CN106750474A - A kind of preparation method of monovalent anion selective diffusion barrier - Google Patents
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
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- C—CHEMISTRY; METALLURGY
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- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
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Abstract
This patent is related to a kind of preparation method of monovalent anion selective diffusion barrier.It is by BPPO（Brominated polyphenylether）Coating knifing, obtains the anion-exchange membrane with BPPO as substrate after solvent portions are quaternized（QPPO）, then using the means of electro-deposition by polyethyleneimine（PEI）Thus aqueous solution deposition just can obtain an amberplex that there is monovalent anion to select performance to the surface of the film（PEI‑ QPPO）.Here the chemism of remaining in QPPO bromomethyl higher is mainly make use of to be reacted with the various types of amine in PEI so that PEI covalence grafts are to QPPO surfaces, while also causing that modified layer becomes finer and close using the means of electro-deposition.Sieving actoion of the alkalescent reduction of PEI to bivalent ions affinity and electro-deposition compacted zone is make use of, and then obtains the monovalent anion selective diffusion barrier with excellent properties and stabilization.
Description
Technical field
The invention belongs to separate technical field of membrane, and in particular to a kind of simple and effective monovalent anion selectively divides
From the preparation method of film.
Background technology
Water is used as Source of life, and importance is self-evident.But current, with the increasingly depleted of global resources, water resource is short
Scarce problem is stood in the breach, and becomes increasingly serious, and the pollution of water resource similarly aggravates, and this is undoubtedly and makes the matter worse.Drink
Rare with water is also global problem, at present in water treatment field, has been formd including micro-filtration, ultrafiltration, nanofiltration, counter-infiltration
With unique water treatment system of the method such as electrodialysis.Wherein, electrodialytic technique because its Water Sproading rate is high, service life of equipment is long and
Operating cost is low, simultaneously for the separation between non-same sex ion, even same sex ion with not replaceable huge advantage
Receive much concern.Electrodialysis is the selective penetrated property energy to ion using amberplex, under the promotion of applying direct current electric field power,
So that ion directional migration, so as to reach a special kind of skill of the separation, purification and concentration of electrolyte solution.
Current electrodialysis has been widely used in sewage disposal as a kind of membrane separation technique, and food processing and medicine are strong
The aspects such as health.Although electrodialytic technique possesses obvious application advantage, increasing, chemical industry life with drinking water treatment difficulty
The progress of product and the raising of aquatic products class requirement, people are consequently increased to electrodialytic expectation.Accordingly, for having
The demand of the amberplex of special separating power also grows to even greater heights, for example：During electrodialysis Utilization of Seawater by Solar, just
Wishing can be with Selective Separation sulfate ion so as to avoid the generation of fouling.In underground drinking water is processed, it is also desirable to can be with
The monovalent ion such as nitrate anion that preferably removal is harmful to, fluorine ion etc. are so as to guarantee drinking water safety of increasing water quality.According to the world
Health organization specifies that the concentration of the fluorine ion in drinking water may not exceed 1.5x10-3kg/m3, the concentration of nitrate can not in water
More than 5x10-2kg/m3, the concentration of nitrite may not exceed 3x10-3kg/m3.It can thus be appreciated that research has Selective Separation
The anion-exchange membrane of one multivalent ion is necessary, and its research also certainly will bring benefit for production and living, also more favourable money
The more preferable development and utilization in source.
Journal of Membrane Science （2015,490,301-310）Propose one kind and utilize poly-dopamine
The method of modified business cavity block is prepared a kind of with monovalent anion selective diffusion barrier.Because dopamine is in air ambient
Poly-dopamine will be converted into, poly-dopamine has absorption adhesive attraction well and the property with both sexes is so can make
The surface for obtaining business cavity block has one layer of negative electrical charge.By SO4 2-/Cl-The electrodialysis experiment of system, it is possible to achieve preferable one, many
Valency ion selectivity is separated.But the method is faced with modified layer and comes off, and the more expensive problem of raw material, be not suitable for the industry in future
Change and promote.
