CN108465460A - A kind of preparation method of super-hydrophobic sponge sorbing material - Google Patents
A kind of preparation method of super-hydrophobic sponge sorbing material Download PDFInfo
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- CN108465460A CN108465460A CN201810475773.3A CN201810475773A CN108465460A CN 108465460 A CN108465460 A CN 108465460A CN 201810475773 A CN201810475773 A CN 201810475773A CN 108465460 A CN108465460 A CN 108465460A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
- B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
Abstract
The invention belongs to technical field of environment function material preparation, and in particular to a kind of preparation method of super-hydrophobic sponge sorbing material.It is as follows：Dopamine cladding sponge matrix is prepared first；Then hexadecyl trimethoxy silane, tetraethyl orthosilicate and ammonium hydroxide are dissolved in ethyl alcohol, form mixed solution；The sponge matrix of poly-dopamine cladding is added, is placed in water-bath progress constant temperature stirring, through water-bath oscillation, cleaning, dry super-hydrophobic sponge sorbing material.The acidproof super-hydrophobic sorbing material of alkali salt of height prepared by the present invention is a kind of simple and environmentally-friendly, at low cost, small investment and the high acidproof super-hydrophobic lipophile material of alkali salt that can be mass produced, it can be used for water-oil separating in industrial complex environment, stable structure, adsorption capacity are strong.
Description
Technical field
The invention belongs to technical field of environment function material preparation, and in particular to a kind of system of super-hydrophobic sponge sorbing material
Preparation Method.
Background technology
With the rapid development of social economy, to the increase of the processing transport of oils, the leakage event of oil product is frequently sent out
It is raw.A large amount of oily wastewater enter water environment not only can serious polluted-water resource, but also huge economic loss can be caused.
Therefore, the research for carrying out water-oil separating material is of great significance.Currently, the method for being usually used in oiliness sewage treatment mainly has weight
Force method, centrifugal process, Bubble-floating Method, absorption method, chemical method, bioanalysis and membrane separation process.Wherein, UF membrane is with low energy consumption, single-stage
The advantages that separative efficiency is high, process flexible is simple, environmental pollution is low, versatile receives significant attention.However before UF membrane
It is oily wastewater collection first to be carried out membrane separation again, but some specific environment cause oily wastewater that cannot collect to carry, such as
Marine oil spill, it is in situ to adsorb rule more this kind of oily wastewater of suitable treatments, it is a kind of method of effective processing oily wastewater,
The oil plant of leakage can be adsorbed or be recycled.Common oil absorption material oil silica gel, woolen knitwear and molecular sieve etc., but due to substance of this kind
Source is few, of high cost, adsorbance is small, the low disadvantage of selectivity limits their use.Therefore, there is an urgent need to develop a kind of warp
Ji is convenient, high adsorption capacity, highly selective sorbing material solve the problems, such as oily pollution.
Super-hydrophobicity is a kind of special wetability of the water contact angle more than 150 °, and surface roughness and surface energy are to influence
An important factor for wetability.Wetability is by the design of the surface of material and the modified low surface energy and appropriate thick of making it have
Rough structure.By constructing the substance of grade micro nano structure and modified low surface energy, super hydrophobic surface is become.Using hydrophobic
Oil-wet behavior can carry out the selective absorbing of effective oil, water-oil separating may be implemented.The preparation on super-hydrophobic super-oleophylic surface
Coarse structure usually is constructed in the surface of solids, this material with super-hydrophobic super-oleophylic property can contain greasy dirt with selective absorption
Oil in water, has a good application prospect.However there is also many problems for the application based on super-hydrophobic sorbing material, such as surely
It is qualitative it is poor, recycling rate of waterused is low, treating capacity is small etc., these problems are all urgently to be resolved hurrily.
Invention content
It is an object of the invention to overcome deficiency in the prior art, a kind of preparation of super-hydrophobic sponge sorbing material is provided
Method, the melamine sponge that super-hydrophobic sponge sorbing material is modified using poly-dopamine are prepared as matrix using sol-gal process
Super-hydrophobic sponge sorbing material, the material have higher stability, repeat and utilize, and large amount of adsorption can be used for high acid-alkali salt
Grease persistently detaches in environment.
