CN108993416A - A kind of preparation method of copper ion blotting membrane - Google Patents
A kind of preparation method of copper ion blotting membrane Download PDFInfo
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- CN108993416A CN108993416A CN201810911804.5A CN201810911804A CN108993416A CN 108993416 A CN108993416 A CN 108993416A CN 201810911804 A CN201810911804 A CN 201810911804A CN 108993416 A CN108993416 A CN 108993416A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/046—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing halogens, e.g. halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The present invention relates to a kind of preparation methods of copper ion blotting membrane, it is the situation for the heavy metal containing wastewater treatment hardly possible of low concentration, it is combined using automatically controlled ion exchange technique and ionic imprinting technique, ion blotting film is prepared using any constant potential method by staircase wave under three-electrode system, this preparation method technique is advanced, it not will cause secondary pollution and waste, data are accurately full and accurate, product is the atrament being aggregated on carbon cloth, microscopic appearance is near-spherical substance, ferrous cyanide ion is doped in film, there is good removal ability for the heavy metal wastewater thereby of low concentration, it is the preparation method of advanced ion blotting film.
Description
Technical field
The present invention relates to a kind of preparation methods of copper ion blotting membrane, belong to the technology neck of the preparation of ion blotting material and application
Domain.
Background technique
With the development of the social economy, the utilization of water resource and unreasonable wasting phenomenon are increasingly severe, water resource lacks
The reason of problem is increasingly significant, causes this phenomenon first is that water body is polluted by industrial wastewater, therefore the Industry Waste that will be polluted
It is very urgent that water is changed into direct available water resource.
Wherein one of the metal that copper finds and uses earliest as the mankind is widely used in metallurgy, plating and chemical industry etc.
Industry, generation largely can all cause damages to animals and plants and human body due to its non-degradable containing the waste water of copper ion.
The method of processing low concentration copper ion waste water mainly has chemical method, ion-exchange, absorption method and bioanalysis at present,
But mostly there is the problems such as secondary pollution, waste and poor selectivity.
Automatically controlled ion exchange receives highest attention as a kind of environmentally friendly ion isolation and recovery method；?
In adsorption process, the absorption to object ion is realized by adjusting the redox reaction state of automatically controlled amberplex and is released
It puts, film can be reused, and will not generate pollution and secondary waste in the whole process；Ionic imprinting technique can due to structure
Predictive and specific recognition and attract extensive attention；Depending on function monomer for object ion specific recognition has
The binding site to match with template ion in size, shape and functional group, is tied by complexing or electrostatic interaction
It closes, realizes the specific recognition for template molecule or ion；Therefore automatically controlled ion exchange technique is mutually tied with ionic imprinting technique
Close, the copper ion blotting membrane that preparation adsorption capacity is strong, selectivity is high and reusing is good be it is feasible, this technology is also in section
It learns in research.
Summary of the invention
Goal of the invention
The purpose of the present invention is being directed to background technique, using copper ion as template ion, potassium ferrocyanide is function monomer,
Pyrroles is conductive crosslinking agent, synthesizes ion imprinted polymer in carbon cloth surfaces using unipolar pulse method, makes the copper ion print of preparation
Mark film is applied in adsorbing separation.
