CN107138055A - A kind of preparation method and its usage of iron tannic acid compound modified PVDF membrane - Google Patents
A kind of preparation method and its usage of iron tannic acid compound modified PVDF membrane Download PDFInfo
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- CN107138055A CN107138055A CN201710404828.7A CN201710404828A CN107138055A CN 107138055 A CN107138055 A CN 107138055A CN 201710404828 A CN201710404828 A CN 201710404828A CN 107138055 A CN107138055 A CN 107138055A
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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
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/04—Breaking emulsions
- B01D17/045—Breaking emulsions with coalescers
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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
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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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- 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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Abstract
The invention provides a kind of preparation method and its usage of iron tannic acid compound modified PVDF membrane, preparation process is as follows：Configure iron salt solutions and tannic acid solution, adjust the pH of tannic acid solution, tannic acid solution after iron salt solutions and regulation pH is admixed together, obtain mixed liquor, then pvdf membrane is impregnated in the mixed liquor, dipping is finished, takes out drying, iron tannic acid compound modified PVDF membrane is made, Fe is designated asIIITA modified PVDF membranes.The present invention is simply impregnated by a step, self-assembly method, in pvdf membrane surface modification FeIIITA compounds, coarse structure is constructed by organic inorganic hybridization.The preparation method operating process is simple.
Description
Technical field
The present invention relates to a kind of preparation method and its usage of iron-tannic acid compound modified PVDF membrane, belong to environmental functional
Technical field of material.
Background technology
Naturally it is a marvellous world, its peculiar attribute and function, the enlightenment important to us and idea go to create
Valuable material and device.Biological surface can provide multi-functional interface, some super hydrophobic surfaces in them, with more than
150 ° of contact angle and roll angle is less than 10 °, such as lotus leaf.Lotus leaf is one less than 3 ° with contact angle higher than 160 ° with slide angle
Individual exemplary.This interesting phenomenon causes Barthlott and Nienhuis concern, and they observe the leaf of many plants
Son, and draw a conclusion:This unique attribute be due to mastoid process (5-9 mm dias) on the micro-meter scale of its rough surface and
Caused by epicutile wax collective effect.Further investigation revealed that, lotus leaf surface is the structure of micro-nano level.Cilium on lotus leaf
Shape nanometer (120 nanometers of diameter) structure also improves the papilary projection of micron size.This micro nano structure and low surface
Energy material is the basic reason for producing the special wetting property in surface.
The plant surface with ultra-hydrophobicity also has many kinds, such as taro leaf and water except lotus leaf in nature
Rice leaf etc., their surface all has the different-shape micro nano structure similar with lotus leaf surface, and such as Rice Leaf surface is covered with breast
Shape projection (about 5-8 mm dias), and these papillas are distributed along parallel blade edge direction ordered arrangement, so as to cause
Super hydrophobic surface, 157 ° of its contact angle and anisotropy are adhered to.Due to such surface texture, water droplet is along parallel blade edge
Direction is rolled.
It is also very common in Animal World super hydrophobic surface except plant world, for example, we are frequently seen the water in pond
Mian can freely walk in the water surface without lifting an eyebrow, without being immersed in the water.Researcher is studied water skipper leg, it was found that water
Mian legs surface has special micro nano structure, and there is micron bristle of many diameters less than 3 μm on surface, and these bristles are by same
Direction arrangement, helical form nano-scale trenches are contained on bristle, this micro-nano phase structure causes water skipper leg surface has super thin
Aqueous, its contact angle is up to 167.6 ° ± 4.4 °；Super hydrophobic surface makes it have very big buoyancy on the water surface, and research shows water
Mian one leg can prop up the weight of 15 times of own body weight on the water surface, and the load force of exactly this superelevation causes water skipper in water
Energy freedom of movement is without being immersed in the water on face.
