CN104815462B - Super-hydrophobic stub and preparation method thereof and purposes - Google Patents
Super-hydrophobic stub and preparation method thereof and purposes Download PDFInfo
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- CN104815462B CN104815462B CN201510163857.XA CN201510163857A CN104815462B CN 104815462 B CN104815462 B CN 104815462B CN 201510163857 A CN201510163857 A CN 201510163857A CN 104815462 B CN104815462 B CN 104815462B
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Abstract
The invention provides a kind of super-hydrophobic stub, belong to field of functional materials；By hydrophobic agents, discarded stub being processed and is dried, obtain super-hydrophobic stub, this stub reaches 156 ° to the contact angle of water, and roll angle is less than 3 °, and the contact angle to oil is 0 °；Described super-hydrophobic stub can apply to oil hydrosol separate, it is possible to having successfully been isolated multiple oil hydrosol, separation efficiency is up to more than 98%, this material use after through simply cleaning reusable edible.And this preparation technology is simple, operability is relatively strong, is easily achieved large-scale application in oil spill field, and can reach the effect of twice laid.
Description
Technical field
The invention belongs to oil-water separation field, the most super-hydrophobic stub and preparation method thereof and purposes.
Background technology
Along with the fast development of petroleum industry, oil spill events takes place frequently simultaneously, oil water mixture, and particularly oil hydrosol endangers
Natural environment and human health.Therefore, study hotspot in recent years is become for this type of processing method polluted.Can oil suction and
The material not absorbed water becomes the focus being concerned.Wherein, due to the wettability that it is special, super-hydrophobic super-oleophylic material is only with it
Special hydrophobicity, good oil-water separation efficiency are studied by numerous research teams.At super-hydrophobic super-oleophylic material of today
Research field, the grapheme foam of three-dimensional, CNT foam, silica aerogel etc. are with its higher oil suction ratio, oil suction efficiency
Become study hotspot.
Article Superhydrophobic and Superoleophilic PVDF Membranes for Effective Separation of
Water-in-OilEmulsions with High Flux (a kind of super-hydrophobic super-oleophylic that can be efficiently applied to water-in-oil emulsion separation
Polyvinylidene difluoride film), Advance Materials, 2013,14:2071-2076, disclose a kind of polyvinylidene difluoride film,
This material is by being dispersed in methylpyrrolidone solution by Kynoar grain dissolution, then adds ammonia in this solution
Water, is subsequently adding water-bath in the matrix of politef and prepares polyvinylidene difluoride film.This have microcellular structure
Thin-film material can successfully carry out oil hydrosol separating experiment, and has higher flux, but owing to preparing material condition
Harshness, relatively costly, and need high-temperature process to be not suitable for use of large-scale production, it is impossible to divide for large-scale oil hydrosol
From.
Summary of the invention
For Shortcomings in prior art, the invention provides a kind of super-hydrophobic stub, using discarded stub is matrix, leaching
In excess of imports hydrophobic sol, obtaining super-hydrophobic stub, preparation method is simple, low cost, can be used for extensive oil hydrosol and separates.
The present invention realizes above-mentioned technical purpose by techniques below means.
The preparation method of a kind of super-hydrophobic stub, comprises the steps:
S1, discarded stub is submerged initially in water ultrasonic, then immerses organic solvent for ultrasonic miscible with water, cleanly dried
Stub；
S2, hexadecyl trichlorosilane or octadecyl trichlorosilane alkane are dissolved in non-polar organic solvent hydrophobic sol, by S1
The stub of described cleaning immerses in described hydrophobic sol, uses described non-polar organic solvent to wash, by gained stub at 70～90 DEG C
Lower dry, cooling, obtain super-hydrophobic stub.
Further, one or more during the organic solvent described in S1 is methanol, ethanol, acetone.
In such scheme, the non-polar organic solvent described in S2 is normal hexane or pentane.
In such scheme, the hexadecyl trichlorosilane described in S2 or octadecyl trichlorosilane alkane quality in described hydrophobic sol
Mark is 1%～4%.
In such scheme, the time that the clean stub described in S2 immerses in described hydrophobic sol is at least 1min, uses described
The time of non-polar organic solvent washing is at least 10min.
In such scheme, the stub described in S2 is dried at 80 DEG C.
Present invention additionally comprises the super-hydrophobic stub obtained by the preparation method of super-hydrophobic stub, described super-hydrophobic stub is to water
Static contact angle is 156 °, and roll angle is less than 3 °, and the contact angle to organic solvent immiscible with water or oils is 0 °.