Electrochimica Acta （2015,174,1113-1121）A kind of covalent modified strategy is proposed, is led to
The chemical reaction for crossing diazol introduces carboxyl on the surface of business cavity block, and penta is recycled after introducing PEI using amidation process
The crosslinking of dialdehyde introduces multilayer PEI on the surface of film.Equally in SO4 2-/Cl-The electrodialysis experiment of system, can obtain preferably
First, multivalent ion Selective Separation.Although the problem operation that comes off this method avoid modified layer is complex also to have used
The glutaraldehyde of poison there is also problem in this approach as crosslinking agent.
Journal of Membrane Science (2016,520,262-271) proposes a kind of electro-deposition layer by layer
The method of modified commercial anionic exchange membrane obtains the anion-exchange membrane with Monovalent selectivity.Synthesis first carries positive charge
Quaternized shitosan, used as polycation electrolyte, this negatively charged material of kayexalate is used as poly- the moon
Ionic electrolytes.Afterwards using the means of electro-deposition, electrolyte and positive electrolysis are born in the surface layer electro-deposition of business cavity block
Matter.In SO4 2-/Cl-The electrodialysis experiment of system, can obtain preferable one, multivalent ion Selective Separation, wherein electro-deposition 9
Chlorion reaches 2.9. and although obtains the cavity block with Monovalent selectivity with respect to the selectivity of sulfate ion during layer, but need
Will electro-deposition layer by layer means complex operation and also also need to synthesis needed for material, it is most important that modified layer relies solely on quiet
Electro Sorb cannot overcome the problem of less stable, be unfavorable for using for a long time.
Chinese patent（CN 104815568A）Proposition is a kind of to use the aryl primary amine with functional group to match somebody with somebody in being dissolved in hydrochloric acid
Certain density solution is made, and to fully being reacted after adding natrium nitrosum in above-mentioned solution system, primary amine groups is changed into diazonium
Base；Then, conventional anion exchange membrane to be modified is placed in one, and adds appropriate reducing agent and reduce diazo to obtain virtue
Base free radical.Then, realize above-mentioned objective function group at film surface the attack on film surface by aryl radical
Covalent bond is fixed, and obtains final product the anion-exchange membrane with unit price selection separation function.Although the method is there is no concern that modified layer
Coming off, but equally exist complex operation will prepare too many solution and the also use of noxious material, be not suitable for futurity industry.
The content of the invention
For the above-mentioned problems in the prior art, it is an object of the invention to provide a kind of simple and effective single
The preparation method of valency anion selectivity seperation film.
The preparation method of described a kind of monovalent anion selective diffusion barrier, it is characterised in that using partial quaternization
The bromomethyl of remaining reacts with the amine in the PEI using electro-deposition means in QPPO anion-exchange membranes so that QPPO
PEI on the film surface covalence graft of anion-exchange membrane, obtains with monovalence, multivalent anions selective diffusion barrier.
The preparation method of described a kind of monovalent anion selective diffusion barrier, it is characterised in that its preparation method is included such as
Lower step：
1）Prepare BPPO solution：To adding 1-Methyl-2-Pyrrolidone to mix in BPPO solids, BPPO solid dissolvings are obtained completely
BPPO solution；
2）By step 1）In BPPO solution add trimethylamine ethanol solution, stirring reaction 1-10h, obtains part quaternary ammonium at room temperature
The QPPO solution of change；
3）By step 2）In QPPO solution be coated on film forming on glass plate, be placed on panel heater and dry, obtain QPPO cloudy
Amberplex；
4）By step 3）In QPPO anion-exchange membranes carry out electro-deposition PEI experiments, in QPPO anion-exchange membranes remaining
Bromomethyl is reacted with the amine in the PEI using electro-deposition means, and PEI chemical bonds are bonded in into QPPO surfaces, obtains unit price
Anion selectivity seperation film PEI- QPPO.
A kind of preparation method of described monovalent anion selective diffusion barrier, it is characterised in that step 1）In BPPO claim
Taken amount is 1-10g, and solvent NMP consumptions are 1-30g, and the BPPO solution concentrations for finally obtaining are 3-90%.
A kind of preparation method of described monovalent anion selective diffusion barrier, it is characterised in that step 2）Middle trimethylamine second
Alcoholic solution concentration is 4.27mol/L, and the volumetric usage of trimethylamine ethanol solution is the 0.2-1ml/g of BPPO mass.