Biological study shows that this unique structure is to realize a key factor of the special wetability in surface.Pass through
The special wetting property on animals and plants surface gives our enlightenment in nature, can simulate and prepare various bionic function water-oil separating materials
Material, realizes the purpose of water-oil separating.It has unique advantage and good application prospect in actual oil water separation process,
It is a kind of booming new function material.
In the past few decades, the fast development of super hydrophobic surface and derivative superoleophobic surface biomimetic under water, for development
Efficiently, automation and recyclable oil/water separation material provide a brand-new theory, i.e., without thorough with any external energy energy
Isolate oil water mixture in bottom.Relative to traditional separation method, the oil-water separation method of special wetability control is in separation speed
Degree and separative efficiency show two big advantages.Super hydrophobic surface as a kind of special wetability, be primarily referred to as when water droplet with
The contact angle of the surface of solids is more than 150 °, and roll angle is less than 10 °；Conversely, when water droplet or the contact angle of oil droplet and the surface of solids
Close to 0 °, then illustrate that surface has super hydrophilic or super-oleophilic.Super hydrophobic surface has the application of many, including self-cleaning window
Family/windshield, antifouling, drag reduction microfluidic device, and oil/water separation material.It is used as most widely used method Jiang et al.
It was found that the oil/water separation material of weight-driven.In 2004, further developed by Jiang et al..In 2011, from initial
Oil/water separation method, it is allowed to the prepared material of oil infiltration, to more advanced method, it is allowed to the material prepared by water penetration.From
From 2004, the Inspiration Sources of the oil/water separation material special wetability in the Nature.By 2013, according to RSC, ACS,
Wiley, Elsevier and Springer literature search, 2004-2009 account for total document about the document of water-oil separating
5%, account within 2010 total document 6%, account for total document in 2011 12%, account for total document in 2012 19%, and
Reach 58% within 2013, illustrate that the research and development in recent years about water-oil separating is rapid.In order to using its special wetability come
Water-oil mixture is separated, oil/water separation material generally has relative wetability to water and oil.In general, oil/water
Separation material has two kinds of preparation methods, i.e., under certain external environment condition, prepares super-hydrophobic/super-oleophilic material or superoleophobic/super
Water wetted material.Previous studies method normally tend to prepare the former (from mixture filter fuel-displaced).Wang etc. is sharp
It is nanocrystalline (iron, cobalt, nickel, copper and silver) with a series of transition metal of the modification of dip-coating and growth in situ method on water wetted material.
The former is popular in the research of early stage, and the latter occurred to 2011, superoleophobic/super hydrophilic due to obtaining in atmosphere
Surface difficulty is very big.Therefore, scientists dexterously devise under water superoleophobic/ultra-hydrophilic surface come realize oil/water separate.
The present invention is using tannic acid (TA) chelation between catechol and metal ion, by simply impregnating, self assembly
Method is modified to pvdf membrane surface, by iron-tannic acid particulate load to pvdf membrane surface, is prepared super hydrophilic-super thin under water
Oily pvdf membrane.
The content of the invention
The present invention relates to the preparation method and its use that a kind of iron-tannic acid compound is modified PVDF (Kynoar) film
On the way, with tannic acid and ferric nitrate (Fe (NO3)·9H2O) it is raw material ,-tannic acid the PVDF that taps a blast furnace is prepared by hybrid inorganic-organic
Film, iron-tannic acid pvdf membrane prepared by the method shows excellent super hydrophilic-superoleophobic property under water, can not only be mixed to profit
Compound is effectively separated, moreover it is possible to handle oil hydrosol.
The present invention is simply impregnated, self-assembly method is in pvdf membrane surface modification Fe using stainless (steel) wire as substrate by a stepIII-
TA compounds, are successfully prepared FeIII- TA modified PVDF membranes, and use it for the separation of oil water mixture and oil hydrosol.
