CN110314560A - A kind of water-oil separationg film and preparation method thereof and a kind of oil-water separation method - Google Patents
A kind of water-oil separationg film and preparation method thereof and a kind of oil-water separation method Download PDFInfo
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- CN110314560A CN110314560A CN201910484693.9A CN201910484693A CN110314560A CN 110314560 A CN110314560 A CN 110314560A CN 201910484693 A CN201910484693 A CN 201910484693A CN 110314560 A CN110314560 A CN 110314560A
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- water
- oil
- levodopa
- poly
- oil separationg
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
-
- 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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/06—Dewatering or demulsification of hydrocarbon oils with mechanical means, e.g. by filtration
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1033—Oil well production fluids
Abstract
The invention discloses a kind of water-oil separationg films and preparation method thereof and a kind of oil-water separation method, the water-oil separationg film includes separation membrane base and overlays at least one layer of composite coating on the separation membrane base, the composite coating is assembled with the second material by poly- levodopa and is formed, and second material is at least one of positively charged polyelectrolyte, positively charged compound polyelectrolyte, the material containing metal cation.Electrostatic interaction, which is carried out, using electronegative poly- levodopa and the second positively charged material is compounded to form composite coating, raw material is inexpensively environmentally protective, the composite coating of formation has the characteristic of good automatically cleaning oil resistant adherency, be not easy to fall off from separation membrane base, crude oil/water separation field with good application prospect.
Description
Technical field
The present invention relates to the separation fields of crude oil/water, more particularly, to a kind of water-oil separationg film and preparation method thereof and one
Kind oil-water separation method.
Background technique
The petroleum strategic reserves goods and materials in short supply as country, it is with a very important position in national economy and Chemical Manufacture.
Petroleum acquisition process includes oil exploration and exploitation, the defeated, oil refining of oil gathering etc..It is well known that all oil fields will be undergone
Aqueous development period, especially rate of oil production, are big and water filling is taken to strengthen the oil field of exploitation, and water-free oil production period is generally shorter, and crude oil contains
Water rate increases fast.In recent years, each elephant in China comes into high water-cut stage, and crude oil Produced Liquid moisture content is even up to
90%.During petroleum obtains, crude oil water containing not only increase storage, conveying, in refining process equipment load, and
Fuel consumption when heating is increased, or even causes the fouling or corrosion of equipment and pipeline because of saliferous in water.Therefore, crude oil
It is dehydrated into a particularly important link in petroleum acquisition process.
To develop the high oily water separation technique of a kind of novel energy-conserving, separative efficiency, target is gathered in by multinational researcher
In membrane separation technique.The membrane material taken at present is broadly divided into three classes, i.e. inorganic ceramic membrane, polymeric membrane and metal by material
Nethike embrane.The common feature of these three types of membrane materials is that and all have special wellability with cellular structure, such as super-hydrophobic or super parent
Aqueous nature achievees the purpose that efficiently separate to keep oil in oil water mixture or water highly selective by fenestra road.Its
In, super-hydrophobic film can stop the infiltration of water, only allow oil by seperation film, but crude oil viscosity is big and complicated component, Yi Zao
Film forming blocking；Super hydrophilic film can stop the infiltration of oil, only allow water by seperation film, the super hydrophilic painting with automatically cleaning property
Tunic shows bigger advantage in terms of crude oil dehydration.The separation membrane surface with automatically cleaning property has been typically prepared painting at present
Layer material, such as super amphiphilic macromolecule brush, the strand of polymer brush is containing permanently charged positive and negative charge, this static-electronic driving shape
At hydration layer can efficiently stop the adherency and blocking of crude oil, but polymer brush coating material is usually to pass through atom to turn
Prepared by the method for moving free radical polymerization, preparation condition is harsh, and preparation process is complicated, and needs to introduce a variety of high toxicity chemistry
Product, product only tens nano thickness, are not easy large scale preparation, expensive.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of water-oil separationg film and preparation method thereof, the water-oil separating
Film has the characteristic of good automatically cleaning oil resistant adherency, and environmentally protective, can be mass-produced.
