CN106606934A - Polyurethane pervaporation recovered solvent membrane and preparation method thereof - Google Patents
Polyurethane pervaporation recovered solvent membrane and preparation method thereof Download PDFInfo
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- CN106606934A CN106606934A CN201611109629.5A CN201611109629A CN106606934A CN 106606934 A CN106606934 A CN 106606934A CN 201611109629 A CN201611109629 A CN 201611109629A CN 106606934 A CN106606934 A CN 106606934A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
- B01D61/362—Pervaporation
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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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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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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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/06—Working-up used lubricants to recover useful products ; Cleaning by ultrafiltration or osmosis
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Abstract
The invention discloses a polyurethane pervaporation recovered solvent membrane and a preparation method thereof. The polyurethane pervaporation recovered solvent membrane comprises a basement membrane and an active layer smeared to the basement membrane, wherein the active layer is a polyurethane membrane doped with TiO2, and the basement membrane is a polyvinylidene fluoride membrane. The polyvinylidene fluoride membrane in the polyurethane pervaporation recovered solvent membrane has high hydrophobic property and is a supporting body for the polyurethane pervaporation recovered solvent membrane; the TiO2 can be used for increasing a distance between polymer chains, so that the polyurethane pervaporation recovered solvent membrane has high permeation flux, and the polyurethane pervaporation recovered solvent membrane can be used for easily separating solvent from waste engine oil. In addition, the waste engine oil can be recovered only by the polyurethane pervaporation recovered solvent membrane, steps are simplified, periods are shortened, and cost is low.
Description
Technical field
The present invention relates to used oil field is reclaimed, more particularly to a kind of polyurethane infiltration evaporation recycling design film and its preparation
Method.
Background technology
Used oil one refers to that machine oil has been mixed into the metal of moisture, dust, other miscellaneous oil and component wears generation in use
The impurity such as powder, two refer to that machine oil gradually goes bad generates organic acid, colloid and asphaltic substances.The regeneration of used oil is exactly to use
The methods such as sedimentation, distillation, pickling, alkali cleaning, filtration remove the impurity in machine oil.
At present regenerating waste oil is comprised the following steps that：
1) precipitate：Waste oil is stood by sedimentation, impurity is declined and is separated.Sedimentation time is determined by oil and oil temperature.Oil temperature
Higher, viscosity is less, and the easier decline of impurity, sedimentation time are shorter；
2) distill：Distillation is to separate lower boiling gasoline, diesel oil etc., and the moisture in waste oil is thoroughly removed, and is protected
Holding regeneration machine oil has certain viscosity, has certain flash-point.What is steamed at 180 DEG C is gasoline, and 180～360 DEG C of fraction is bavin
Oil, what is stayed is machine oil；
3) pickling：Pickling is exactly the effect by concentrated sulphuric acid, makes the most of impurity precipitation separation in waste oil get off.Pickling
Concentrated sulphuric acid, the concentration of concentrated sulphuric acid will play flocculating agent, the layering of accelerating impurity more than 98%.5 points are stirred after acid adding
Clock, standing a period of time, occurs as soon as substantially layering, and upper strata is oily in yellow green, the impurity such as no black particle；
4) alkali neutralization：Sulfur when alkali cleaning this step is to remove the organic acid in used oil and neutralization pickling under residual
Acid.PH value 7 is measured with PH reagent paper by the coil neutralization of acid sludge, neutralization are removed after pickling with sodium hydroxide solution, needed during neutralization
Stirring.If fruit oil is neutral, at this moment machine oil should become limpid；
5) wash：The water-solubility impurities such as the acid in oil, alkali are washed off.Washing gondola water faucet is equably sprinkled water just toward in oil.
With oil mass almost just, the oil washed will precipitate an evening to watering amount, allow water fully to sink to the bottom；
6) bleaching earth adsorption：Principle is under the high temperature conditions, with active hargil by the impurity absorption in oil.First following water
Put net, oil is heated to into 130 DEG C then, put the active hargil for accounting for oil mass 8% or so into, stir five minutes.Bleaching earth adsorption
The speed of heating can not be too fast, and the too fast oil of heating can substantial amounts of foam overflow；
7) filter：The oil of high temperature after bleaching earth adsorption is used vacuum filtration while hot, oil is leached to come.Caught on a filter is exactly finished product
Oil, the whole production process for regenerating machine oil are just completed.Filter and industrially filtered with oil filter, domestic machine oil can be with 4～6 layers of silk fabric
Cloth is filtered 2～4 times repeatedly, that is, obtain qualified machine oil.
