CN107213797A - A kind of preparation method of phosphorus alkene poly-dopamine composite membrane - Google Patents
A kind of preparation method of phosphorus alkene poly-dopamine composite membrane Download PDFInfo
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- CN107213797A CN107213797A CN201710495564.0A CN201710495564A CN107213797A CN 107213797 A CN107213797 A CN 107213797A CN 201710495564 A CN201710495564 A CN 201710495564A CN 107213797 A CN107213797 A CN 107213797A
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
- B01D46/543—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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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
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/60—Polyamines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0666—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0672—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/35—Use of magnetic or electrical fields
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- Polymers & Plastics (AREA)
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of preparation method of phosphorus alkene poly-dopamine composite membrane, including:Phosphorus alkene is coated on conducting metal phosphorus alkene electrode is made;Dopamine hydrochloride is placed in phosphate buffer solution and is uniformly dispersed, Dopamine hydrochloride electrolyte is made;The phosphorus alkene electrode and metal are placed in electrode in the Dopamine hydrochloride electrolyte, and reacted using chronoptentiometry, current density is 0.1~5mA/cm2, the reaction time be 0.1~72h so that phosphorus alkene poly-dopamine, which is made, is combined film precursor;The phosphorus alkene poly-dopamine is combined film precursor and is placed in pH value and is not higher than in 5 solution and soaks 0.1~72h, so that phosphorus alkene poly-dopamine composite membrane is made.The present invention can not only effectively prepare the comprehensive phosphorus alkene poly-dopamine composite membrane for playing both phosphorus alkene and poly-dopamine advantage, and simple to operate, low for equipment requirements, good product quality, yield are high, be very suitable for carrying out large-scale production.
Description
Technical field
The present invention relates to the preparation method of phosphorus alkene field of compound material, more particularly to a kind of phosphorus alkene-poly-dopamine composite membrane.
Background technology
Phosphorus alkene material be by the tightly packed new phosphorus nano material into bi-dimensional cellular shape lattice structure of individual layer phosphorus atoms, its
Special stable micro-structure makes it have excellent chemical property and heat-conductive characteristic, therefore phosphorus alkene material is logical in electronics
The fields such as letter, communications and transportation have broad prospect of application.
Phosphorus alkene material because phosphorus atoms interlayer have stronger Van der Waals force, it is prone to stratification and form similar film
Laminated structure, this structure can cause specific surface area significantly to reduce, thus can the distinctive absorption of heavy losses phosphorus alkene, it is conductive,
The excellent properties such as heat conduction.In addition, the stronger chemism of phosphorus alkene makes it easily be corroded by materials such as oxygen gas and waters and lose original property
Energy.The mechanical performance and water-oil separating performance of phosphorus alkene are poor, are easily acted on and are destroyed by external force when in use, and can be because specific
Use environment limits and loses separating property.
In the prior art, the phosphorus alkene material specific surface area of preparation is smaller, and mechanical performance and water-oil separating performance are weaker, separately
Outer stratification to phosphorus alkene and it is oxidized easily the shortcoming of erosion and does not have good processing method, and phosphorus alkene-poly- does not occur
Dopamine composite membrane and its synthetic method.
The content of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of system of phosphorus alkene-poly-dopamine composite membrane
Preparation Method, can not only effectively prepare the comprehensive phosphorus alkene-poly-dopamine composite membrane for playing both phosphorus alkene and poly-dopamine advantage,
And simple to operate, low for equipment requirements, good product quality, yield are high, it is very suitable for carrying out large-scale production.The phosphorus alkene-poly-
Dopamine composite membrane has good mechanical performance and excellent adhesion property and gas liquid separating property, can extensive use
In fields such as gas-liquid separation purifying.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of phosphorus alkene-poly-dopamine composite membrane, comprises the following steps:
Step A, phosphorus alkene is coated on conducting metal phosphorus alkene electrode is made;
Step B, Dopamine hydrochloride be placed in phosphate buffer solution be uniformly dispersed, be made concentration be 0.01~
0.5mol/L Dopamine hydrochloride electrolyte;
Step C, the phosphorus alkene electrode and metal be placed in electrode in the Dopamine hydrochloride electrolyte, and use timing
Potentiometry is reacted, and current density is 0.1~5mA/cm2, the reaction time be 0.1~72h, so that phosphorus alkene-poly- DOPA is made
Amine is combined film precursor;
Step D, the phosphorus alkene-poly-dopamine is combined film precursor be placed in pH value be not higher than in 5 solution immersion 0.1~
72h, then carries out separation of solid and liquid, and the solid that separation of solid and liquid is obtained is dried, and is combined so that phosphorus alkene-poly-dopamine is made
Film.