The technical solution used in the present invention is:
The present invention provides a kind of water-oil separationg film, including separation membrane base and overlay on the separation membrane base at least one
Layer composite coating, the composite coating assembles with the second material by poly- levodopa and formed, second material for band just
Polyelectrolyte, positively charged compound polyelectrolyte, at least one of the material containing metal cation of electricity.Polyelectrolyte
Compound refers to the polymer being compounded to form by least two polyelectrolyte with positive and negative charge.
Preferably, the positively charged polyelectrolyte includes polyallylamine, polyethyleneimine, diallyl dimethyl
Any one of ammonium chloride.
Preferably, the positively charged compound polyelectrolyte includes polyallylamine/polyacrylic acid composite, polyethylene
Any one of imines/polyacrylic acid composite, diallyl dimethyl ammoniumchloride/kayexalate.It is above-mentioned to enumerate
Positively charged compound polyelectrolyte be compounded to form by two kinds of polyelectrolyte, the compound of formation is known in the art existing
Compound, the positively charged compound polyelectrolyte that the present invention uses is including but not limited to the above-mentioned specific compound enumerated.
Preferably, the material containing metal cation be metal salt, the metal cation include copper, iron, titanium,
The corresponding cation of at least one of manganese, cobalt, nickel, zinc, aluminium metal.
Preferably, the separation membrane base includes any one of stainless (steel) wire, copper mesh, Teflon film.
The present invention also provides a kind of preparation methods of above-mentioned water-oil separationg film, comprising the following steps:
(1) separation membrane base is taken to be soaked in the solution containing the second material, second material is positively charged poly- electrolysis
Matter and/or positively charged compound polyelectrolyte；
(2) it after taking out and cleaning, is soaked in the solution containing poly- levodopa；
(3) it takes out, wash and dry.
Preferably, circulation carries out step (1) and (2) at least once.In some preferred embodiments, circulation is walked
Suddenly the number of (1) and (2) is 2~200.
Preferably, contain in step (1) in the solution and/or step (2) of the second material and add in the solution containing poly- levodopa
Added with salt.Since poly- levodopa is a kind of electronegative high molecular polymer, water-soluble fabulous, itself is difficult to form coating,
, must be with other positively charged material effects to form coating, and positively charged polyelectrolyte or positively charged polyelectrolyte are multiple
Adduct molecule segment positive charge rich in easily carries out electrostatic attraction effect, Jin Ertong with electronegative poly- levodopa
Cross the layer assembly that static-electronic driving completes composite coating.
In the embodiment for more having choosing, the concentration of poly- levodopa is 1~5mg/mL in the solution containing poly- levodopa, is contained
The concentration of the second material is 1~5mg/mL in the solution of second material.
Further, the salt is sodium salt or sylvite.Polyelectrolyte is shielded by the way that salt ion is added or polyelectrolyte is multiple
The charge for closing object surface, makes its strand that certain rolled state be presented, to be conducive to the increasing when being assembled into composite coating
Add the thickness of assembling coating every time.
In a more preferred embodiment, the concentration of sodium salt or sylvite is 0~2M.
The present invention also provides a kind of preparation methods of water-oil separationg film, comprising the following steps:
(1) it is 2~12 left-handed more containing gathering to be formed that pH adjusting agent is added in the aqueous solution of poly- levodopa and adjusts pH value
Bar solution；
(2) the second material is added in the solution containing poly- levodopa, and to form poly- levodopa/metal cation multiple
Object disperse system is closed, second material contains metal cation；
(3) separation membrane base is soaked in the poly- levodopa/metal cation compound disperse system.
Preferably, the pH adjusting agent is hydrochloric acid or sodium hydroxide.
Preferably, second material is metal salt, including but not limited to mantoquita, molysite, titanium salt, manganese salt, cobalt salt, nickel
Salt, zinc salt, aluminium salt.
The present invention also provides a kind of oil-water separation methods, use above-mentioned water-oil separationg film.