But above-mentioned used oil recovery method is cumbersome, and return period is longer, distillation in removal process, is needed, the category energy is close
Collection type, and acid adding is needed in removal process, adds alkali, the quality of meeting contaminated product to improve cost.
The content of the invention
In view of this, the present invention provides a kind of polyurethane infiltration evaporation recycling design film and preparation method thereof, the method letter
Single, return period is short, low cost.
The technical scheme is that what is be achieved in that：
A kind of polyurethane infiltration evaporation recycling design film, including counterdie and the active layer being applied on the counterdie；
The active layer is doping TiO2Polyurethane film；The counterdie is polyvinylidene fluoride film.
Preferably, the thickness of the active layer is 30～50 μm；The thickness of the counterdie is 180～200 μm.
Present invention also offers a kind of preparation method of above-mentioned polyurethane infiltration evaporation recycling design film, including following step
Suddenly：
A) constant temperature in round-bottomed flask is added to stir 18～30h Kynoar, N-Methyl pyrrolidone, Polyethylene Glycol,
Then filter pressing, degassing, knifing, drying are carried out, polyvinylidene fluoride film is obtained；
B) polyurethane is mixed homogeneously with tetrahydrofuran, obtains mixed liquor；
C) the mixed liquor doping TiO obtained to step b)2Nano sol, after mix homogeneously, filtration, deaeration are obtained
Casting solution；
D) casting solution that step c) is obtained is coated on the polyvinylidene fluoride film that step a) is obtained, drying is
Obtain polyurethane infiltration evaporation recycling design film.
Preferably, the mean molecule quantity of the Polyethylene Glycol is 2000.
Preferably, Kynoar described in step a), the N-Methyl pyrrolidone, the mass ratio of the Polyethylene Glycol
For (6～7):(40～50)：(0.8～1.5).
Preferably, the temperature of the stirring of constant temperature described in step a) is 45～55 DEG C.
Preferably, polyurethane described in step b) and the mass ratio of the tetrahydrofuran are 1：(6～10).
Preferably, the TiO2The preparation scheme of Nano sol is：Under agitation to the first N-Methyl pyrrolidone
In, glacial acetic acid is sequentially added with positive butyl titanate；Concentrated hydrochloric acid and the second N-Methyl pyrrolidone are added after 10～20min of stirring
Mixed liquor, stirring 10～15h after, add acetic anhydride in system, be further continued for 10～15h of stirring, obtain final product TiO2Nanometer is molten
Glue.
Preferably, the aperture of the copper mesh for adopting is filtered in step c) for 250～350 mesh.
Preferably, the polyurethane and the TiO2The mass ratio of Nano sol is (8～12)：(2.5～3.5).
The invention provides a kind of polyurethane infiltration evaporation recycling design film and preparation method thereof, the polyurethane infiltration evaporation
Recycling design film includes counterdie and the active layer being applied on the counterdie；Active layer is doping TiO2Polyurethane film；Counterdie
For polyvinylidene fluoride film.In the present invention, polyvinylidene fluoride film has stronger hydrophobic performance, is that the recovery of polyurethane infiltration evaporation is molten
The supporter of agent film；TiO2The distance between polymer chain and chain can be increased so that polyurethane infiltration evaporation recycling design film
With high permeation flux so that polyurethane infiltration evaporation recycling design film can easily by the solvent in used oil point
Separate out and.In addition, the present invention only needs polyurethane infiltration evaporation recycling design film just reclaim used oil, step is simplified, contracted
Short cycle, and low cost.
Specific embodiment
The invention discloses a kind of polyurethane infiltration evaporation recycling design film and preparation method thereof, those skilled in the art can
To use for reference present disclosure, technological parameter realization is suitably modified.Specifically, the similar replacement and change are to this
It is it will be apparent that they are considered as being included in the present invention for art personnel.The method of the present invention and reference are
It is described by preferred embodiment, related personnel substantially can be in without departing from present invention, spirit and scope to herein
Described methods and applications are modified or suitably change and combine, and realize and apply the technology of the present invention.