Preferably, described conducting metal is at least one of gold, platinum, silver, copper, iron, nickel, zinc, tin, lead, stainless steel.
Preferably, described conducting metal is shaped as sheet, netted, bar-shaped, thread or foam-like.
Preferably, the metal is identical with the conducting metal to the composition of electrode.
Preferably, it is at least one of sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid that the pH value, which is not higher than 5 solution,.
Preferably, the pH value be not higher than 5 solution at least one of sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid with
Second group of solution is mixed;Second group of solution is:Water, methanol, ethanol, propyl alcohol, acetone, tetrahydrofuran, carbon tetrachloride,
Acetonitrile, ether, petroleum ether, pentane, hexane, carbon disulfide, dichloromethane, dichloroethanes, chloroform, trichloroethanes, acetic acid
In ethyl ester, butanone, benzene, hexamethylene, N,N-dimethylformamide, formaldehyde, ammoniacal liquor, hydrazine hydrate, 1-METHYLPYRROLIDONE at least
It is a kind of.
As seen from the above technical solution provided by the invention, phosphorus alkene-poly-dopamine composite membrane provided by the present invention
Preparation method phosphorus alkene is coated on conducting metal phosphorus alkene electrode is made, and using chronoptentiometry on phosphorus alkene electrode it is electrochemical
Polymerization generation phosphorus alkene-conductive polymer composite presoma is learned, is then removed before the phosphorus alkene-conductive polymer composite
Conducting metal in body is driven, so that phosphorus alkene-poly-dopamine composite membrane is made;Phosphorus alkene-poly-dopamine the composite membrane have phosphorus alkene and
The two-fold advantage of poly-dopamine, specific surface area are big, good mechanical property, and the stalling characteristic with good gas, liquid with
And excellent stability and flexibility, it can be widely applied to the fields such as gas-liquid separation purifying.Phosphorus alkene provided by the present invention-poly- DOPA
The preparation method of amine composite membrane is simple to operate, low for equipment requirements, good product quality, yield are high, is very suitable for carrying out scale
Production.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, being used required in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is the electron scanning micrograph of the N doping phosphorus alkene prepared by the embodiment of the present invention 1.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to protection scope of the present invention.
The preparation method to phosphorus alkene-poly-dopamine composite membrane provided by the present invention is described in detail below.
A kind of preparation method of phosphorus alkene-poly-dopamine composite membrane, comprises the following steps:
Step A, phosphorus alkene is coated on conducting metal phosphorus alkene electrode is made.Wherein, described conducting metal be gold, platinum,
At least one of silver, copper, iron, nickel, zinc, tin, lead, stainless steel, and the shape of conducting metal can be sheet, netted, rod
Shape, thread or foam-like.
Step B, Dopamine hydrochloride be placed in phosphate buffer solution be uniformly dispersed, be made concentration be 0.01~
0.5mol/L Dopamine hydrochloride electrolyte.
Step C, the phosphorus alkene electrode and metal be placed in electrode in the Dopamine hydrochloride electrolyte, and use timing
Potentiometry is reacted, and current density is 0.1~5mA/cm2, the reaction time be 0.1~72h, so that phosphorus alkene-poly- DOPA is made
Amine is combined film precursor.
Step D, the phosphorus alkene-poly-dopamine is combined film precursor be placed in pH value be not higher than in 5 solution immersion 0.1~
72h, to remove conducting metal in the phosphorus alkene-conductive polymer composite presoma, then carries out separation of solid and liquid, and to solid
The isolated solid of liquid is dried, so that phosphorus alkene-poly-dopamine composite membrane is made.Wherein, the metal can be with to electrode
, can also be identical with conducting metal described in step A using any conducting metal.Wherein, the pH value be not higher than 5 solution can
It is individually composed by first group of solution, can be also mixed and constituted with second group of solution by first group.First group of solution is:Sulfuric acid, hydrochloric acid,
At least one of nitric acid, acetic acid, propionic acid.Second group of solution is:Water, methanol, ethanol, propyl alcohol, acetone, tetrahydrofuran, tetrachloro
Change carbon, acetonitrile, ether, petroleum ether, pentane, hexane, carbon disulfide, dichloromethane, dichloroethanes, chloroform, trichloroethanes,
In ethyl acetate, butanone, benzene, hexamethylene, N,N-dimethylformamide, formaldehyde, ammoniacal liquor, hydrazine hydrate, 1-METHYLPYRROLIDONE
It is at least one.
