CN105935503B - A kind of super-hydrophobic carbon fabric carries the preparation method and its usage of nickel cobalt double-hydroxide composite material - Google Patents
A kind of super-hydrophobic carbon fabric carries the preparation method and its usage of nickel cobalt double-hydroxide composite material Download PDFInfo
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- CN105935503B CN105935503B CN201610368814.XA CN201610368814A CN105935503B CN 105935503 B CN105935503 B CN 105935503B CN 201610368814 A CN201610368814 A CN 201610368814A CN 105935503 B CN105935503 B CN 105935503B
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- carbon fabric
- nickel cobalt
- super
- composite material
- cobalt double
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
Abstract
The present invention provides the preparation method and its usages that a kind of super-hydrophobic carbon fabric carries nickel cobalt double-hydroxide composite material, carry out as steps described below：Prepare carbon fabric；It prepares carbon fabric and carries nickel cobalt double-hydroxide；It prepares super-hydrophobic carbon fabric and carries nickel cobalt double-hydroxide composite material.Super-hydrophobic carbon fabric obtained by the present invention carries that nickel cobalt double-hydroxide composite material machinery performance is good, stable structure.
Description
Technical field
The present invention relates to the preparation methods that a kind of super-hydrophobic carbon fabric carries nickel cobalt double-hydroxide composite material, belong to environment work(
It can technical field of material.
Background technology
Environmental problem has become a major challenge of facing mankind, haze, sewage, waste residue, exhaust gas, white pollution etc.,
All in the environment of serious threat this earth and the health of the mankind.And the appearance of this each problem, be all mankind itself development
It brings, the solution of each problem, scientific worker will also be made to pay the effort of hardships.And the processing of waste water undoubtedly can
It solves the problems, such as that environmental problem and water resource lack to play, reaches the act of the two-win for effect of killing two birds with one stone.Wherein oil extraction, sea
A large amount of oily waste water caused by upper oil accident, sanitary sewage etc. has become a major challenge of puzzlement environment.Oily waste water meeting
Huge harm is caused to environment, such as oil floating across the sea, diffuseing to form one layer of air-locked oil film rapidly can hinder
The reoxygenation effect of water body, leads to ocean water body anoxic, influences halomereid growth, destroys marine ecology balance.Containing greasy dirt
Water process get up also it is extremely difficult, efficiency is low, of high cost, Oil in Sewage Water is divided into four kinds by physical state：Free oil, dispersed oil,
Oil emulsion, dissolved oil.
Being usually used in the method for oiliness sewage treatment mainly has gravitational method, centrifugal process, Bubble-floating Method, absorption method, chemical method, biology
Method and membrane separation process.Wherein UF membrane is with low energy consumption, single-stage separative efficiency is high, process flexible is simple, environmental pollution is low, general
The advantages that property is strong, but UF membrane application efficiency is by internal factors and films such as the resistance tocrockings, thermal stability, chemical stability of film
The limitation of the external factors such as kit form, operating condition.With table of the development of material science in recent years based on special wetability
Plane materiel material research and development is swift and violent, mainly including super hydrophilic, super-hydrophobic, super oleophylic, superoleophobic, super-amphiphobic, super parents surface etc.,
Self-cleaning surface, anti-fog coating, nonpolluting coating, anti-fingerprint coating, microlayer model Transfer Technology, water-oil separating etc. achieve one
Serial application.The essence of water-oil separating is interface problem, by the special wellability on designing material surface, obtain it is superoleophobic or
Super-hydrophobic separation material undoubtedly improves its most effective means of water-oil separating performance.However based on the film of special wetability
The application of material is there is also many problems, such as the resistance to swelling of film is poor, chemical resistance is poor, flux decline is very fast, processing
The limited types of oily wastewater, separative efficiency be not high etc., these problems are all urgently to be resolved hurrily.
The present invention has super-hydrophobic super-oleophylic characteristic by carbon fabric, nickel cobalt double-hydroxide, by simply modifying to prepare
Composite material, which has higher stability, available for water-oil separating.