The purposes that super-hydrophobic stub of the present invention separates as oil hydrosol.
Beneficial effects of the present invention:
The preparation method of super-hydrophobic stub of the present invention, the method uses raw material simplicity to be easy to get, low cost, preparation method letter
Single, oil-water separation is good, through simply cleaning reusable edible after use, can be mass-produced and on a large scale
Oil hydrosol separates.
Accompanying drawing explanation
Fig. 1 is the present invention super-hydrophobic stub contact angle to water.
Fig. 2 is the super-hydrophobic stub of the present invention contact angle to hexadecane.
Fig. 3 is the high power Electronic Speculum figure of super-hydrophobic stub of the present invention.
Fig. 4 is the super-hydrophobic stub of the present invention absorption situation map to water and hexadecane.
Fig. 5 is super-hydrophobic stub emulsion separation graph of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings and specific embodiment the present invention is further illustrated, but protection scope of the present invention is not limited to
This.
Super-hydrophobic stub of the present invention is used for oil-water separation, and oil is organic solvent immiscible with water or oil based solvent, such as two
Chloromethanes, chloroform, hexadecane, toluene, isobutyltrimethylmethane., paraffin etc..
Embodiment 1
1, the preparation of super-hydrophobic stub: discarded stub is immersed in deionized water and takes out after ultrasonic 30min, immerse dehydrated alcohol
In ultrasonic 30min, take out stub constant pressure and dry 2h at 60 DEG C obtain clean stub；Preparation mass fraction is the hexadecane of 1%
The hexane solution 20mL of base trichlorosilane, takes out after clean stub is immersed 2min to immerse and soaks 30 in normal hexane
Min, washes the unreacted hexadecyl trichlorosilane of remained on surface off, and taking-up stub is put into and is dried 1h in baking oven at 80 DEG C,
Super-hydrophobic stub is obtained after natural cooling.
As shown in Figure 1, Figure 2 for stub super-hydrophobic described in the present embodiment to water and the contact angle to hexadecane, illustrate of the present invention
Super-hydrophobic stub has oil properties hydrophobic, close.
The high power Electronic Speculum figure of super-hydrophobic stub as shown in Figure 3 shows that stub surface covers one layer of hydrophobic membrane.
Such as Fig. 4, the stub left side be water, the right be hexadecane, water droplet is on stub surface, and hexadecane is inhaled in stub, table
Bright super-hydrophobic stub hydrophobic oleophilic oil of the present invention.
The preparation of oil hydrosol: add 0.5g Span 80, ultrasonic disperse with 90mL toluene after being mixed by 10mL deionized water
2h, is uniformly dispersed, and obtains oil hydrosol.
Super-hydrophobic stub is placed in the centre position clamping of glass separation, pours the oil hydrosol obtained into glass separation upper strata,
It is observed that oil hydrosol is become the solution of clarification behind bottom through super-hydrophobic stub from separator overhead stream from milky, as
Shown in Fig. 5, oil hydrosol separation efficiency reaches 98%.
Embodiment 2
1, the preparation of super-hydrophobic stub: immersed in deionized water by discarded stub and take out after ultrasonic 30min, immerses in acetone super
Sound 30min, takes out stub constant pressure and dry 2h at 60 DEG C and obtains clean stub；The octadecyl trichlorosilane alkane of preparation 2% is just
Pentane solution 20mL, takes out after clean stub is immersed 5min to immerse and soaks 30min in pentane, wash surface off
The unreacted octadecyl trichlorosilane alkane of residual, taking-up stub is put into and is dried 1.5h in baking oven at 70 DEG C, obtains after natural cooling
Super-hydrophobic stub.
The preparation of oil hydrosol: addition 0.5g Span 80 after 10mL deionized water is mixed with 90mL hexadecane, ultrasonic point
Dissipate 2h, be uniformly dispersed, obtain oil hydrosol.
Super-hydrophobic stub is placed in the centre position clamping of glass separation, pours the oil hydrosol obtained into glass separation upper strata,
It is observed that oil hydrosol is become the solution of clarification, oil behind bottom through super-hydrophobic stub from separator overhead stream from milky
Aqueous emulsion separation efficiency reaches 98%.