A kind of polyurethane infiltration evaporation recycling design film that the present invention is provided, including counterdie and be applied on the counterdie
Active layer；
Active layer is doping TiO2Polyurethane film；Counterdie is polyvinylidene fluoride film.
In above-mentioned technical proposal, polyvinylidene fluoride film has stronger hydrophobic performance, is that the recovery of polyurethane infiltration evaporation is molten
The supporter of agent film；TiO2The distance between polymer chain and chain can be increased so that polyurethane infiltration evaporation recycling design film
With high permeation flux such that it is able to allow polyurethane infiltration evaporation recycling design film easily by used oil
Solvent separate.In addition, the present invention only needs polyurethane infiltration evaporation recycling design film just reclaim used oil, simplify
Step, shortens cycle, and low cost.
In an embodiment of the present invention, the thickness of active layer is 30～50 μm；In other embodiments, the thickness of active layer
For 35～45 μm；In a further embodiment, the thickness of active layer is 38～42 μm.
In an embodiment of the present invention, the thickness of counterdie is 180～200 μm；In other embodiments, the thickness of counterdie is
185～195 μm；In a further embodiment, the thickness of counterdie is 188～192 μm.
Present invention also offers a kind of preparation method of polyurethane infiltration evaporation recycling design film, comprises the following steps：
A) constant temperature in round-bottomed flask is added to stir 18～30h Kynoar, N-Methyl pyrrolidone, Polyethylene Glycol,
Then filter pressing, degassing, knifing, drying are carried out, polyvinylidene fluoride film is obtained；
B) polyurethane is mixed homogeneously with tetrahydrofuran, obtains mixed liquor；
C) the casting solution doping TiO obtained to step b)2Nano sol, after mix homogeneously, filtration, deaeration obtain casting film
Liquid；
D) casting solution that step c) is obtained is coated on the polyvinylidene fluoride film that step a) is obtained, is drying to obtain polyurethane
Infiltration evaporation recycling design film.
The polyurethane infiltration evaporation recycling design film that above-mentioned technical proposal is prepared, with high permeation flux so that
Solvent in used oil easily can be separated by polyurethane infiltration evaporation recycling design film.
During Kynoar, N-Methyl pyrrolidone, Polyethylene Glycol add round-bottomed flask, constant temperature stirs 18～30h, then
Filter pressing, degassing, knifing, drying are carried out, polyvinylidene fluoride film is obtained.
In an embodiment of the present invention, Kynoar, N-Methyl pyrrolidone, Polyethylene Glycol mass ratio for (6～
7):(40～50)：(0.8～1.5)；The present invention has no spy to the source of Kynoar, N-Methyl pyrrolidone, Polyethylene Glycol
It is different to require, can be general commercially available.
In an embodiment of the present invention, the mean molecule quantity of Polyethylene Glycol is 2000.
In an embodiment of the present invention, the temperature of constant temperature stirring is 45～55 DEG C；In other embodiments, constant temperature is stirred
Temperature is 48～52 DEG C.
In an embodiment of the present invention, the substrate of knifing is non-woven fabrics or glass, be put into after knifing 30 in deionized water～
60h carries out split-phase.
In an embodiment of the present invention, the thickness of the polyvinylidene fluoride film being dried to obtain is 180～200 μm；In other realities
Apply in example, the thickness of counterdie is 185～195 μm；In a further embodiment, the thickness of counterdie is 188～192 μm.
Polyurethane is mixed homogeneously with tetrahydrofuran, obtains mixed liquor；In an embodiment of the present invention, polyurethane and tetrahydrochysene furan
The mass ratio muttered is 1：(6～10)；In other embodiments, polyurethane and the mass ratio of the tetrahydrofuran are 1：(7.5～
8.5)；Source of the present invention to polyurethane with tetrahydrofuran has no particular/special requirement, can be general commercially available.
After obtaining mixed liquor, adulterate TiO2Nano sol, after mix homogeneously, filtration, deaeration obtain casting solution.