Invention content
The present invention relates to the preparation methods that a kind of super-hydrophobic carbon fabric carries nickel cobalt double-hydroxide composite material.It takes first suitable
It measures cotton fabric and is warming up to 400~600 DEG C under nitrogen protection with the heating rate of 5 DEG C/min in tube furnace, maintain at 2h carbonizations
It manages, the sample with ethanol washes clean after carbonization treatment is dried in baking oven.Again by 2.5mmol nickel chlorides (NiCl2·6H2O)、
5mmol cobalt chlorides (CoCl2·6H2O), 2mmol cetyl trimethylammonium bromides (CTAB) and 9mmol urea (CO (NH2)2)
It is dissolved in 50mL deionized waters.Then the solution is transferred to 65mL hydrothermal reaction kettles, 0.5~1g of carbon fabric is put into reaction kettle,
100~150 DEG C of 9~12h of processing.After Temperature fall, carbon fabric is carried into nickel cobalt double-hydroxide compound and is taken out, is washed with ethyl alcohol
Several times, 60 DEG C of drying.Finally, carbon fabric load nickel cobalt double-hydroxide is put into the stearic acid ethanol solution of 0.05-1.0mol/L
Vibrate 6h (80~120 turns/min) in an oscillator at room temperature.The composite material of preparation has super-hydrophobic super-oleophylic, can use
In the separation of oil water mixture.
The technical solution adopted by the present invention is：
A kind of super-hydrophobic carbon fabric carries the preparation method of nickel cobalt double-hydroxide composite material, carries out as steps described below：
Step 1 prepares carbon fabric：Cotton fabric is taken to carry out carbonization treatment under inert gas shielding in tube furnace, is carbonized
Sample with ethanol washing that treated, which is placed in baking oven, dries, and obtains carbon fabric；
Step 2 prepares carbon fabric load nickel cobalt double-hydroxide：By nickel chloride (NiCl2·6H2O), cobalt chloride (CoCl2·
6H2O), cetyl trimethylammonium bromide (CTAB) and urea (CO (NH2)2) be dissolved in deionized water, mixed liquor A is obtained, so
The mixed liquor A is transferred in hydrothermal reaction kettle afterwards, then carbon fabric is added in hydrothermal reaction kettle, it is anti-to carry out incubation water heating
It should；After Temperature fall, product is taken out, is washed with ethyl alcohol, is dried, carbon fabric is obtained and carries nickel cobalt double-hydroxide；
Step 3 prepares super-hydrophobic carbon fabric load nickel cobalt double-hydroxide composite material：Carbon fabric is carried into the double hydroxides of nickel cobalt
Object is immersed in stearic ethanol solution, is vibrated in an oscillator at room temperature, is obtained super-hydrophobic carbon fabric and is carried the double hydrogen of nickel cobalt
Oxide composite.
In step 1, the quality of used cotton fabric is 3~10g, and the inert gas is nitrogen；The carbonization
The method of processing is：400~600 DEG C are warming up to, and 2h is maintained at 400~600 DEG C with the heating rate of 5 DEG C/min, it is described
Drying temperature is 60 DEG C.
In step 2, when preparing mixed liquor A, the nickel chloride (NiCl2·6H2O), cobalt chloride (CoCl2·6H2O), 16
Alkyl trimethyl ammonium bromide (CTAB) and urea (CO (NH2)2) with the amount ratio of deionized water it is 2.5mmol：5mmol：2mmol：
9mmol：50mL；The amount ratio of the dosage of the carbon fabric and used deionized water is 0.5~1g：50mL.
In step 2, the temperature of incubation water heating reaction is 100~150 DEG C, and the reaction time is 6~12h；Described
Drying temperature is 60 DEG C.
In step 3, in used stearic ethanol solution, stearic a concentration of 0.05~0.1mol/L；It is shaking
The oscillation method swung in device is：6h is vibrated with 80~120 turns/min.
The super-hydrophobic carbon fabric carries nickel cobalt double-hydroxide composite material, has super-hydrophobic super-oleophylic, and stability
By force, it prepares simply, there are some potential applications, such as the oil stain in separation oily wastewater, make water-oil separating.
The beneficial effects of the present invention are：
(1) textile material is cheap, derives from a wealth of sources used in the present invention, environmentally protective；
(2) super-hydrophobic carbon fabric made from carries good nickel cobalt double-hydroxide composite material machinery performance, stable structure, simultaneously
With super-hydrophobic super-oleophylic, the separation available for oily wastewater.
(3) preparation method of the invention is simple and practicable, flow is shorter, easy controlled operation, suitable for promoting the use of.