The beneficial effects of the present invention are:
The present invention carries out electrostatic interaction using electronegative poly- levodopa and the second positively charged material and is compounded to form
Object coating is closed, raw material is inexpensively environmentally protective, and the composite coating of formation has the characteristic of good automatically cleaning oil resistant adherency, also has
There are higher water-oil separating efficiency and separation flux, hydratability is strong, be not easy dehydration, grease proofing characteristic has duration, compound
Coating acid-fast alkali-proof is corrosion-resistant, is not easy to fall off from separation membrane base, crude oil/water separation field with good application prospect.
Preparation method preparation condition provided by the invention is simple, the requirement of no special instruments and equipment, soaking at room temperature can be complete
At, easily be mass produced, by the way of immersion made from composite coating can equably cover in separation membrane base
Surface and outer surface have good wear resistance, and the water-oil separationg film of preparation can be made to have high separating efficiency for a long time and divide
From flux.
Detailed description of the invention
Fig. 1 is that construction from part prepares water-oil separationg film and prepares schematic diagram layer by layer in embodiment 1；
Fig. 2 is the scanning electron microscope diagram piece of the water-oil separationg film prepared in embodiment 1；
Fig. 3 is the photo and scanning electron microscope diagram piece of commercialized all kinds of separation membrane bases；
Fig. 4 is poly- levodopa and Fe in embodiment 33+Act on the optical microscope photograph and embodiment of the complex formed
The scanning electron microscope diagram piece of the water-oil separationg film prepared in 3；
Fig. 5 is that water-oil separationg film carries out oil preventing performance test chart in water in effect example 1；
Fig. 6 is that water-oil separationg film carries out oil-water separation lab diagram in effect example 2.
Specific embodiment
It is clearly and completely described below with reference to technical effect of the embodiment to design and generation of the invention, with
It is completely understood by the purpose of the present invention, feature and effect.Obviously, described embodiment is that a part of the invention is implemented
Example, rather than whole embodiments, based on the embodiment of the present invention, those skilled in the art is not before making the creative labor
Other embodiments obtained are put, the scope of protection of the invention is belonged to.
Embodiment 1
The present embodiment provides a kind of water-oil separationg films, are prepared according to the following steps:
(1) it prepares poly- levodopa: preparing levodopa (L-Dopa) aqueous solution of 1-2mg/mL, be added into solution
Alkali adjusts solution ph to 8.5, and stirring 24 hours at 80 DEG C can be obtained the water-soluble of water-soluble poly levodopa (PDopa)
Liquid.Reaction process is as follows:
(2) it prepares the solution containing poly- levodopa: being added into the aqueous solution of the poly- levodopa prepared a certain amount of
The salting liquid of poly- levodopa is made in sodium chloride, wherein the concentration of poly- levodopa is 1mg/mL, the concentration of sodium chloride is
0.5M；
Preparation contains the salting liquid of diallyl dimethyl ammoniumchloride (polycation), wherein diallyl dimethyl chlorine
The concentration for changing ammonium is 1mg/mL, and the concentration of sodium chloride is 0.5M.
(3) layer assembly method prepares water-oil separationg film: referring to Fig. 1, separation membrane base being immersed in preparation in step (2)
In salting liquid (i.e. in said polycation solution) containing diallyl dimethyl ammoniumchloride, then washes and be soaked in step (2)
In the solution (i.e. polyanion solution) containing poly- levodopa of middle preparation, take out separation membrane base washing, and circulation immersion in
Composite coating is formed in polycation and polyanion solution, circulation immersion 20 times, washes and dries up, and grease point is prepared
From film.
Fig. 2 is the scanning electron microscope diagram piece of water-oil separationg film manufactured in the present embodiment, wherein (a) indicates water-oil separating
The front scan electron microscope picture of film (b) indicates the section scanning electron microscope picture of water-oil separationg film.
By taking stainless (steel) wire substrate as an example, the separation membrane base of actual use includes but not separation membrane base in the present embodiment
It is limited to the commercialized all kinds of seperation films such as stainless (steel) wire, copper mesh, Teflon film, Fig. 3 is commercialized all kinds of separation membrane bases
Photo and scanning electron microscope diagram piece, wherein (a) indicates stainless (steel) wire photo, (b) and (c) indicates sweeping for different pore size copper mesh
Electron microscope picture is retouched, (d) indicates the scanning electron microscope diagram of Teflon film.