A kind of preparation method of described monovalent anion selective diffusion barrier, it is characterised in that step 2）In reaction when
Between be 3-8h, quaternization degree be less than 100%.
A kind of preparation method of described monovalent anion selective diffusion barrier, it is characterised in that step 3）In QPPO it is molten
The scraper thickness that liquid coating filmform is used is 550-650 μm, and panel heater temperature is 55-65 DEG C, and the heat time is 7-9h, excellent
It is 600 μm to select scraper thickness, and panel heater temperature is 60 DEG C, and the heat time is 8h.
A kind of preparation method of described monovalent anion selective diffusion barrier, it is characterised in that step 4）In electro-deposition
The concentration of PEI is the aqueous solution of 1-20g/L, and electrodeposition time is 0.5-2h, and current density is 1-20mA/cm2, temperature is room
Temperature.
A kind of preparation method of described monovalent anion selective diffusion barrier, it is characterised in that step 4）In chemical bond
Bonded process is the mixed solution of the NMP/ water in PEI, and the mass content of NMP is less than 50%.
A kind of preparation method of described monovalent anion selective diffusion barrier, it is characterised in that step 4）In PEI point
In 1000-800000, the concentration of PEI is 1-20g/L to son amount, and the bromomethyl content of remaining is less than 75%.
A kind of preparation method of described monovalent anion selective diffusion barrier, it is characterised in that monovalent anion selectivity
Seperation film PEI- QPPO are the ionic membrane that single or double electro-deposition is modified.
BPPO, QPPO and polyethyleneimine（PEI）Structural formula difference is as follows：
BPPO structural formulas,
QPPO structural formulas；
。
By using above-mentioned technology, compared with prior art, beneficial effects of the present invention are as follows：
The present invention just can reach the one, purpose of multivalent anions Selective Separation by using simple electro-deposition means, together
When by the membrane modifying of strong chemical bond bonded acquisition layer and basement membrane, the stability of modified layer is guaranteed, while the choosing
For industrializing very big directive significance from now on, its preparation process is simple, simply certain hour for the preparation of the cavity block of selecting property
Electro-deposition, avoid the complex processes such as LBL self-assembly and the asking of coming off of modified layer using Electrostatic Absorption Modified Membrane surface
Topic, with industrialized potential.
Brief description of the drawings
Fig. 1 is the preparation process schematic diagram of monovalent anion selective diffusion barrier of the present invention；
Fig. 2 is the process schematic of partial quaternization QPPO film electrodepositions PEI of the present invention；
Fig. 3 a are QPPO films surface electron microscope；
Fig. 3 a1 are QPPO film section electron microscopes；
Fig. 3 b are PEI- QPPO films surface electron microscope；
Fig. 3 b1 are PEI- QPPO film section electron microscopes；
Fig. 4 is Monovalent selectivity electrodialysis experimentation schematic diagram；
Fig. 5 is the relative sulfate radical of chlorion of former film and Modified Membrane in diluting compartment when the Monovalent selectivity electrodialysis of 1h is tested
The selectivity and sulfate ion slip figure of ion, A1 in figure：QPPO films；EA1：The modified PEI- QPPO of one side electro-deposition
Film；EA2:The modified PEI- QPPO films of two-sided electro-deposition；
Fig. 6 a are tested for Monovalent selectivity electrodialysis, and unmodified QPPO films are in diluting compartment intermediate ion concentration changes with time figure；
Fig. 6 b are tested for Monovalent selectivity electrodialysis, and the modified PEI- QPPO films of two-sided electro-deposition are in diluting compartment intermediate ion concentration
Change over time figure.
Specific embodiment
The preferred embodiments of the present invention are described in detail below, so that present disclosure feature is easy to by this area
In researcher understand, so as to make more full and accurate defining to protection scope of the present invention.
Embodiment 1
The BPPO solids that the bromination degree of 5g is 57.8% are added in small beaker, the nmp solution of 20g is then slowly added into.Magnetic force
Stirring until BPPO be completely dissolved amber transparent is molten, then in the solution add 1.5ml trimethylamine ethanol solution, continue
QPPO solution is obtained after stirring reaction 8h.One piece of cleaned glass plate is taken, a certain amount of QPPO solution is toppled on its surface, use thickness
For 600 μm of scrapers scraped solution rapidly, the glass plate is put on panel heater afterwards, heter temperature is set as 60
DEG C, the heat time is set as the QPPO films that 8h, heating are removed on glass plate after terminating, and dries stand-by.