Specifically, phosphorus alkene is coated on conductive gold by the preparation method of phosphorus alkene-poly-dopamine composite membrane provided by the present invention
Phosphorus alkene electrode is made on category, and electrochemical polymerization generation phosphorus alkene-conducting polymer is multiple on phosphorus alkene electrode using chronoptentiometry
Condensation material presoma, then removes conducting metal in the phosphorus alkene-conductive polymer composite presoma, so that phosphorus is made
Alkene-poly-dopamine composite membrane;Phosphorus alkene-poly-dopamine the composite membrane has the two-fold advantage of phosphorus alkene and poly-dopamine, specific surface area
Greatly, good mechanical property, and with good gas, the stalling characteristic of liquid and excellent stability and flexibility, can be extensive
Applied to fields such as gas-liquid separation purifying.The preparation method of phosphorus alkene-poly-dopamine composite membrane provided by the present invention is simple to operate,
Low for equipment requirements, good product quality, yield are high, are very suitable for carrying out large-scale production.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, below with tool
The preparation method for phosphorus alkene-poly-dopamine composite membrane that body embodiment is provided the embodiment of the present invention is described in detail.
Embodiment 1
A kind of preparation method of phosphorus alkene-poly-dopamine composite membrane, comprises the following steps:
Step a1, phosphorus alkene is coated on nickel foam phosphorus alkene electrode is made.
Step b1, Dopamine hydrochloride is placed in phosphate buffer solution be uniformly dispersed, it is 0.02mol/L's that concentration, which is made,
Dopamine hydrochloride electrolyte.
Step c1, the phosphorus alkene electrode and goldleaf be placed in electrode in the Dopamine hydrochloride electrolyte, and using meter
When potentiometry reacted, current density is 0.1mA/cm2, the reaction time be 72h, be combined so that phosphorus alkene-poly-dopamine is made
Film precursor;
Step d1, by the phosphorus alkene-poly-dopamine be combined film precursor be placed in the hydrochloric acid solution of pH value 0.001 soak
0.2h, then carries out separation of solid and liquid, and the solid that separation of solid and liquid is obtained is dried, so that obtained phosphorus alkene as shown in Figure 1-
Poly-dopamine composite membrane.
Embodiment 2
A kind of preparation method of phosphorus alkene-poly-dopamine composite membrane, comprises the following steps:
Step a2, phosphorus alkene is coated on aluminium foil phosphorus alkene electrode is made.
Step b2, Dopamine hydrochloride is placed in phosphate buffer solution be uniformly dispersed, it is 0.1mol/L's that concentration, which is made,
Dopamine hydrochloride electrolyte.
Step c2, the phosphorus alkene electrode and aluminium foil be placed in electrode in the Dopamine hydrochloride electrolyte, and using meter
When potentiometry reacted, current density is 0.5mA/cm2, the reaction time be 60h, be combined so that phosphorus alkene-poly-dopamine is made
Film precursor;
Step d2, the phosphorus alkene-poly-dopamine is combined film precursor it is placed in the sulfuric acid solution of pH value 0.01 and soaks 6h,
Then separation of solid and liquid is carried out, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine composite membrane is made.
Embodiment 3
A kind of preparation method of phosphorus alkene-poly-dopamine composite membrane, comprises the following steps:
Step a3, phosphorus alkene is coated on copper wire phosphorus alkene electrode is made.
Step b3, Dopamine hydrochloride is placed in phosphate buffer solution be uniformly dispersed, it is 0.25mol/L's that concentration, which is made,
Dopamine hydrochloride electrolyte.
Step c3, the phosphorus alkene electrode and copper wire be placed in electrode in the Dopamine hydrochloride electrolyte, and using meter
When potentiometry reacted, current density is 2mA/cm2, the reaction time be 48h, so that phosphorus alkene-poly-dopamine composite membrane is made
Presoma;
Step d3, by the phosphorus alkene-poly-dopamine be combined film precursor be placed in the sulfuric acid and acetonitrile mixed solution of pH value 1
24h is soaked, separation of solid and liquid is then carried out, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine is made
Composite membrane.
Embodiment 4
A kind of preparation method of phosphorus alkene-poly-dopamine composite membrane, comprises the following steps:
Step a4, phosphorus alkene is coated on stainless (steel) wire phosphorus alkene electrode is made.
Step b4, Dopamine hydrochloride is placed in phosphate buffer solution be uniformly dispersed, it is 0.35mol/L's that concentration, which is made,
Dopamine hydrochloride electrolyte.