Embodiment 2
The present embodiment provides a kind of water-oil separationg films, are prepared according to the following steps:
(1) poly- levodopa is prepared: in the same manner as in Example 1.
(2) it prepares the solution containing poly- levodopa: a certain amount of chlorine is added into the poly- levodopa aqueous solution prepared
Change sodium, the salting liquid of poly- levodopa is made, wherein the concentration of poly- levodopa is 1~5mg/mL, the concentration of sodium chloride is 0~
2M；
Prepare positively charged diallyl dimethyl ammoniumchloride/kayexalate compound polyelectrolyte salt
Solution, wherein the concentration of compound polyelectrolyte is 1~5mg/mL, and the concentration of sodium chloride is 0~2M.
(3) layer assembly method prepares water-oil separationg film: separation membrane base is immersed in the polyelectrolyte prepared in step (2)
In the solution containing poly- levodopa prepared in the salting liquid and step (2) of compound, circulation immersion 50 times, washes and dries up,
Water-oil separationg film is prepared.
Embodiment 3
The present embodiment provides a kind of water-oil separationg films, are prepared according to the following steps:
(1) poly- levodopa is prepared: in the same manner as in Example 1.
(2) it prepares the solution containing poly- levodopa: being added into the poly- levodopa aqueous solution of 0.1~1.0mg/mL a certain amount of
Hydrochloric acid or sodium hydroxide, adjust its pH value be 2~12；
Trivalent iron salt is added into the above-mentioned solution containing poly- levodopa, so that Fe3+Content is 1~5mg/mL, is gathered
Levodopa/Fe3+Compound disperse system.
(3) separation membrane base is immersed in compound disperse system obtained in step (2), soaking time be 0.5~
For 24 hours, it washes and dries up, water-oil separationg film is prepared.
It, can be with divalent or trivalent metal ion because poly- levodopa contains bisphenol group, carboxyl and amino in the present embodiment
Chelating forms complex, poly- levodopa and Fe3+It acts in the optical microscope photograph such as Fig. 4 of the complex formed (a)
It is shown, in the scanning electron microscope diagram piece such as Fig. 4 of the water-oil separating membrane coat being finally prepared shown in (b).
Effect example 1
The water-oil separationg film that is prepared in Example 1 carries out oil preventing performance test in water, as a result as shown in figure 5, its
In (a) indicate displaing micro picture of the water-oil separationg film close to (1.), contact (2.) and when leaving (3., 4.) oil droplet in water phase；
(b) indicate water phase in dichloroethanes in the contact angle of water-oil separating film surface and water phase hexadecane in water-oil separating film surface
Contact angle；(c) indicate that hexadecane is in the layer of the contact angle size of water-oil separating film surface and the composite coating of assembling in water phase
Relational graph between number.Experimental result shows that water-oil separationg film prepared by the present invention is in water phase with the contact angle of superelevation
With ultralow slip angle, they have the performance of efficient oil resistant substance adherency pollution in water phase.
Effect example 2
The water-oil separationg film that is prepared in Example 1 carries out oil-water separation experiment, as a result as shown in fig. 6, its
In (a) indicate both ends open pipe the fixedly separated film in one end photo；(b) it indicates to topple over oil mixing with water from other end opening
The photo of object；(c) and (d) is the separation membrane base of not set composite coating of the present invention and the grease point in embodiment 1 respectively
Photo after being washed from film water；(e) indicate only under Gravity Separation in embodiment 1 water-oil separationg film oil-water separation photo.
As can be seen from the figure water-oil separationg film of the invention has efficient, high-throughput water-oil separating performance and good automatically cleaning is anti-
The characteristic of oil adherency washes the petroleum that can effectively remove adherency after carrying out water-oil separating, is conducive to be recycled.
Claims (11)
1. a kind of water-oil separationg film, which is characterized in that including separation membrane base and overlay on the separation membrane base at least one
Layer composite coating, the composite coating assembles with the second material by poly- levodopa and formed, second material for band just
Polyelectrolyte, positively charged compound polyelectrolyte, at least one of the material containing metal cation of electricity.