In an embodiment of the present invention, TiO2The preparation method of Nano sol is under agitation to a N- methyl pyrroles
In pyrrolidone, glacial acetic acid is sequentially added with positive butyl titanate；Concentrated hydrochloric acid and the 2nd N- methyl pyrroles are added after 10～20min of stirring
The mixed liquor of pyrrolidone, after 10～15h of stirring, adds acetic anhydride in system, is further continued for 10～15h of stirring, obtains final product TiO2
Nano sol.The present invention to N-Methyl pyrrolidone, glacial acetic acid, positive butyl titanate, concentrated hydrochloric acid, acetic anhydride source have no it is special
Require, can be general commercially available.
In an embodiment of the present invention, the mass concentration of concentrated hydrochloric acid is 20～35%.
In an embodiment of the present invention, the first N-Methyl pyrrolidone, glacial acetic acid, positive butyl titanate, concentrated hydrochloric acid, the 2nd N-
The volume ratio of methyl pyrrolidone acetic anhydride is (8～12)：(8～12)：(8～12)：(1～3)：(8～12)：(8～12).
In an embodiment of the present invention, the aperture of the copper mesh for adopting is filtered for 250～350 mesh；In other embodiments, copper
The aperture of net is 280～320 mesh.
After obtaining casting solution, casting solution is coated on polyvinylidene fluoride film, be drying to obtain polyurethane infiltration evaporation and reclaim molten
Agent film.
In an embodiment of the present invention, baking temperature is 35～45 DEG C.
In order to further illustrate the present invention, molten is reclaimed to the polyurethane infiltration evaporation that the present invention is provided with reference to embodiments
Agent film and preparation method thereof is described in detail.
In following examples, raw material used is commercially available.
Embodiment 1
76.4721g Kynoar, 514.0868g N-Methyl pyrrolidone, 11.7640g Macrogol 2000s are put
50 DEG C of waters bath with thermostatic control in entering round-bottomed flask are stirred 24 hours, then carry out filter pressing, degassing；Scraped on non-woven fabrics using knifing machine
Film, the film scraped is immersed two days in deionized water, oven drying is put into, is obtained the polyvinylidene fluoride film that thickness is 180 μm；
2g polyurethane is put into magnetic agitation 12h in conical flask with 16g tetrahydrofurans, obtains mixed liquor；
10mL N-Methyl pyrrolidone is pipetted in 100mL conical flasks, under violent stirring, successively the ice of 10mL
Acetic acid is slowly added to the positive butyl titanate of 10mL, after 15min to be mixed, 2mL concentrated hydrochloric acid and 10ml N- first is added in system
The mixed liquor of base ketopyrrolidine；At room temperature, continue strong agitation 12h, then plus 10mL acetic anhydride in system, be further continued for stirring
12h is mixed, TiO has been obtained2Nano sol；
0.6g TiO are added in mixed liquor2Nano sol, mix homogeneously are filtered with the copper mesh of 300 mesh, stand one day with
Removing bubble, obtains casting solution；
Casting solution is coated on Kynoar counterdie, is dried in being placed in the baking oven of 40 DEG C of constant temperature, after being dried
The thickness of the active layer that casting solution is formed is 40 μm, obtains polyurethane infiltration evaporation recycling design film.
Embodiment 1 is obtained into polyurethane infiltration evaporation recycling design film and is cut into 4cm × 4cm, and be put into the useless of 20mL black
In lubricating oil, after 2h, waste lubricating oil becomes colourless.
Embodiment 2
88.23g Kynoar, 588.2g N-Methyl pyrrolidone, 11.7640g Macrogol 2000s are put into into round bottom
55 DEG C of waters bath with thermostatic control in flask are stirred 18 hours, then carry out filter pressing, degassing；Using knifing machine on non-woven fabrics knifing, will scrape
Two days in good film immersion deionized water, oven drying is put into, the polyvinylidene fluoride film that thickness is 200 μm is obtained；
2g polyurethane is put into magnetic agitation 15h in conical flask with 12g tetrahydrofurans, obtains mixed liquor；
8mL N-Methyl pyrrolidone is pipetted in 100mL conical flasks, under violent stirring, successively the ice second of 8mL
Acid is slowly added to the positive butyl titanate of 8mL, after 10min to be mixed, 1mL concentrated hydrochloric acid and 8ml N- methyl pyrroles is added in system
The mixed liquor of pyrrolidone；At room temperature, continue strong agitation 10h, then plus 8mL acetic anhydride in system, be further continued for stirring
10h, has obtained TiO2Nano sol；
0.625g TiO are added in mixed liquor2Nano sol, mix homogeneously are filtered with the copper mesh of 250 mesh, stand one day
To remove bubble, casting solution is obtained；
Casting solution is coated on Kynoar counterdie, is dried in being placed in the baking oven of 38 DEG C of constant temperature, after being dried
The thickness of the active layer that casting solution is formed is 30 μm, obtains polyurethane infiltration evaporation recycling design film.