It is as follows：
(1) dopamine cladding sponge matrix is prepared：Sponge matrix is put into ultrasound pretreatment in ethyl alcohol, drying first；So
Three (methylol) aminomethanes, dopamine are dissolved in deionized water afterwards and carry out ultrasound, sponge matrix is added, carries out water-bath oscillation
Reaction, is then cleaned with ethyl alcohol, is dried to obtain the sponge matrix of poly-dopamine cladding；
(2) super-hydrophobic sponge sorbing material is prepared：Hexadecyl trimethoxy silane, tetraethyl orthosilicate and ammonium hydroxide are dissolved in
In ethyl alcohol, mixed solution is formed；The sponge matrix for the poly-dopamine cladding that step (1) obtains is added, is placed in water-bath and carries out
Constant temperature stirs, and then switches in oscillator water-bath and vibrates, and sponge that oscillation is completed is cleaned with ethyl alcohol, dry super-hydrophobic sea
Continuous sorbing material.
Preferably, in step (1), a concentration of 10mM, pH 8.5 of three (methylol) aminomethane solution；Dopamine is dense
Degree is 2mg/mL；
Preferably, in step (1), bath temperature is 25 DEG C, 100~120r/min of hunting speed, duration of oscillation 6h.
Preferably, in step (2), hexadecyl trimethoxy silane, tetraethyl orthosilicate, ammonium hydroxide and ethyl alcohol amount ratio be
0.05~0.25g：0.25g：2mL：20~40mL；
Preferably, in step (2), the temperature of constant temperature stirring is 60~80 DEG C, and rotating speed is 20~40r/min, and the time is
30min；
Preferably, in step (2), the temperature of water-bath oscillation is 25 DEG C, 120~140r/min of hunting speed, duration of oscillation 6
~for 24 hours；
Preferably, in step (1) and (2), the drying temperature is 60 DEG C.
Obtained super-hydrophobic sponge material has super-hydrophobic super-oleophylic characteristic, and stability is strong, prepares simply, can use
Grease persistently detaches in high acid-alkali salt environment.
Advantageous effect：
(1) persursor material used in the present invention is sponge, abundance, cheap.
(2) super-hydrophobic sponge sorbing material contact angle produced by the present invention is more than 150 °, has superhydrophobic characteristic；And
Super-hydrophobic sponge surface closely has one layer of micro-nano silicon layer, forms micro-nano multilevel hierarchy with three-dimensional net structure, favorably
In the super-hydrophobicity of material.
(3) super-hydrophobic sponge sorbing material large amount of adsorption produced by the present invention, can to the quality of adsorption capacity of dichloroethanes
Up to 107g/g or so, other oils reach tens times of sole mass；Meanwhile the material has high stability, it is strong acid, strong
Alkali, high concentration salting liquid can exist in its surface-stable, can be used for water-oil separating in industrial complex environment, performance is stablized.
(4) the circulation absorption quality capacity for the super-hydrophobic sponge absorption petroleum ether that prepared by the present invention, inhales by 80 cycles
Attached, the quality of adsorption capacity of super-hydrophobic sponge absorption petroleum ether not decreased significantly, and it is good to show that super-hydrophobic sponge has
Repeatable usability.
(5) operation is simple, does not need Large expensive instrument, is economic and environment-friendly for manufacturing process of the present invention.
(6) super-hydrophobic sponge sorbing material produced by the present invention is closed with pump group, can be used for lasting water-oil separating, anticorrosion
With the fields such as automatically cleaning.
Description of the drawings
Fig. 1 is the photo of original melamine sponge matrix (a) and the super-hydrophobic sponge (b) of the preparation of embodiment 3.
The SEM figures of 1000 times of super-hydrophobic sponge (a), 5000 times (b) that Fig. 2 is prepared for embodiment 3.
Fig. 3 be original melamine sponge (a), embodiment 3 prepare super-hydrophobic sponge (b) contact angle figure and contain soda acid
Saline solution drops in sponge surface figure (c).
It is experimentation (a of super-hydrophobic sponge absorption petroleum ether prepared by embodiment 3 in Fig. 41)-(a4) and the system of embodiment 3
Experimentation (the b of standby super-hydrophobic sponge absorption 1,2- dichloroethanes1)-(b4)。
Fig. 5 is the experimental provision and experimentation that super-hydrophobic sponge prepared by embodiment 3 persistently detaches petroleum ether；(a) it is
Experimental equipment is (b) that suction pipe is inserted into super-hydrophobic sponge, and (c1), (c2) and (c3) is the experimentation for persistently detaching petroleum ether.