Description of the drawings
(a) and (b) is the scanning electron microscope (SEM) photograph of carbon fabric prepared by embodiment 1 in Fig. 1；
Fig. 2 is that super-hydrophobic carbon fabric prepared by embodiment 1 carries nickel cobalt double-hydroxide composite material scanning electron microscope (SEM) photograph；
Fig. 3 is the water contact angle that super-hydrophobic carbon fabric prepared by embodiment 1 carries nickel cobalt double-hydroxide composite material；
Fig. 4 is the oily contact angle that super-hydrophobic carbon fabric prepared by embodiment 1 carries nickel cobalt double-hydroxide composite material, wherein
(a) it is by contact material for dichloroethanes, (b) is moment of dichloroethanes contact material, and (c) is immersed for dichloroethanes in material
Portion.
Specific embodiment
With reference to specific embodiment, the invention will be further described：
Embodiment 1：
(1) carbon fabric is prepared：Appropriate cotton fabric is taken to heat up under nitrogen protection with the heating rate of 5 DEG C/min in tube furnace
To 400 DEG C, 2h carbonization treatments are maintained, the 60 DEG C of drying in baking oven of the sample with ethanol washes clean after carbonization treatment.
(2) carbon fabric carries the preparation of nickel cobalt double-hydroxide：By 2.5mmol nickel chlorides (NiCl2·6H2O), 5mmol chlorinations
Cobalt (CoCl2·6H2O), 2mmol cetyl trimethylammonium bromides (CTAB) and 9mmol urea (CO (NH2)2) it is dissolved in 50mL
Ionized water.Then the solution is transferred to 65mL hydrothermal reaction kettles, 0.5g carbon fabrics is put into reaction kettle, 100 DEG C of processing 12h.
After Temperature fall, carbon fabric is carried into nickel cobalt double-hydroxide compound and is taken out, is washed several times with ethyl alcohol, 60 DEG C of drying.
(3) it prepares super-hydrophobic carbon fabric and carries nickel cobalt double-hydroxide composite material：Carbon fabric is carried into nickel cobalt double-hydroxide
The stearic acid ethanol solution for being immersed in 0.05mol/L vibrates 6h (80~120 turns/min) in an oscillator at room temperature.
(a) and (b) is the scanning electron microscope (SEM) photograph of carbon fabric prepared by embodiment 1 in Fig. 1；From figure (a) it can be seen that carbon is knitted
Object is made of many micron order fibers, and some fibers are interweaved together.From (b) it can be seen that micron order fiber surface compared with
To be smooth, without coarse structure.
Fig. 2 is that super-hydrophobic carbon fabric prepared by embodiment 1 carries nickel cobalt double-hydroxide composite material scanning electron microscope (SEM) photograph；From figure
2 understand that with a large amount of nickel cobalt double-hydroxide, in acicular texture, micro nano structure is formed with carbon fiber for carbon fabric surface.
Fig. 3 is the water contact angle that super-hydrophobic carbon fabric prepared by embodiment 1 carries nickel cobalt double-hydroxide composite material；From figure
In it can be seen that water contact angle be 156 ± 1 ° (150 ° of ＞), show super hydrophilic property.
Fig. 4 is the oily contact angle that super-hydrophobic carbon fabric prepared by embodiment 1 carries nickel cobalt double-hydroxide composite material, wherein
(a) it is by contact material for dichloroethanes, (b) is moment of dichloroethanes contact material, and (c) is immersed for dichloroethanes in material
Portion；It can be seen that dichloroethanes can just immerse material internal in 32ms, super-oleophilic is shown.
Embodiment 2：
(1) carbon fabric is prepared：Appropriate cotton fabric is taken to heat up under nitrogen protection with the heating rate of 5 DEG C/min in tube furnace
To 500 DEG C, 2h carbonization treatments are maintained, the 60 DEG C of drying in baking oven of the sample with ethanol washes clean after carbonization treatment.
(2) carbon fabric carries the preparation of nickel cobalt double-hydroxide：By 2.5mmol nickel chlorides (NiCl2·6H2O), 5mmol chlorinations
Cobalt (CoCl2·6H2O), 2mmol cetyl trimethylammonium bromides (CTAB) and 9mmol urea (CO (NH2)2) it is dissolved in 50mL
Ionized water.Then the solution is transferred to 65mL hydrothermal reaction kettles, 0.7g carbon fabrics is put into reaction kettle, 120 DEG C of processing 9h.From
So after cooling, carbon fabric is carried into nickel cobalt double-hydroxide compound and is taken out, is washed several times with ethyl alcohol, 60 DEG C of drying.