Embodiment 2 is obtained into polyurethane infiltration evaporation recycling design film and is cut into 4cm × 4cm, and be put into the useless of 20mL black
In lubricating oil, after 1h, waste lubricating oil becomes colourless.
Embodiment 3
54.8987g Kynoar, 392.1333g N-Methyl pyrrolidone, 11.7640g Macrogol 2000s are put
45 DEG C of waters bath with thermostatic control in entering round-bottomed flask are stirred 30 hours, then carry out filter pressing, degassing；Scraped on non-woven fabrics using knifing machine
Film, the film scraped is immersed two days in deionized water, oven drying is put into, is obtained the polyvinylidene fluoride film that thickness is 185 μm；
2g polyurethane is put into magnetic agitation 10h in conical flask with 14g tetrahydrofurans, obtains mixed liquor；
12mL N-Methyl pyrrolidone is pipetted in 100mL conical flasks, under violent stirring, successively the ice of 12mL
Acetic acid is slowly added to the positive butyl titanate of 12mL, after 20min to be mixed, 3mL concentrated hydrochloric acid and 12ml N- first is added in system
The mixed liquor of base ketopyrrolidine；At room temperature, continue strong agitation 15h, then plus 12mL acetic anhydride in system, be further continued for stirring
15h is mixed, TiO has been obtained2Nano sol；
0.622g TiO are added in mixed liquor2Nano sol, mix homogeneously are filtered with the copper mesh of 330 mesh, stand one day
To remove bubble, casting solution is obtained；
Casting solution is coated on Kynoar counterdie, is dried in being placed in the baking oven of 42 DEG C of constant temperature, after being dried
The thickness of the active layer that casting solution is formed is 50 μm, obtains polyurethane infiltration evaporation recycling design film.
Embodiment 3 is obtained into polyurethane infiltration evaporation recycling design film and is cut into 4cm × 4cm, and be put into the useless of 20mL black
In lubricating oil, after 3h, waste lubricating oil becomes colourless.
Embodiment 4
63.7217g Kynoar, 441.15g N-Methyl pyrrolidone, 11.7640g Macrogol 2000s are put into
48 DEG C of waters bath with thermostatic control in round-bottomed flask are stirred 21 hours, then carry out filter pressing, degassing；Using knifing machine on non-woven fabrics knifing,
The film scraped is immersed two days in deionized water, oven drying is put into, is obtained the polyvinylidene fluoride film that thickness is 195 μm；
2g polyurethane is put into magnetic agitation 11h in conical flask with 20g tetrahydrofurans, obtains mixed liquor；
10mL N-Methyl pyrrolidone is pipetted in 100mL conical flasks, under violent stirring, successively the ice second of 8mL
Acid is slowly added to the positive butyl titanate of 11mL, after 12min to be mixed, 1.5mL concentrated hydrochloric acid and 9ml N- first is added in system
The mixed liquor of base ketopyrrolidine；At room temperature, continue strong agitation 13h, then plus 10mL acetic anhydride in system, be further continued for stirring
14h is mixed, TiO has been obtained2Nano sol；
0.582g TiO are added in mixed liquor2Nano sol, mix homogeneously are filtered with the copper mesh of 350 mesh, stand one day
To remove bubble, casting solution is obtained；
Casting solution is coated on Kynoar counterdie, is dried in being placed in the baking oven of 45 DEG C of constant temperature, after being dried
The thickness of the active layer that casting solution is formed is 45 μm, obtains polyurethane infiltration evaporation recycling design film.
Embodiment 4 is obtained into polyurethane infiltration evaporation recycling design film and is cut into 4cm × 4cm, and be put into the useless of 20mL black
In lubricating oil, after 2.5h, black waste lubricating oil becomes colourless.