As depicted in figs. 1 and 2, the side of the QPPO films of preparation is carried out into electro-deposition PEI experiments, wherein PEI solubility is
10g/L, effective electro-deposition area of film is 19.625cm2, electrodeposition time is 1h, and current density is 10mA/cm2.Electro-deposition knot
The film is taken out after beam, the surface of film is cleaned with deionized water and is dried.Thus a monovalent anion selectivity can just be obtained
Seperation film.The presence of modified layer is can clearly be seen that from the section of Fig. 3 a, Fig. 3 a1, the electron microscope of Fig. 3 b and Fig. 3 b1.
The film that this one side electro-deposition is modified carries out dianion selectivity electrodialysis and tests according to Fig. 4：Experiment with
Cl-/SO4 2- Be test system, and initial concentration is all 0.05mol/L, wherein the solution for taking diluting compartment after one hour utilize from
Sub- chromatography Cl-And SO4 2- Concentration, and calculate Cl-With respect to SO4 2- Selectivity is through value and SO4 2- Slip.In order to
Compare modified effect change, also ibid do the divalent selectivity electrodialysis experiment of unmodified QPPO films.Result from
Fig. 5 can be seen that the modified Cl of one side electro-deposition-With respect to SO4 2- Selectivity increases through the more unmodified QPPO films of value from 0.79
To 4.19, SO4 2- Slip drops to 26.4% from 39.6%.
Embodiment 2
The ethanol solution addition of the trimethylamine in examples detailed above 1 is changed to 1ml, other steps are constant.
Embodiment 3
The ethanol solution addition of the trimethylamine in examples detailed above 1 is changed to 2ml, other steps are constant.
Embodiment 4
The continuation reaction time of the addition trimethylamine ethanol solution in examples detailed above 1 is changed to 1h, other steps are constant.
Embodiment 5
The continuation reaction time of the addition trimethylamine ethanol solution in examples detailed above 1 is changed to 10h, other steps are constant.
Embodiment 6
The concentration of the electro-deposition PEI in examples detailed above 1 is changed to 1g/L, other steps are constant.
Embodiment 7
The concentration of the electro-deposition PEI in examples detailed above 1 is changed to 10g/L, other steps are constant.
Embodiment 8
Electrodeposition time in examples detailed above 1 is changed to 0.5h, other steps are constant.
Embodiment 9
Electrodeposition time in examples detailed above 1 is changed to 2h, other steps are constant.
Embodiment 10
Current density during by electro-deposition in examples detailed above 1 is changed to 1mA/cm2, other steps are constant.
Embodiment 11
Current density during by electro-deposition in examples detailed above 1 is changed to 20mA/cm2, other steps are constant.
Embodiment 12
Electro-deposition one side in examples detailed above 1 is changed into all electro-deposition of two faces to be modified, other steps are constant.
The modified QPPO films of two-sided electro-deposition, electron microscope is similar with one side as shown in Figure 3.
The film that this two-sided electro-deposition is modified carries out dianion selectivity electrodialysis and tests according to Fig. 4.Experiment with
Cl-/SO4 2- Be test system, and initial concentration is all 0.05mol/L, wherein the solution for taking diluting compartment after one hour utilize from
Sub- chromatography Cl-And SO4 2- Concentration, and calculate Cl-With respect to SO4 2- Selectivity is through value and SO4 2- Slip.In order to
Compare modified effect change, also ibid do unmodified QPPO films and the modified QPPO films of one side a divalence
Selective electrodialysis experiment.The result modified Cl of two-sided electro-deposition as can be seen from Figure 5-With respect to SO4 2- Selectivity passes through value more not
Modified QPPO films increase to 4.27, SO from 0.794 2- Slip drops to 19.4% from 39.6%.
As shown in Fig. 6 a, Fig. 6 b, while according to Cl-With respect to SO4 2- Selectivity passes through value and understands, relatively unmodified QPPO
For film, the best results of the modified PEI- QPPO films of two-sided electro-deposition then have the PEI- being modified to two-sided electro-deposition
QPPO films have carried out two electrodialysis experiments of hour, and diluting compartment solution is taken using ion chromatography concentration every 20min.