Step c4, the phosphorus alkene electrode and stainless (steel) wire be placed in electrode in the Dopamine hydrochloride electrolyte, and adopted
Reacted with chronoptentiometry, current density is 3.5mA/cm2, the reaction time be 12h, so that phosphorus alkene-poly-dopamine is made
Compound film precursor;
Step d4, the phosphorus alkene-poly-dopamine is combined film precursor it is placed in the salpeter solution of pH value 3 and soaks 48h, so
After carry out separation of solid and liquid, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine composite membrane is made.
Embodiment 5
A kind of preparation method of phosphorus alkene-poly-dopamine composite membrane, comprises the following steps:
Step a5, phosphorus alkene is coated on zinc bar phosphorus alkene electrode is made.
Step b5, Dopamine hydrochloride is placed in phosphate buffer solution be uniformly dispersed, it is 0.5mol/L's that concentration, which is made,
Dopamine hydrochloride electrolyte.
Step c5, the phosphorus alkene electrode and zinc bar be placed in electrode in the Dopamine hydrochloride electrolyte, and using meter
When potentiometry reacted, current density is 5mA/cm2, the reaction time be 0.2h, so that phosphorus alkene-poly-dopamine composite membrane is made
Presoma;
Step d5, the phosphorus alkene-poly-dopamine is combined film precursor it is placed in the nitric acid and N, N- dimethyl formyl of pH value 5
72h is soaked in amine mixed solution, separation of solid and liquid is then carried out, and the solid that separation of solid and liquid is obtained is dried, so as to be made
Phosphorus alkene-poly-dopamine composite membrane.
As fully visible, the comprehensive phosphorus alkene-poly- many for playing both phosphorus alkene and poly-dopamine advantage can not only effectively be prepared
Bar amine composite membrane, and simple to operate, low for equipment requirements, good product quality, yield are high, are very suitable for carry out scale metaplasia
Production.Phosphorus alkene-poly-dopamine the composite membrane has good mechanical performance and excellent adhesion property and gas liquid separation property
Can, it can be widely applied to the fields such as gas-liquid separation purifying.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (6)
1. a kind of preparation method of phosphorus alkene-poly-dopamine composite membrane, it is characterised in that comprise the following steps:
Step A, phosphorus alkene is coated on conducting metal phosphorus alkene electrode is made;
Step B, Dopamine hydrochloride is placed in phosphate buffer solution be uniformly dispersed, it is 0.01~0.5mol/L's that concentration, which is made,
Dopamine hydrochloride electrolyte;
Step C, the phosphorus alkene electrode and metal be placed in electrode in the Dopamine hydrochloride electrolyte, and use time-measuring electric potential
Method is reacted, and current density is 0.1~5mA/cm2, the reaction time be 0.1~72h so that it is multiple that phosphorus alkene-poly-dopamine is made
Close film precursor;
Step D, the phosphorus alkene-poly-dopamine is combined film precursor it is placed in pH value and be not higher than in 5 solution 0.1~72h of immersion,
Then separation of solid and liquid is carried out, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine composite membrane is made.
2. the preparation method of phosphorus alkene-poly-dopamine composite membrane according to claim 1, it is characterised in that described conduction
Metal is at least one of gold, platinum, silver, copper, iron, nickel, zinc, tin, lead, stainless steel.
3. the preparation method of phosphorus alkene-poly-dopamine composite membrane according to claim 1 or 2, it is characterised in that described leads
Electric metal is shaped as sheet, netted, bar-shaped, thread or foam-like.
4. the preparation method of phosphorus alkene-poly-dopamine composite membrane according to claim 1 or 2, it is characterised in that the metal
It is identical with the conducting metal to the composition of electrode.
5. the preparation method of phosphorus alkene-poly-dopamine composite membrane according to claim 1 or 2, it is characterised in that the pH value
Not higher than 5 solution is at least one of sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid.
6. the preparation method of phosphorus alkene-poly-dopamine composite membrane according to claim 1 or 2, it is characterised in that the pH value
Not higher than 5 solution is that at least one of sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid are mixed with second group of solution;It is described
Second group of solution be water, methanol, ethanol, propyl alcohol, acetone, tetrahydrofuran, carbon tetrachloride, acetonitrile, ether, petroleum ether, pentane, oneself
Alkane, carbon disulfide, dichloromethane, dichloroethanes, chloroform, trichloroethanes, ethyl acetate, butanone, benzene, hexamethylene, N, N-
At least one of dimethylformamide, formaldehyde, ammoniacal liquor, hydrazine hydrate, 1-METHYLPYRROLIDONE.
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