Embodiment 5
61.5348g Kynoar, 434.361g N-Methyl pyrrolidone, 11.7640g Macrogol 2000s are put into
52 DEG C of waters bath with thermostatic control in round-bottomed flask are stirred 27 hours, then carry out filter pressing, degassing；Using knifing machine on non-woven fabrics knifing,
The film scraped is immersed two days in deionized water, oven drying is put into, is obtained the polyvinylidene fluoride film that thickness is 190 μm；
2g polyurethane is put into magnetic agitation 14h in conical flask with 18g tetrahydrofurans, obtains mixed liquor；
11mL N-Methyl pyrrolidone is pipetted in 100mL conical flasks, under violent stirring, successively the ice of 10mL
Acetic acid is slowly added to the positive butyl titanate of 12mL, after 18min to be mixed, 2.5mL concentrated hydrochloric acid and 10ml N- is added in system
The mixed liquor of methyl pyrrolidone；At room temperature, continue strong agitation 11h, then plus 8mL acetic anhydride in system, be further continued for
Stirring 12h, has obtained TiO2Nano sol；
0.583g TiO are added in mixed liquor2Nano sol, mix homogeneously are filtered with the copper mesh of 280 mesh, stand one day
To remove bubble, casting solution is obtained；
Casting solution is coated on Kynoar counterdie, is dried in being placed in the baking oven of 35 DEG C of constant temperature, after being dried
The thickness of the active layer that casting solution is formed is 35 μm, obtains polyurethane infiltration evaporation recycling design film.
Embodiment 5 is obtained into polyurethane infiltration evaporation recycling design film and is cut into 4cm × 4cm, and be put into the useless of 20mL black
In lubricating oil, after 1.5h, waste lubricating oil becomes colourless.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (10)
1. a kind of polyurethane infiltration evaporation recycling design film, it is characterised in that including counterdie and the work being applied on the counterdie
Property layer；
The active layer is doping TiO2Polyurethane film；The counterdie is polyvinylidene fluoride film.
2. polyurethane infiltration evaporation recycling design film as claimed in claim 1, it is characterised in that the thickness of the active layer is
30～50 μm；The thickness of the counterdie is 180～200 μm.
3. a kind of preparation method of polyurethane infiltration evaporation recycling design film as claimed in claim 1 or 2, it is characterised in that
Comprise the following steps：
A) constant temperature in round-bottomed flask is added to stir 18～30h Kynoar, N-Methyl pyrrolidone, Polyethylene Glycol, then
Filter pressing, degassing, knifing, drying are carried out, polyvinylidene fluoride film is obtained；
B) polyurethane is mixed homogeneously with tetrahydrofuran, obtains mixed liquor；
C) the mixed liquor doping TiO obtained to step b)2Nano sol, after mix homogeneously, filtration, deaeration obtain casting film
Liquid；
D) casting solution that step c) is obtained is coated on the polyvinylidene fluoride film that step a) is obtained, is drying to obtain poly-
Urethane infiltration evaporation recycling design film.
4. preparation method as claimed in claim 3, it is characterised in that the mean molecule quantity of the Polyethylene Glycol is 2000.
5. preparation method as claimed in claim 3, it is characterised in that Kynoar described in step a), the N- methyl
Ketopyrrolidine, the mass ratio of the Polyethylene Glycol are (6～7):(40～50)：(0.8～1.5).
6. preparation method as claimed in claim 3, it is characterised in that the temperature of the stirring of constant temperature described in step a) is 45～55
℃。
7. preparation method as claimed in claim 3, it is characterised in that polyurethane described in step b) and the tetrahydrofuran
Mass ratio is 1：(6～10).
8. preparation method as claimed in claim 3, it is characterised in that the TiO2The preparation scheme of Nano sol is：In stirring
Under the conditions of in the first N-Methyl pyrrolidone, sequentially add glacial acetic acid with positive butyl titanate；Add after 10～20min of stirring
The mixed liquor of concentrated hydrochloric acid and the second N-Methyl pyrrolidone, after 10～15h of stirring, adds acetic anhydride in system, is further continued for
10～15h of stirring, obtains final product TiO2Nano sol.
9. preparation method as claimed in claim 3, it is characterised in that the aperture of the copper mesh for adopting is filtered in step c) for 250
～350 mesh.