The technical solution adopted by the present invention is：
A kind of preparation method of iron-tannic acid compound modified PVDF membrane, step is as follows：
Iron salt solutions and tannic acid solution are configured, the pH of tannic acid solution is adjusted, by the list after iron salt solutions and regulation pH
Peaceful acid solution is admixed together, obtains mixed liquor, then impregnates pvdf membrane in the mixed liquor, dipping is finished, and takes out and dries
It is dry, iron-tannic acid compound modified PVDF membrane is made, Fe is designated asIII- TA modified PVDF membranes.
The concentration of the iron salt solutions is 3.0~15mg/mL.
The concentration of the tannic acid solution is 3.0~15mg/mL.
The tannic acid solution pH is 3-11, hydrochloric acid and 0.1mol/L ammoniacal liquor that it is 0.1mol/L with concentration that the pH, which is,
Solution regulation.
The volume ratio of the iron salt solutions and the tannic acid solution after regulation pH is 1：5~5：1.
The molysite is Fe (NO3)·9H2O。
The dip time is 0.5~5.0min.
The drying temperature is 40~60 DEG C, and the time is 2~5min.
The iron-tannic acid compound modified PVDF membrane is used for oil water mixture and oil hydrosol is separated.
Beneficial effect：
(1) present invention simply impregnated by a step, self-assembly method, in pvdf membrane surface modification FeIII- TA compounds, pass through
Hybrid inorganic-organic constructs coarse structure.The preparation method operating process is simple.
(2) Fe is utilizedIIIWhen-TA modified PVDF membranes are separated to oil water mixture and oil hydrosol, with good point
From effect, and a variety of oil water mixtures and oil hydrosol can be separated.
(3)FeIII- TA modified PVDF membranes stability preferably, and can be recycled for multiple times, and be 1 to 100mL volume ratios：1
Oil water mixture separate 15 times and to 100mL profits volume ratio be 1：After 99 oil hydrosol is separated 10 times, still keep good
Good oil-water separation.
Brief description of the drawings
Fig. 1 is pure pvdf membrane (a) and the SEM figures of the modified PVDF membrane (b) in embodiment 2.
Fig. 2 is the angle of the droplets contact under water schematic diagram of embodiment 2.
Embodiment
In order to illustrate technical scheme and technical purpose, below in conjunction with the accompanying drawings and specific embodiment is done to the present invention
It is further to introduce.
Embodiment 1：
Step 1：
Configure certain density Fe (NO3)·9H2O and TA solution, the hydrochloric acid and 0.1mol/L for being 0.1mol/L with concentration
Ammonia spirit adjusts the pH=3 of TA solution, and the mixed cumulative volume of two solution is 30mL, Fe (NO3)·9H2O concentration is 3.0mg/
ML, TA concentration are 3.0mg/mL；Pvdf membrane is impregnated in mixed solution, after reaction 0.5min, is put into 40 DEG C of baking oven and does
Dry 2min；Obtain 3FeIII- 3TA-1 modified PVDF membranes.
Step 2：
By obtained 3FeIII- 3TA-1 modified PVDF membranes are fixed to homemade oily-water seperating equipment, will with a small amount of distilled water
Retinal surface is soaked, and is then 1 by 100mL volume ratios：1 hexamethylene and the mixed solution of water are poured into the device put up.For
More accurately determine the water-oil separating efficiency of composite membrane, sample is divided into 3 parts, and each sample test 3 times.Entirely tested
Journey is carried out under 0.01kPa air pressure conditions.Water-oil separating efficiency is calculated as follows：
Wherein R is separative efficiency, M0And MpThe weight of oil before and after respectively separating.
Test result indicates that 3FeIII- 3TA-1 modified PVDF membranes have excellent water-oil separating performance, and its separative efficiency reaches
To 98.3%.