Technical solution
The chemical substance material that the present invention uses are as follows: copper chloride, potassium ferrocyanide, pyrroles, potassium chloride, deionized water, a combination thereof
It is as follows to prepare dosage: being measurement unit with gram, milliliter, millimeter
Copper chloride: CuCl2•2H2O 0.1704g±0.0001g
Potassium ferrocyanide: K4Fe(CN)6•3H2O 0.4224g±0.0001g
Pyrroles: C4H5N 0.14mL±0.0001mL
Potassium chloride: KCl 0.3725g ± 0.0001g
Deionized water: H2O 2000mL±20mL
Carbon cloth 30mm × 20mm × 0.4mm
Stainless steel substrates 30mm × 20mm × 0.2mm
Calomel electrode 140mm × 22mm × 10mm
The preparation method is as follows:
(1) selected chemical substance material
The chemical substance material that uses of preparation to be carried out selected, and carry out quality purity control:
Copper chloride: solid state purity 99%
Potassium ferrocyanide: solid state purity 99.5%
Pyrroles: liquid liquid purity 99%
Potassium chloride: solid state purity 99.5%
Deionized water: liquid liquid purity 99.99%
(2) preparation of copper ion blotting membrane
The preparation of copper ion blotting membrane carries out under DC power supply three-electrode system: working electrode: carbon cloth, to electrode: stainless steel
Piece, reference electrode: calomel electrode, recycle 10,000 times using any constant potential ladder wave method and be made: operating potential :+0.8V is held
The continuous time: 0.8s, open circuit potential :+0.2V, duration: 0.8s；
1. measuring 50 mL of deionized water, potassium chloride 0.3725g ± 0.0001g, copper chloride 0.1704g ± 0.0001g, Asia are weighed
Potassium ferricyanide 0.4224g ± 0.0001g is added stirring in beaker and forms mixed solution；
2. being cleaned by ultrasonic stainless steel substrates, supersonic frequency 40kHz, scavenging period 10min；
3. carbon cloth is clipped on platinized platinum folder, presss from both sides working electrode with platinized platinum and be connected, stainless steel substrates are clipped in on electrode, are saturated calomel
Electrode holder is dipped in mixed solution on reference electrode；
4. to using parameter to be configured, operating potential :+0.8V, duration: 0.8s, open circuit potential :+0.2V, continue when
Between: 0.8s, cycle-index: 10000 times；
5. after reaction, being rinsed with deionized water to prepared blotting membrane, standing is dried；As copper ion trace
Film；
(3) it is dried in vacuo
Copper ion blotting membrane is placed in quartz container, is subsequently placed in vacuum oven, 30 DEG C of drying temperature, vacuum degree 2Pa,
Drying time 40min is final product: copper ion blotting membrane after dry；
(4) test, analysis and characterization
The pattern of the copper ion blotting membrane of preparation, color, ingredient, Chemical Physics performance, absorption property are detected, analyzed,
Characterization；
Morphology analysis is carried out with field emission scanning electron microscope；
Microcosmic elemental analysis is carried out with energy disperse spectroscopy；
Surface functional group analysis is carried out with infrared spectrometer；
Concentration analysis is carried out with plasma emission spectrometer；
Conclusion: copper ion blotting membrane covers one layer of black solid in carbon cloth surfaces, and microscopic appearance is near-spherical substance, passes through energy
Spectrometer and infrared spectrometer show wherein to adulterate ferrous cyanide ion have good removal energy for the copper ion of low concentration
Power.
(5) product storage
The copper ion blotting membrane of preparation is stored in surface plate, and 20 DEG C of storage temperature, relative humidity 10%.
Beneficial effect
There is apparent advance compared with the background technology, the present invention, be the feelings for the heavy metal containing wastewater treatment hardly possible of low concentration
Condition is combined using automatically controlled ion exchange technique and ionic imprinting technique, and any constant potential rank is used under three-electrode system
Terraced wave method prepares ion blotting film, this preparation method technique is advanced, and it is accurately full and accurate not will cause secondary pollution and waste, data,
Product is the atrament being aggregated on carbon cloth, and microscopic appearance is near-spherical substance, and ferrous cyanide ion is doped in film, for
The heavy metal wastewater thereby of low concentration has good removal ability, is the preparation method of advanced ion blotting film.
Detailed description of the invention
Fig. 1, ion blotting film preparation state diagram
Fig. 2, ion blotting film shape appearance figure
Fig. 3, ion blotting film energy spectrum diagram
The infrared spectrogram of Fig. 4, ion blotting film
Fig. 5, ion blotting film removal ability figure
Fig. 6, ion blotting film and non-blotting membrane removal ability compare figure
As shown in the figure, list of numerals is as follows:
1, glass electrolytic cell, 2, direct current electrochemical workstation, 3, electric cabinet, 4, magneton blender, the 5, first hang spring, 6, second hangs
Silk, 7, third hang spring, 8, working electrode, 9, to electrode, 10, reference electrode, 11, mixed solution, 12, display screen, 13, instruction
Lamp, 14, power switch, 15, mixing control device, 16, heating controller.
Specific embodiment
The present invention will be further described below with reference to the accompanying drawings:
It is ion blotting film preparation state diagram, each portion position, connection relationship will be matched correctly according to quantity, sequentially be operated shown in Fig. 1.
The magnitude for preparing the chemical substance used is determined by pre-set range, is metering with gram, milliliter, millimeter
Unit.