Embodiment 3
1, the preparation of super-hydrophobic stub: immersed in deionized water by discarded stub and take out after ultrasonic 30min, immerses in methanol super
Sound 30min, takes out stub constant pressure and dry 2h at 60 DEG C and obtains clean stub；The hexadecyl trichlorosilane of preparation 4% is just
Pentane solution 20mL, takes out after clean stub is immersed 5min to immerse and soaks 30min in pentane, wash surface off
The unreacted hexadecyl trichlorosilane of residual, taking-up stub is put into and is dried 40min in baking oven at 90 DEG C, after natural cooling
Obtain super-hydrophobic stub.
The preparation of oil hydrosol: addition 0.5g Span 80 after 10mL deionized water is mixed with 90mL isobutyltrimethylmethane., ultrasonic point
Dissipate 2h, be uniformly dispersed, obtain oil hydrosol.
Super-hydrophobic stub is placed in the centre position clamping of glass separation, pours the oil hydrosol obtained into glass separation upper strata,
It is observed that oil hydrosol is become the solution of clarification, oil behind bottom through super-hydrophobic stub from separator overhead stream from milky
Aqueous emulsion separation efficiency reaches 98%.
Described embodiment be the present invention preferred embodiment, but the present invention is not limited to above-mentioned embodiment, without departing substantially from this
In the case of the flesh and blood of invention, any conspicuously improved, replacement or modification that those skilled in the art can make are equal
Belong to protection scope of the present invention.
Claims (7)
1. the preparation method of a super-hydrophobic stub, it is characterised in that comprise the steps:
S1, discarded stub is submerged initially in water ultrasonic, then immerses organic solvent for ultrasonic miscible with water, cleanly dried
Stub；
S2, hexadecyl trichlorosilane or octadecyl trichlorosilane alkane are dissolved in non-polar organic solvent hydrophobic sol, by S1
The stub of described cleaning immerses in described hydrophobic sol, uses described non-polar organic solvent to wash, by gained stub at 70～90 DEG C
Lower dry, cooling, obtain super-hydrophobic stub；
Hexadecyl trichlorosilane or octadecyl trichlorosilane alkane mass fraction in described hydrophobic sol described in S2 are 1%～4%.
The preparation method of super-hydrophobic stub the most as claimed in claim 1, it is characterised in that the organic solvent described in S1 is first
One or more in alcohol, ethanol, acetone.
The preparation method of super-hydrophobic stub the most as claimed in claim 1, it is characterised in that nonpolar organic molten described in S2
Agent is normal hexane or pentane.
The preparation method of super-hydrophobic stub the most as claimed in claim 1, it is characterised in that the clean stub described in S2 immerses
Time in described hydrophobic sol is at least 1min, and the time using described non-polar organic solvent to wash is at least 10min.
The preparation method of super-hydrophobic stub the most as claimed in claim 1, it is characterised in that the stub described in S2 is at 80 DEG C
It is dried.
6. the super-hydrophobic stub that the preparation method of the super-hydrophobic stub as described in any one in Claims 1 to 5 obtains, its feature
Being, described super-hydrophobic stub is 156 ° to the static contact angle of water, and roll angle is less than 3 °, to immiscible with water organic
The contact angle of solvent or oils is 0 °.
The purposes that super-hydrophobic stub the most as claimed in claim 6 separates as oil hydrosol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510163857.XA CN104815462B (en) | 2015-04-08 | 2015-04-08 | Super-hydrophobic stub and preparation method thereof and purposes |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510163857.XA CN104815462B (en) | 2015-04-08 | 2015-04-08 | Super-hydrophobic stub and preparation method thereof and purposes |
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| CN104815462B true CN104815462B (en) | 2016-08-31 |
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| CN105664534A (en) * | 2016-01-19 | 2016-06-15 | 南昌航空大学 | Method or preparing super-hydrophobic cigarette butts applicable to separating oil and water |
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| GB201108334D0 (en) * | 2011-05-18 | 2011-06-29 | Schlumberger Holdings | Separation of oil droplets from water |
| CN103276590B (en) * | 2013-06-04 | 2015-07-08 | 东北林业大学 | Method for preparing super-hydrophobic super-oleophylic cotton |
| CN103526549B (en) * | 2013-10-30 | 2016-02-03 | 东北林业大学 | For the preparation method of the super-hydrophobic glass cloth of water-oil separating |
| CN104194028B (en) * | 2014-08-15 | 2017-01-18 | 中国科学院新疆理化技术研究所 | Preparation method and application of three-element siloxane sponge |
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