Fig. 6 is super-hydrophobic sponge absorption petroleum ether, dichloroethanes, hexane, toluene, diesel oil, soybean oil prepared by embodiment 3
Quality of adsorption capacity.
Fig. 7 is the super-hydrophobic sponge of the preparation of embodiment 3 in highly acid, neutrality, strong basicity, high salt solution petrochina ether
Quality of adsorption capacity.
Fig. 8 is the circulation absorption quality capacity of super-hydrophobic sponge absorption petroleum ether prepared by embodiment 3.
Specific implementation mode
In order to clarify the technical solutions and technical objectives of the present invention, the present invention is done further with reference to specific embodiment
Introduction.
Embodiment 1：
(1) dopamine cladding sponge body is prepared：Sponge is put into ultrasound pretreatment 10min in ethyl alcohol, is put into baking oven
60 DEG C of drying；Preparation 10mM, pH=8.5 volume is 100mL tri- (methylol) aminomethane solution, and it is more that 0.2g hydrochloric acid is then added
Bar amine, then the sponge of wash clean is put into above-mentioned solution, 25 DEG C of oscillations 6h, hunting speed 100r/ in water bath chader
min.After the completion of oscillation, sponge is taken out, is cleaned repeatedly with ethyl alcohol, 60 DEG C of drying in baking oven are put into.Obtain poly-dopamine cladding
Sponge
(2) super-hydrophobic sponge is prepared：By 0.05g hexadecyl trimethoxy silanes, 0.25g tetraethyl orthosilicates, 2mL ammonium hydroxide
It is dissolved in 20mL ethyl alcohol, the sponge of drying is put into, be placed in 60 DEG C of heating stirring 30min in water-bath, mixing speed 20r/
min.It is then transferred into oscillator and vibrates for 24 hours for 25 DEG C, hunting speed 120r/min.Sponge is taken out after the completion of oscillation, is used
Ethyl alcohol cleaning is multiple, is placed in 60 DEG C of bakings in baking oven, obtains super-hydrophobic lipophile sponge.
Embodiment 2：
(1) dopamine cladding sponge body is prepared：Sponge is put into ultrasound pretreatment 10min in ethyl alcohol, is put into baking oven
60 DEG C of drying；10mM is prepared, pH=8.5 volumes are 100mL tri- (methylol) aminomethane solution, and it is more that 0.2g hydrochloric acid is then added
Bar amine, then the sponge of wash clean is put into above-mentioned solution, 25 DEG C of oscillations 6h, hunting speed 110r/ in water bath chader
min.After the completion of oscillation, sponge is taken out, is cleaned repeatedly with ethyl alcohol, 60 DEG C of drying in baking oven are put into.Obtain poly-dopamine cladding
Sponge
(2) super-hydrophobic sponge is prepared：By 0.15g hexadecyl trimethoxy silanes, 0.25g tetraethyl orthosilicates, 2mL ammonium hydroxide
It is dissolved in 30mL ethyl alcohol, the sponge of drying is put into, be placed in 60 DEG C of heating stirring 30min in water-bath, mixing speed 30r/
Min is then transferred into 25 DEG C of oscillations 12h, hunting speed 130r/min in oscillator.Sponge is taken out after the completion of oscillation, is used
Ethyl alcohol cleaning is multiple, is placed in 60 DEG C of drying in baking oven, obtains super-hydrophobic lipophile sponge.
Embodiment 3：
(1) dopamine cladding sponge body is prepared：Sponge is put into ultrasound pretreatment 10min in ethyl alcohol, is put into baking oven
60 DEG C of drying；10mM is prepared, pH=8.5 volumes are 100mL tri- (methylol) aminomethane solution, and it is more that 0.2g hydrochloric acid is then added
Bar amine, then the sponge of wash clean is put into above-mentioned solution, 25 DEG C of oscillation (120r/min) 6h in water bath chader.Oscillation is completed
Afterwards, sponge is taken out, is cleaned repeatedly with ethyl alcohol, be put into 60 DEG C of drying in baking oven.Obtain poly-dopamine cladding sponge
(2) super-hydrophobic sponge is prepared：By 0.25g hexadecyl trimethoxy silanes, 0.25g tetraethyl orthosilicates, 2mL ammonium hydroxide
It is dissolved in 40mL ethyl alcohol, the sponge of drying is put into, be placed in 60 DEG C of heating stirring 30min in water-bath, mixing speed 40r/
Min is then transferred into 5 DEG C of oscillations 6h, hunting speed 140r/min in oscillator.Sponge is taken out after the completion of oscillation, uses second
Alcohol cleaning is multiple, is placed in 60 DEG C of drying in baking oven, obtains super-hydrophobic lipophile sponge.