Direct current electrochemical workstation 2 is vertical, is glass electrolytic cell 1 in the lower part of electrochemical workstation 2, in glass electrolysis
The lower part of slot 1 is electric cabinet 3；The first hang spring 5, the second hang spring 6, third hang spring are equipped in the lower part of direct current electrochemical workstation 2
7, and protrude into glass electrolytic cell 1；First hang spring, 5 lower part connects working electrode 8, and 6 lower part of the second hang spring is connected to electrode 9, the
Three hang springs, 7 lower part connects reference electrode 10；Put magneton blender 4 in 1 bottom of glass electrolytic cell；It is put into glass electrolytic cell 1 mixed
Close solution 11；Working electrode 8 protrudes into mixed solution 11 electrode 9, reference electrode 10；Display screen is equipped on electric cabinet 3
12, indicator light 13, power switch 14, mixing control device 15, heating controller 16.
It is ion blotting film shape appearance figure shown in Fig. 2, as shown in the figure, polymeric material is atrament on ion blotting film,
For spherical shape particle.
Shown in Fig. 3, there are the elements such as C, N, Au, Cl, Fe on ion blotting film as shown in the figure for ion blotting film energy spectrum diagram,
Show during pyrroles polymerize, Cl-With Fe (CN)6 4-It is doped in pyrroles's film as counter ion counterionsl gegenions.
It is ion blotting film infrared spectrogram, as shown in the figure, 1036 cm shown in Fig. 4-1For N-H key bending vibration,
1163 cm-1For the stretching vibration of C-N key, 1295 cm-1For=in plane vibration of c h bond, 1387 cm-1For C-N key, 1462 cm-1
For pyrrole ring asymmetric stretching vibration, 1536 cm-1For pyrrole ring symmetrical stretching vibration, 1640 cm-1For water angle vibration,
2060 cm-1For C ≡ N key, 2847 cm-1For alkane symmetric vibration, 2922 cm-1For alkane nonsymmetrical vibration, 3445 cm-1For
N-H key.
It is ion blotting film removal ability figure, as shown in the figure, ion blotting film reaches the removal of copper ion shown in Fig. 5
The time of balance needs 5 hours, removal rate 90.1%.
Shown in Fig. 6, compare figure for blotting membrane and non-blotting membrane removal ability, as shown in the figure, blotting membrane removes copper ion
Except the time for reaching balance needs 5 hours, removal rate 90.1%；Non- blotting membrane is 65.9% to the removal rate of copper ion, trace
Film is non-blotting membrane to 1.4 times of the removal rate of copper ion to the removal rate of copper ion.
Claims (2)
1. a kind of preparation method of copper ion blotting membrane, it is characterised in that: the chemical substance material used are as follows: copper chloride, ferrous iron
Potassium cyanide, pyrroles, potassium chloride, deionized water, it is as follows that a combination thereof prepares dosage: being measurement unit with gram, milliliter, millimeter
Copper chloride: CuCl2•2H2O 0.1704g±0.0001g
Potassium ferrocyanide: K4Fe(CN)6•3H2O 0.4224g±0.0001g
Pyrroles: C4H5N 0.14mL±0.0001mL
Potassium chloride: KCl 0.3725g ± 0.0001g
Deionized water: H2O 2000mL±20mL
Carbon cloth 30mm × 20mm × 0.4mm
Stainless steel substrates 30mm × 20mm × 0.2mm
Calomel electrode 140mm × 22mm × 10mm
The preparation method is as follows:
(1) selected chemical substance material
The chemical substance material that uses of preparation to be carried out selected, and carry out quality purity control:
Copper chloride: solid state purity 99%
Potassium ferrocyanide: solid state purity 99.5%
Pyrroles: liquid liquid purity 99%
Potassium chloride: solid state purity 99.5%
Deionized water: liquid liquid purity 99.99%
(2) preparation of copper ion blotting membrane
The preparation of copper ion blotting membrane carries out under DC power supply three-electrode system: working electrode: carbon cloth, to electrode: stainless steel
Piece, reference electrode: calomel electrode, recycle 10,000 times using any constant potential ladder wave method and be made: operating potential :+0.8V is held
The continuous time: 0.8s, open circuit potential :+0.2V, duration: 0.8s；
1. measuring 50 mL of deionized water, potassium chloride 0.3725g ± 0.0001g, copper chloride 0.1704g ± 0.0001g, Asia are weighed
Potassium ferricyanide 0.4224g ± 0.0001g is added stirring in beaker and forms mixed solution；
2. being cleaned by ultrasonic stainless steel substrates, supersonic frequency 40kHz, scavenging period 10min；
3. carbon cloth is clipped on platinized platinum folder, presss from both sides working electrode with platinized platinum and be connected, stainless steel substrates are clipped in on electrode, are saturated calomel