2. water-oil separationg film according to claim 1, which is characterized in that the positively charged polyelectrolyte includes polyene third
Any one of base amine, polyethyleneimine, diallyl dimethyl ammoniumchloride.
3. water-oil separationg film according to claim 1, which is characterized in that the positively charged compound polyelectrolyte includes
Polyallylamine/polyacrylic acid composite, polyethyleneimine/polyacrylic acid composite, diallyl dimethyl ammoniumchloride/poly-
Any one of sodium styrene sulfonate.
4. water-oil separationg film according to claim 1, which is characterized in that the metal cation include copper, iron, titanium, manganese,
The corresponding cation of at least one of cobalt, nickel, zinc, aluminium metal.
5. water-oil separationg film according to claim 1-4, which is characterized in that the separation membrane base includes stainless
Any one of steel mesh, copper mesh, Teflon film.
6. the preparation method of the described in any item water-oil separationg films of claim 1-5, which comprises the following steps:
(1) separation membrane base is taken to be soaked in the solution containing the second material, second material be positively charged polyelectrolyte and/
Or positively charged compound polyelectrolyte；
(2) it after taking out and cleaning, is soaked in the solution containing poly- levodopa；
(3) it takes out, wash and dry.
7. the preparation method of water-oil separationg film according to claim 6, which is characterized in that circulation carries out step (1) and (2)
At least once.
8. the preparation method of water-oil separationg film according to claim 6 or 7, which is characterized in that contain the second material in step (1)
Salt is added in the solution and/or step (2) of material in solution containing poly- levodopa.
9. the preparation method of water-oil separationg film according to claim 8, which is characterized in that the salt is sodium salt or sylvite.
10. the preparation method of the described in any item water-oil separationg films of claim 1-5, which comprises the following steps:
(1) it is 2~12 to be formed containing poly- levodopa that pH adjusting agent is added in the aqueous solution of poly- levodopa and adjusts pH value
Solution；
(2) the second material is added in the solution containing poly- levodopa and forms poly- levodopa/metal cation compound
Disperse system, second material contain metal cation；
(3) separation membrane base is soaked in the poly- levodopa/metal cation compound disperse system.
11. a kind of oil-water separation method, which is characterized in that use the described in any item water-oil separationg films of claim 1-5.
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| CN201910484693.9A CN110314560A (en) | 2019-06-05 | 2019-06-05 | A kind of water-oil separationg film and preparation method thereof and a kind of oil-water separation method |
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| CN201910484693.9A CN110314560A (en) | 2019-06-05 | 2019-06-05 | A kind of water-oil separationg film and preparation method thereof and a kind of oil-water separation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115873429A (en) * | 2022-11-24 | 2023-03-31 | 深圳市宏日嘉净化设备科技有限公司 | Super-hydrophilic titanium phosphate oil-water separation coating and preparation method thereof |
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| CN107486021A (en) * | 2017-09-26 | 2017-12-19 | 南京理工大学 | Preparation method for the self assembly composite nanometer filtering film of water softening |
| CN109046034A (en) * | 2018-08-28 | 2018-12-21 | 浙江工业大学 | A kind of hydrophilic PVDF filter membrane and its application |
| CN109589646A (en) * | 2019-01-30 | 2019-04-09 | 青岛大学 | A kind of oil-water separation mesh film and preparation method thereof that high stable is metal oxide supported |
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| WO1998030318A2 (en) * | 1997-01-08 | 1998-07-16 | The Regents Of The University Of California | Compounds for producing nanoporous polymers, nanocomposite and membranes thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115873429A (en) * | 2022-11-24 | 2023-03-31 | 深圳市宏日嘉净化设备科技有限公司 | Super-hydrophilic titanium phosphate oil-water separation coating and preparation method thereof |
| CN115873429B (en) * | 2022-11-24 | 2023-09-29 | 深圳市宏日嘉净化设备科技有限公司 | Super-hydrophilic titanium phosphate oil-water separation coating and preparation method thereof |
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