(3) it prepares super-hydrophobic carbon fabric and carries nickel cobalt double-hydroxide composite material：Carbon fabric is carried into nickel cobalt double-hydroxide
The stearic acid ethanol solution for being immersed in 0.08mol/L vibrates 6h (80~120 turns/min) in an oscillator at room temperature.
Embodiment 3：
(1) carbon fabric is prepared：Appropriate cotton fabric is taken to heat up under nitrogen protection with the heating rate of 5 DEG C/min in tube furnace
To 600 DEG C, 2h carbonization treatments are maintained, the 60 DEG C of drying in baking oven of the sample with ethanol washes clean after carbonization treatment.
(2) carbon fabric carries the preparation of nickel cobalt double-hydroxide：By 2.5mmol nickel chlorides (NiCl2·6H2O), 5mmol chlorinations
Cobalt (CoCl2·6H2O), 2mmol cetyl trimethylammonium bromides (CTAB) and 9mmol urea (CO (NH2)2) it is dissolved in 50mL
Ionized water.Then the solution is transferred to 65mL hydrothermal reaction kettles, 1g carbon fabrics is put into reaction kettle, 150 DEG C of processing 6h.It is natural
After cooling, carbon fabric is carried into nickel cobalt double-hydroxide compound and is taken out, is washed several times with ethyl alcohol, 60 DEG C of drying.
(3) it prepares super-hydrophobic carbon fabric and carries nickel cobalt double-hydroxide composite material：Carbon fabric is carried into nickel cobalt double-hydroxide
The stearic acid ethanol solution for being immersed in 0.1mol/L vibrates 6h (80~120 turns/min) in an oscillator at room temperature.
Claims (6)
1. a kind of super-hydrophobic carbon fabric carries the preparation method of nickel cobalt double-hydroxide composite material, which is characterized in that according to following
Step carries out：
Step 1 prepares carbon fabric：Cotton fabric is taken to carry out carbonization treatment, carbonization treatment under inert gas shielding in tube furnace
Sample with ethanol washing afterwards, which is placed in baking oven, dries, and obtains carbon fabric；
Step 2 prepares carbon fabric load nickel cobalt double-hydroxide：By nickel chloride, cobalt chloride, cetyl trimethylammonium bromide and urine
Element is dissolved in deionized water, obtains mixed liquor A, then the mixed liquor A is transferred in hydrothermal reaction kettle, then carbon fabric is added in
Into hydrothermal reaction kettle, incubation water heating reaction is carried out；After Temperature fall, product is taken out, is washed with ethyl alcohol, 60 DEG C of drying obtain
Nickel cobalt double-hydroxide is carried to carbon fabric；
Step 3 prepares super-hydrophobic carbon fabric load nickel cobalt double-hydroxide composite material：Carbon fabric is carried into the leaching of nickel cobalt double-hydroxide
It not in stearic ethanol solution, vibrates in an oscillator at room temperature, obtains super-hydrophobic carbon fabric and carry the double hydroxides of nickel cobalt
Object composite material.
2. a kind of super-hydrophobic carbon fabric according to claim 1 carries the preparation method of nickel cobalt double-hydroxide composite material,
It is characterized in that, in step 1, the quality of used cotton fabric is 3 ~ 10g, and the inert gas is nitrogen；The carbon
Changing the method handled is：400 ~ 600 DEG C are warming up to, and 2 h are maintained at 400 ~ 600 DEG C with the heating rate of 5 DEG C/min, it is described
Drying temperature be 60 DEG C.
3. a kind of super-hydrophobic carbon fabric according to claim 1 carries the preparation method of nickel cobalt double-hydroxide composite material,
It is characterized in that, in step 2, when preparing mixed liquor A, the nickel chloride, cobalt chloride, cetyl trimethylammonium bromide and urea
Amount ratio with deionized water is 2.5 mmol：5 mmol：2 mmol：9 mmol：50 mL；The dosage of the carbon fabric with
The amount ratio of used deionized water is 0.5 ~ 1g：50mL.