Claims (10)
1. a kind of preparation method of monovalent anion selective diffusion barrier, it is characterised in that the QPPO using partial quaternization is cloudy
The bromomethyl of remaining is reacted with the amine in the PEI using electro-deposition means in amberplex so that QPPO anion are handed over
PEI on the film surface covalence graft of film is changed, is obtained with monovalence, multivalent anions selective diffusion barrier.
2. a kind of preparation method of monovalent anion selective diffusion barrier according to claim 1, it is characterised in that its system
Preparation Method comprises the following steps：
1）Prepare BPPO solution：To adding 1-Methyl-2-Pyrrolidone to mix in BPPO solids, BPPO solid dissolvings are obtained completely
BPPO solution；
2）By step 1）In BPPO solution add trimethylamine ethanol solution, stirring reaction 1-10h, obtains part quaternary ammonium at room temperature
The QPPO solution of change；
3）By step 2）In QPPO solution be coated on film forming on glass plate, be placed on panel heater and dry, obtain QPPO cloudy
Amberplex；
4）By step 3）In QPPO anion-exchange membranes carry out electro-deposition PEI experiments, in QPPO anion-exchange membranes remaining
Bromomethyl is reacted with the amine in the PEI using electro-deposition means, and PEI chemical bonds are bonded in into QPPO surfaces, obtains unit price
Anion selectivity seperation film PEI- QPPO.
3. a kind of preparation method of monovalent anion selective diffusion barrier according to claim 2, it is characterised in that step
1）In the BPPO amounts of weighing be 1-10g, solvent NMP consumptions be 1-30g, the BPPO solution concentrations for finally obtaining be 3-90%.
4. a kind of preparation method of monovalent anion selective diffusion barrier according to claim 2, it is characterised in that step
2）Middle trimethylamine ethanol solution concentration is 4.27mol/L, and the volumetric usage of trimethylamine ethanol solution is the 0.2- of BPPO mass
1ml/g。
5. a kind of preparation method of monovalent anion selective diffusion barrier according to claim 2, it is characterised in that step
2）In reaction time be 3-8h, quaternization degree be less than 100%.
6. a kind of preparation method of monovalent anion selective diffusion barrier according to claim 2, it is characterised in that step
3）In the scraper thickness that is used of QPPO solution coating filmforms be 550-650 μm, panel heater temperature is 55-65 DEG C, heating
Time is 7-9h, and preferably scraper thickness is 600 μm, and panel heater temperature is 60 DEG C, and the heat time is 8h.
7. a kind of preparation method of monovalent anion selective diffusion barrier according to claim 2, it is characterised in that step
4）In electro-deposition PEI concentration for 1-20g/L the aqueous solution, electrodeposition time is 0.5-2h, and current density is 1-20mA/
cm2, temperature is room temperature.
8. a kind of preparation method of monovalent anion selective diffusion barrier according to claim 2, it is characterised in that step
4）In the bonded process of chemical bond be the NMP/ water in PEI mixed solution, the mass content of NMP is less than 50%.
9. a kind of preparation method of monovalent anion selective diffusion barrier according to claim 2, it is characterised in that step
4）In PEI molecular weight in 1000-800000, the concentration of PEI is 1-20g/L, and the bromomethyl content of remaining is less than 75%.
10. a kind of preparation method of monovalent anion selective diffusion barrier according to claim 2, it is characterised in that unit price
Anion selectivity seperation film PEI- QPPO are the ionic membrane that single or double electro-deposition is modified.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107482239A (en) * | 2017-07-18 | 2017-12-15 | 中国地质大学（武汉） | A kind of PEM with high alcohol-rejecting ability and preparation method thereof |
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| CN113413926B (en) * | 2021-06-01 | 2022-05-10 | 浙江工业大学 | Preparation method of antibacterial anion exchange membrane |
| CN116196768A (en) * | 2023-02-08 | 2023-06-02 | 中国科学技术大学 | Preparation method of mono/divalent selective anion membrane |
| CN116196768B (en) * | 2023-02-08 | 2024-05-07 | 中国科学技术大学 | Preparation method of mono/divalent selective anion membrane |
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