(a) and (b) is respectively Protospongia and super-hydrophobic sponge prepared by embodiment 3 in Fig. 1, is compared from figure (a) and (b)
It can be seen that super-hydrophobic sponge color changes in (b), the basic structure of sponge does not change, and shows Protospongia by success
It is modified.
(a) and (b) is respectively 1000 times of super-hydrophobic sponge, 5000 times of scanning electron microscope (SEM) photograph prepared by embodiment 3 in Fig. 2；
From figure (a) it can be seen that super-hydrophobic sponge has three-dimensional net structure；It is close from can see super-hydrophobic sponge surface in (b)
With one layer of micro-nano silicon layer, micro-nano multilevel hierarchy is formed with three-dimensional net structure, is conducive to the super-hydrophobicity of material.
Fig. 3 be respectively the water contact angle of Protospongia, embodiment 3 prepare super-hydrophobic sponge water contact angle and high antacid
The sponge surface of alkali salt；It is hydrophily from figure (a) it can be seen that the water contact angle of Protospongia is 0 °；It can see from figure (b)
The water contact angle of super-hydrophobic sponge is 155 ° ± 1 ° (150 ° of ＞), shows superhydrophobic characteristic；From figure (c) it can be seen that super thin
Water sponge surface strong acid, highly basic, high level salt solution can be stabilized, and be shown with high chemical stability.
2, with reference to adsorption experiment, the present invention will be further described：
(1) the absorption property evaluation of super-hydrophobic sponge carries out by the following method in the present invention：It is completed using adsorption experiment.
Weigh quality m before the absorption of super-hydrophobic sponge respectively first0, by the petroleum ether of certain mass, 1,2- dichloroethanes, hexane, first
Benzene, diesel oil, soybean oil are added separately in beaker, and water appropriate is then added and forms oil water mixture, adds respectively into beaker
Enter the sponge weighed, after adsorption saturation, weighs super-hydrophobic sponge quality mf, finally, the mass adsorption of sponge is obtained by calculation
Capacity (Q).
Wherein mf(mg) and m0(mg) it is respectively the quality after sponge is adsorbed and the quality before absorption.
(2) suction pipe is inserted into super-hydrophobic sponge, put it into oil water mixture, the other end of suction pipe connects beaker, profit
With peristaltic pump separator, the oil that super-hydrophobic sponge is adsorbed is transferred in beaker, point that grease is a large amount of, lasting may be implemented
From.
Fig. 4 (a1)、(a2)、(a3) and (a4) it is that super-hydrophobic sponge prepared by embodiment 3 adsorbs the experimentation of petroleum ether,
Specifically (a1) be the Sudan's red colouring petroleum ether/deionized water mixture photo, (a2) it is super-hydrophobic sponge absorption dyeing stone
The photo of oily ether, (a3) it is super-hydrophobic sponge by the photo of the petroleum ether extrusion of absorption, (a4) it is after super-hydrophobic sponge squeezes
Reinstatement photo；(b1)、(b2)、(b3) and (b4) it is the experimentation that super-hydrophobic sponge adsorbs 1,2- dichloroethanes, specifically
(b1) it is with the mixture photo of dichloroethanes/deionized water of the Sudan's red colouring, (b2) it is that super-hydrophobic sponge stretches into underwater absorption
Dye the photo of dichloroethanes process, (b3) it is super-hydrophobic sponge by the dichloroethanes extrusion photo of absorption, (b4) it is super thin
Restore to the original state photo after the extruding of water sponge；Show that super-hydrophobic sponge can not only adsorb light oil, but also light attached heavy oil can be inhaled.