4. a kind of super-hydrophobic carbon fabric according to claim 1 carries the preparation method of nickel cobalt double-hydroxide composite material,
It is characterized in that, in step 2, the temperature of incubation water heating reaction is 100 ~ 150 DEG C, and the reaction time is 6 ~ 12 h；It is described
Drying temperature be 60 DEG C.
5. a kind of super-hydrophobic carbon fabric according to claim 1 carries the preparation method of nickel cobalt double-hydroxide composite material,
It is characterized in that, in step 3, in used stearic ethanol solution, stearic a concentration of 0.05 ~ 0.1 mol/L；
Oscillation method in oscillator is：6h is vibrated with 80 ~ 120 turns/min.
6. super-hydrophobic carbon fabric prepared by the method described in claim 1 ~ 5 any one carries nickel cobalt double-hydroxide composite material
Purposes, which is characterized in that the super-hydrophobic carbon fabric carries nickel cobalt double-hydroxide composite material for adsorbing in oily wastewater
Oil stain, make water-oil separating.
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| CN106520075B (en) * | 2016-10-09 | 2018-10-09 | 江苏大学 | A kind of microwave method prepares the method and application thereof of superhydrophobic fabric@nickel cobalt double-hydroxide composite materials |
| CN107008162B (en) * | 2017-04-06 | 2020-03-31 | 江苏大学 | Nickel hydroxide/carboxymethyl cellulose gel modified composite membrane and preparation method and application thereof |
| CN108771975B (en) * | 2018-06-13 | 2021-04-20 | 江苏大学 | Preparation method and application of super-hydrophilic/underwater super-oleophobic polyvinylidene fluoride composite membrane |
| CN110433671B (en) * | 2019-07-23 | 2021-09-10 | 江苏大学 | Preparation method and application of visible light induced self-cleaning carbon fiber film |
| CN112768653A (en) * | 2021-01-08 | 2021-05-07 | 天津工业大学 | Preparation method and application of flexible nickel-cobalt double hydroxide/metal organic frame/fabric electrode |
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| JPS5212687A (en) * | 1975-07-19 | 1977-01-31 | Sumitomo Metal Ind Ltd | Process for recovering oil |
| CA2850442A1 (en) * | 2011-09-28 | 2013-04-04 | King Abdullah University Of Science And Technology | Grafted membranes and substrates having surfaces with switchable superoleophilicity and superoleophobicity and applications thereof |
| CN103173998B (en) * | 2011-12-23 | 2016-01-13 | 中国科学院兰州化学物理研究所 | For the preparation method of the superhydrophobic woven fabric of water-oil separating |
| CN102961893B (en) * | 2012-11-07 | 2014-11-26 | 清华大学 | Super-hydrophobic and super-oleophylic oil-water separating mesh membrane and preparation method thereof |
| CN103157392B (en) * | 2013-03-22 | 2014-12-10 | 清华大学 | Biodegradable oil-water separation net film with super-hydrophobic and super-oleophylic properties and preparation method thereof. |
| CN103752041B (en) * | 2013-12-23 | 2015-04-15 | 电子科技大学 | Oil-water separation granule and preparation method thereof |
| CN104004498B (en) * | 2014-05-27 | 2015-05-20 | 哈尔滨工业大学 | Method for preparing carbonized cotton fiber oil absorbing material-carbamate oil coagulation agent composite oil spilling treatment material |
| CN104888497B (en) * | 2015-05-28 | 2016-07-06 | 南京理工大学 | A kind of oleophylic fluorocarbon resin block super-hydrophobic, super and preparation method |
| CN104906828A (en) * | 2015-06-27 | 2015-09-16 | 中国科学院合肥物质科学研究院 | Foam metal-based oil slick collection material and preparation method thereof |
| CN105217603B (en) * | 2015-11-12 | 2017-05-31 | 中国科学院新疆理化技术研究所 | A kind of preparation method of CNT foamed material |
| CN105369248B (en) * | 2015-11-16 | 2018-06-26 | 河南大学 | One kind has the super-hydrophobic Co of micron and nanometer composite structure3O4The preparation method of film |
| CN105461849A (en) * | 2015-12-28 | 2016-04-06 | 重庆市环境科学研究院 | Preparation method of hydrophobic oleophilic resin and application of hydrophobic oleophilic resin in oil-water separation material |
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