Embodiment 2：
Step 1：
Configure certain density Fe (NO3)·9H2O and TA solution, the hydrochloric acid and 0.1mol/L for being 0.1mol/L with concentration
Ammonia spirit adjusts the pH=3 of TA solution, and the mixed cumulative volume of two solution is 30mL, Fe (NO3)·9H2O concentration is 3.0mg/
ML, TA concentration are 9.0mg/mL；Pvdf membrane is impregnated in mixed solution, after reaction 0.5min, is put into 40 DEG C of baking oven and does
Dry 2min；Obtain 3FeIII- 9TA-3 modified PVDF membranes.
Step 2：
By obtained 3FeIII- 9TA-3 modified PVDF membranes are fixed to homemade oily-water seperating equipment, are walked according in embodiment 1
Rapid 2 operation carries out water-oil separating experiment, test result indicates that water-oil separating efficiency is 99.6%.
Fig. 1 is that pure pvdf membrane (a) and the SEM of the modified PVDF membrane (b) in embodiment 2 scheme, as can be seen from the figure FeIII-
TA particles successfully load to pvdf membrane surface.
Fig. 2 is the angle of the droplets contact under water schematic diagram of embodiment 2, FeIIIThe contact angle of-TA modified PVDF membranes reaches
151°。
Embodiment 3：
Step 1：
Configure certain density Fe (NO3)·9H2O and TA solution, the hydrochloric acid and 0.1mol/L for being 0.1mol/L with concentration
Ammonia spirit adjusts the pH=3 of TA solution, and the mixed cumulative volume of two solution is 30mL, Fe (NO3)·9H2O concentration is 3.0mg/
ML, TA concentration are 15mg/mL；Pvdf membrane is impregnated in mixed solution, after reaction 0.5min, is put into 40 DEG C of baking oven and dries
2min；Obtain 3FeIII- 15TA-5 modified PVDF membranes.
Step 2：
By obtained 3FeIII- 15TA-5 modified PVDF membranes are fixed to homemade oily-water seperating equipment, according in embodiment 1
The operation of step 2 carries out water-oil separating experiment, test result indicates that water-oil separating efficiency is 99.0%.
Embodiment 4：
Step 1：
Configure certain density Fe (NO3)·9H2O and TA solution, the hydrochloric acid and 0.1mol/L for being 0.1mol/L with concentration
Ammonia spirit adjusts the pH=7 of TA solution, and the mixed cumulative volume of two solution is 50mL, Fe (NO3)9H2O concentration is 5.0mg/
ML, TA concentration are 10mg/mL；Pvdf membrane is impregnated in mixed solution, after reaction 3min, is put into 50 DEG C of baking oven and dries
4min；Obtain 5FeIII- 10TA-2 modified PVDF membranes.
Step 2：
By obtained 5FeIII- 10TA-2 modified PVDF membranes are fixed to homemade oily-water seperating equipment, according in embodiment 1
The operation of step 2 carries out water-oil separating experiment, is 1 with volume ratio：99 hexamethylene-water oil hydrosol substitutes oil water mixture,
Test result indicates that oil hydrosol successfully can be separated into You Heshui by modified pvdf membrane.
Embodiment 5：
Step 1：
Configure certain density Fe (NO3)·9H2O and TA solution, the hydrochloric acid and 0.1mol/L for being 0.1mol/L with concentration
Ammonia spirit adjusts the pH=7 of TA solution, and the mixed cumulative volume of two solution is 50mL, Fe (NO3)9H2O concentration is 15.0mg/
ML, TA concentration are 5mg/mL；Pvdf membrane is impregnated in mixed solution, after reaction 3min, is put into 50 DEG C of baking oven and dries
4min；Obtain 15FeIII- 5TA-3 modified PVDF membranes.
Step 2：
By obtained 15FeIII- 5TA-3 modified PVDF membranes are fixed to homemade oily-water seperating equipment, according in embodiment 1
The operation of step 2 carries out water-oil separating experiment, test result indicates that water-oil separating efficiency is 98.8%.