Electrode holder is dipped in mixed solution on reference electrode；
4. to using parameter to be configured, operating potential :+0.8V, duration: 0.8s, open circuit potential :+0.2V, continue when
Between: 0.8s, cycle-index: 10000 times；
5. after reaction, being rinsed with deionized water to prepared blotting membrane, standing is dried；As copper ion trace
Film；
(3) it is dried in vacuo
Copper ion blotting membrane is placed in quartz container, is subsequently placed in vacuum oven, 30 DEG C of drying temperature, vacuum degree 2Pa,
Drying time 40min is final product: copper ion blotting membrane after dry；
(4) test, analysis and characterization
The pattern of the copper ion blotting membrane of preparation, color, ingredient, Chemical Physics performance, absorption property are detected, analyzed,
Characterization；
Morphology analysis is carried out with field emission scanning electron microscope；
Microcosmic elemental analysis is carried out with energy disperse spectroscopy；
Surface functional group analysis is carried out with infrared spectrometer；
Concentration analysis is carried out with plasma emission spectrometer；
Conclusion: copper ion blotting membrane covers one layer of black solid in carbon cloth surfaces, and microscopic appearance is near-spherical substance, passes through energy
Spectrometer and infrared spectrometer show wherein to adulterate ferrous cyanide ion have good removal energy for the copper ion of low concentration
Power；
(5) product storage
The copper ion blotting membrane of preparation is stored in surface plate, and 20 DEG C of storage temperature, relative humidity 10%.
2. a kind of preparation method of copper ion blotting membrane according to claim 1, it is characterised in that:
Direct current electrochemical workstation (2) is vertical, is glass electrolytic cell (1) in the lower part of electrochemical workstation (2), in vitreous electricity
The lower part for solving slot (1) is electric cabinet (3)；The first hang spring (5) are equipped in the lower part of direct current electrochemical workstation (2), the second hang spring
(6), third hang spring (7), and protrude into glass electrolytic cell (1)；；First hang spring (5) lower part connects working electrode (8), and second hangs
The connection of silk (6) lower part connects reference electrode (10) to electrode (9), third hang spring (7) lower part；It puts glass electrolytic cell (1) bottom
Magneton blender (4)；Mixed solution (11) are put into glass electrolytic cell (1)；Working electrode (8), to electrode (9), reference electrode
(10) it protrudes into mixed solution (11)；It is equipped with display screen (12) on electric cabinet (3), indicator light (13), power switch (14), stirs
Mix controller (15), heating controller (16).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124631A (en) * | 2019-04-16 | 2019-08-16 | 太原理工大学 | A method of lithium ion blotting membrane is prepared based on automatically controlled ion exchange |
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| CN102794153A (en) * | 2012-07-12 | 2012-11-28 | 清华大学 | Compound ferrous iron cyanide titanium potassium magnetic ball and preparation method thereof |
| CN103214689A (en) * | 2013-03-20 | 2013-07-24 | 太原理工大学 | Preparation method of ion imprinted polymer film |
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| CN107149880A (en) * | 2016-03-02 | 2017-09-12 | 天津工业大学 | A kind of copper ion selection seperation film and preparation method thereof |
| CN107768150A (en) * | 2017-10-26 | 2018-03-06 | 吉林大学 | Copper ion doped polyaniline electrode with carbon cloth as substrate and preparation method thereof |
| CN107879318A (en) * | 2017-11-01 | 2018-04-06 | 太原理工大学 | A kind of method that bubble stripping method prepares class graphite phase carbon nitride nanometer sheet |
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| CN101787123A (en) * | 2010-03-05 | 2010-07-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | Molecular engram polymer and preparation and application thereof |
| CN102794153A (en) * | 2012-07-12 | 2012-11-28 | 清华大学 | Compound ferrous iron cyanide titanium potassium magnetic ball and preparation method thereof |
| CN103214689A (en) * | 2013-03-20 | 2013-07-24 | 太原理工大学 | Preparation method of ion imprinted polymer film |
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Application publication date: 20181214 |
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| RJ01 | Rejection of invention patent application after publication |