10. preparation method as claimed in claim 3, it is characterised in that the polyurethane and the TiO2The quality of Nano sol
Than for (8～12)：(2.5～3.5).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020087761A1 (en) * | 2018-10-31 | 2020-05-07 | 中国石油大学(华东) | Polyurethanee/polyvinylidene fluoride composite film for extracting organic sulfide from naphtha and preparation method therefor |
| CN115305143A (en) * | 2022-09-14 | 2022-11-08 | 重庆中吉达环保科技有限公司 | Method for refining waste mineral oil |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401700A (en) * | 2002-10-17 | 2003-03-12 | 天津工业大学 | Polyurethane/inorganic particle blended composite film and mfg. method thereof |
| CN103084077A (en) * | 2013-01-27 | 2013-05-08 | 北京工商大学 | Preparation method of polyurethane pervaporation phenol/water separating membrane compounded by inorganic particles |
| CN103752182A (en) * | 2014-01-20 | 2014-04-30 | 中国石油大学(华东) | Ethyl cellulose pervaporation gasoline desulfurization film and preparation method thereof |
| CN103816813A (en) * | 2014-03-04 | 2014-05-28 | 中国石油大学(华东) | Ethyecellulose pervaporation gasoline desulfurization membrane doped with MWCNTs (multiwalled carbon nanotubes) and preparing method thereof |
| CN104151585A (en) * | 2014-08-12 | 2014-11-19 | 娄尤来 | Preparation method of hydrophobic nano-grade calcium carbonate filled polyurethane pervaporation membrane |
| CN104624062A (en) * | 2015-01-23 | 2015-05-20 | 中国石油大学(华东) | Polydimethylsiloxane/polyvinylidene fluoride composite film and preparation method thereof |
| CN104725596A (en) * | 2015-03-26 | 2015-06-24 | 浙江工商大学 | Nano-silver/carbon nano tube/polyurethane hybrid membrane and preparation method thereof |
-
2016
- 2016-12-02 CN CN201611109629.5A patent/CN106606934A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401700A (en) * | 2002-10-17 | 2003-03-12 | 天津工业大学 | Polyurethane/inorganic particle blended composite film and mfg. method thereof |
| CN103084077A (en) * | 2013-01-27 | 2013-05-08 | 北京工商大学 | Preparation method of polyurethane pervaporation phenol/water separating membrane compounded by inorganic particles |
| CN103752182A (en) * | 2014-01-20 | 2014-04-30 | 中国石油大学(华东) | Ethyl cellulose pervaporation gasoline desulfurization film and preparation method thereof |
| CN103816813A (en) * | 2014-03-04 | 2014-05-28 | 中国石油大学(华东) | Ethyecellulose pervaporation gasoline desulfurization membrane doped with MWCNTs (multiwalled carbon nanotubes) and preparing method thereof |
| CN104151585A (en) * | 2014-08-12 | 2014-11-19 | 娄尤来 | Preparation method of hydrophobic nano-grade calcium carbonate filled polyurethane pervaporation membrane |
| CN104624062A (en) * | 2015-01-23 | 2015-05-20 | 中国石油大学(华东) | Polydimethylsiloxane/polyvinylidene fluoride composite film and preparation method thereof |
| CN104725596A (en) * | 2015-03-26 | 2015-06-24 | 浙江工商大学 | Nano-silver/carbon nano tube/polyurethane hybrid membrane and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| HOU YINGFEI 等: "Gasoline desulfurization by a TiO2-filled ethyl cellulose pervaporation membrane", 《JOURNAL OF APPLIED POLYMER SCIENCE》 * |
| 石丽: "聚氨酯/无机氧化物共混膜的制备及其氧氮渗透性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020087761A1 (en) * | 2018-10-31 | 2020-05-07 | 中国石油大学(华东) | Polyurethanee/polyvinylidene fluoride composite film for extracting organic sulfide from naphtha and preparation method therefor |
| US11458438B2 (en) * | 2018-10-31 | 2022-10-04 | China University Of Petroleum(East China) | Polyurethane/polyvinylidene fluoride composite membrane for extracting organic sulfide from naphtha and preparation method therefor |
| CN115305143A (en) * | 2022-09-14 | 2022-11-08 | 重庆中吉达环保科技有限公司 | Method for refining waste mineral oil |
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