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, by porous
Support membrane previous step deposits to form tannic acid-titanium separation surface layer, and preparation method is easy to operate, mild condition, low in cost, environment
Close friend finally obtains the composite nanometer filtering film haveing excellent performance.The composite nanometer filtering film has outstanding separation function, resistance tocrocking simultaneously
Energy and antibacterial activity.
Claims (10)
1. a kind of using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, which is characterized in that include the following steps：
Basement membrane is immersed in the aqueous solution of tannic acid by S1；
Metal titanium salt is added in S2, and in-situ deposition generates tannic acid-titanium crosslink functional skin layer on the basement membrane, obtains compound receive
Filter membrane.
2. according to claim 1 using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, feature exists
In the basement membrane is perforated membrane.
3. according to claim 1 or 2 using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, feature
It is, the basement membrane is in polysulfone porous membrane, polyethersulfone porous membrane, polyacrylonitrile porous membrane, polyvinylidene fluoride porous film
It is any.
4. according to claim 1 using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, feature exists
In in the tannin aqueous acid, the concentration of tannic acid is 0.1~50mmol/L.
5. according to claim 1 using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, feature exists
In the metal titanium salt is being selected from titanium tetrachloride, titanium trichloride, butyl titanate, tetraethyl titanate, tetraisopropyl titanate, four just
Any one of butanol titanium, isopropyl titanate, isopropoxy titanium chloride, isopropyl titanate.
6. according to claim 1 using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, feature exists
In the molar ratio of the tannic acid and the titanium salt is 50/1~1/30.
7. according to claim 1 using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, feature exists
In in S2 step, sedimentation time is 0.1~48h.
8. according to claim 7 using tannic acid-titanium as the preparation method of the composite nanometer filtering film of separating layer, feature exists
In, in S2 step, reaction temperature≤100 DEG C.
9. a kind of using tannic acid-titanium as the composite nanometer filtering film of separating layer, which is characterized in that as described in claim any one of 1-8
Preparation method be made.
10. according to claim 9 using tannic acid-titanium as the composite nanometer filtering film of separating layer, which is characterized in that the tannin
Acid-titanium separating layer is using tannic acid-titanium ion chelate and titanium dioxide as the network structure of binary inorganic crosslinking point.
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Cited By (6)
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| CN109847598A (en) * | 2019-01-28 | 2019-06-07 | 四川大学 | A kind of superhydrophilic self-cleaning water-oil separationg film and its preparation method and application |
| CN111672339A (en) * | 2020-04-30 | 2020-09-18 | 重庆理工大学 | Ceramic composite nanofiltration membrane for dye removal and preparation method thereof |
| CN112452159A (en) * | 2020-11-06 | 2021-03-09 | 浙江工业大学 | Preparation method of super-hydrophilic-underwater super-oleophobic microfiltration membrane |
| CN112690148A (en) * | 2021-01-15 | 2021-04-23 | 四川大学 | Greenhouse covering film material easy to clean, preparation method and cleaning method |
| CN114797508A (en) * | 2022-04-19 | 2022-07-29 | 南京信息工程大学 | Preparation method of tannic acid-Zr (IV) hybrid membrane for treating heavy metal-containing wastewater |
| CN115212728A (en) * | 2022-07-18 | 2022-10-21 | 同济大学 | Tannin-iron acid-resistant nanofiltration membrane with stable metal organic framework nano material and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109847598A (en) * | 2019-01-28 | 2019-06-07 | 四川大学 | A kind of superhydrophilic self-cleaning water-oil separationg film and its preparation method and application |
| CN111672339A (en) * | 2020-04-30 | 2020-09-18 | 重庆理工大学 | Ceramic composite nanofiltration membrane for dye removal and preparation method thereof |
| CN112452159A (en) * | 2020-11-06 | 2021-03-09 | 浙江工业大学 | Preparation method of super-hydrophilic-underwater super-oleophobic microfiltration membrane |
| CN112452159B (en) * | 2020-11-06 | 2022-05-24 | 浙江工业大学 | Preparation method of super-hydrophilic-underwater super-oleophobic microfiltration membrane |
| CN112690148A (en) * | 2021-01-15 | 2021-04-23 | 四川大学 | Greenhouse covering film material easy to clean, preparation method and cleaning method |
| CN114797508A (en) * | 2022-04-19 | 2022-07-29 | 南京信息工程大学 | Preparation method of tannic acid-Zr (IV) hybrid membrane for treating heavy metal-containing wastewater |
| CN114797508B (en) * | 2022-04-19 | 2023-01-17 | 南京信息工程大学 | Preparation method of tannin-Zr (IV) hybrid membrane for treating heavy metal-containing wastewater |
| CN115212728A (en) * | 2022-07-18 | 2022-10-21 | 同济大学 | Tannin-iron acid-resistant nanofiltration membrane with stable metal organic framework nano material and preparation method thereof |
| CN115212728B (en) * | 2022-07-18 | 2023-08-04 | 同济大学 | Tannic acid-iron acid-resistant nanofiltration membrane with stable metal organic frame nano material and preparation method thereof |
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