Embodiment 6：
Step 1：
Configure certain density Fe (NO3)·9H2O and TA solution, the hydrochloric acid and 0.1mol/L for being 0.1mol/L with concentration
Ammonia spirit adjusts the pH=9 of TA solution, and the mixed cumulative volume of two solution is 50mL, Fe (NO3)9H2O concentration is 10.0mg/
ML, TA concentration are 5mg/mL；Pvdf membrane is impregnated in mixed solution, after reaction 5min, is put into 50 DEG C of baking oven and dries
4min；Obtain 10FeIII- 5TA-2 modified PVDF membranes.
Step 2：
By obtained 10FeIII- 5TA-2 modified PVDF membranes are fixed to homemade oily-water seperating equipment, according in embodiment 1
The operation of step 2 carries out water-oil separating experiment, test result indicates that water-oil separating efficiency is 98.5%.
Embodiment 7：
Step 1：
Configure certain density Fe (NO3)·9H2O and TA solution, the hydrochloric acid and 0.1mol/L for being 0.1mol/L with concentration
Ammonia spirit adjusts the pH=11 of TA solution, and the mixed cumulative volume of two solution is 60mL, Fe (NO3)9H2O concentration is 15.0mg/
ML, TA concentration are 3mg/mL；Pvdf membrane is impregnated in mixed solution, after reaction 5min, is put into 60 DEG C of baking oven and dries
5min；Obtain 15FeIII- 3TA-5 modified PVDF membranes.
Step 2：
By obtained 15FeIII- 3TA-5 modified PVDF membranes are fixed to homemade oily-water seperating equipment, according in embodiment 1
The operation of step 2 carries out water-oil separating experiment, test result indicates that water-oil separating efficiency is 98.2%.
Claims (9)
1. the preparation method of a kind of iron-tannic acid compound modified PVDF membrane, it is characterised in that step is as follows：
Iron salt solutions and tannic acid solution are configured, the pH of tannic acid solution is adjusted, by the tannic acid after iron salt solutions and regulation pH
Solution is admixed together, obtains mixed liquor, then impregnates pvdf membrane in the mixed liquor, dipping is finished, and takes out drying, system
Obtain iron-tannic acid compound modified PVDF membrane.
2. a kind of preparation method of iron according to claim 1-tannic acid compound modified PVDF membrane, it is characterised in that
The concentration of the iron salt solutions is 3.0~15mg/mL.
3. a kind of preparation method of iron according to claim 1-tannic acid compound modified PVDF membrane, it is characterised in that
The concentration of the tannic acid solution is 3.0~15mg/mL.
4. a kind of preparation method of iron according to claim 1-tannic acid compound modified PVDF membrane, it is characterised in that
The tannic acid solution pH is 3-11.
5. a kind of preparation method of iron according to claim 1-tannic acid compound modified PVDF membrane, it is characterised in that
The volume ratio of the iron salt solutions and the tannic acid solution after regulation pH is 1：5~5：1.
6. a kind of preparation method of iron according to claim 1-tannic acid compound modified PVDF membrane, it is characterised in that
The molysite is Fe (NO3)·9H2O。
7. a kind of preparation method of iron according to claim 1-tannic acid compound modified PVDF membrane, it is characterised in that
The dip time is 0.5~5.0min.
8. a kind of preparation method of iron according to claim 1-tannic acid compound modified PVDF membrane, it is characterised in that
The drying temperature is 40~60 DEG C, and the time is 2~5min.
9. iron-tannic acid compound modified PVDF membrane prepared by the method described in claim 1~8 any one is mixed for profit
Compound and the purposes of oil hydrosol separation.
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| CN109233371A (en) * | 2018-08-09 | 2019-01-18 | 深圳市天得环境科技有限公司 | Nano self-cleaning coating liquid, automatically cleaning product and preparation method thereof |
| CN109675444A (en) * | 2019-02-11 | 2019-04-26 | 刘云晖 | A kind of preparation method of the underwater superoleophobic oil-water separation mesh film based on tannic acid modification |
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