Fig. 5 is the experimental provision and experimentation that super-hydrophobic sponge prepared by embodiment 3 persistently detaches petroleum ether；(a) it is
The oil collector sump tank of super-hydrophobic sponge and peristaltic pump composition is (b) that suction pipe is inserted into the photo inside sponge, and c figures are super-hydrophobic sponge
Process oily in oil water mixture in large beaker is collected, specific (c1) is original state photo, (c2) is collection status photo
With the photo (c3) for collecting end；Show that super-hydrophobic sponge can continue oil-water separation mixture, a small amount of material can be handled greatly
Measure oil water mixture.
Fig. 6 is the adsorption capacity that super-hydrophobic sponge adsorbs several oils, and super-hydrophobic sponge is to dichloroethanes as we know from the figure
Quality of adsorption capacity be 107g/g, be 80g/g to the quality of adsorption capacity of soya-bean oil, to the quality of adsorption capacity of other all kinds of oil
Reach tens times of sole mass, there is good adsorption capacity.
Fig. 7 is super-hydrophobic sponge in highly acid, the quality of adsorption capacity of neutrality, strong basicity, high salt solution petrochina ether,
Soda acid salt environment is influenced on super-hydrophobic sponge on the adsorption capacity of oil there is no apparent as we know from the figure, shows super-hydrophobic sponge
It is with good stability.
Fig. 8 is the circulation absorption quality capacity that super-hydrophobic sponge adsorbs petroleum ether, by 80 circulation absorptions, super-hydrophobic sea
The quality of adsorption capacity of silk floss absorption petroleum ether not decreased significantly, show that super-hydrophobic sponge has good repeatable utilization
Property.
Claims (8)
1. a kind of preparation method of super-hydrophobic sponge sorbing material, which is characterized in that be as follows：
（1）Prepare dopamine cladding sponge matrix；
（2）Prepare super-hydrophobic sponge sorbing material：Hexadecyl trimethoxy silane, tetraethyl orthosilicate and ammonium hydroxide are dissolved in ethyl alcohol
In, form mixed solution；Step is added（1）The sponge matrix of obtained poly-dopamine cladding, is placed in water-bath and carries out constant temperature
Stirring then switches in oscillator water-bath and vibrates, then cleaned with ethyl alcohol, dry super-hydrophobic sponge sorbing material.
2. a kind of preparation method of super-hydrophobic sponge sorbing material according to claim 1, which is characterized in that step（2）
Described in hexadecyl trimethoxy silane, tetraethyl orthosilicate, ammonium hydroxide and ethyl alcohol amount ratio be 0.05 ~ 0.25g：0.25g：
2mL：20~40mL.
3. a kind of preparation method of super-hydrophobic sponge sorbing material according to claim 1, which is characterized in that step（2）
Described in constant temperature stirring temperature be 60 ~ 80 DEG C.
4. a kind of preparation method of super-hydrophobic sponge sorbing material according to claim 1, which is characterized in that step（2）
Described in constant temperature stirring rotating speed be 20 ~ 40r/min, time 30min.
5. a kind of preparation method of super-hydrophobic sponge sorbing material according to claim 1, which is characterized in that step（2）
In, the temperature of the water-bath is 25 DEG C.
6. a kind of preparation method of super-hydrophobic sponge sorbing material according to claim 1, which is characterized in that step（2）
In, the speed of the oscillation is 120 ~ 140r/min, duration of oscillation is 6 ~ for 24 hours.
7. a kind of preparation method of super-hydrophobic sponge sorbing material according to claim 1, which is characterized in that step（2）
Described in drying temperature be 60 DEG C.
8. the super-hydrophobic sea prepared according to a kind of preparation method of any super-hydrophobic sponge sorbing material of claim 1 ~ 7
Continuous sorbing material is applied to the lasting separation of grease in soda acid salt environment.
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Cited By (5)
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| CN109629234A (en) * | 2018-11-30 | 2019-04-16 | 杭州师范大学 | A kind of preparation method of silazane and dopamine cooperative flame retardant super-hydrophobic coat |
| CN111410767A (en) * | 2020-04-20 | 2020-07-14 | 南京工业大学 | Carborane-based super-hydrophobic material and preparation method and application thereof |
| CN113980347A (en) * | 2021-09-09 | 2022-01-28 | 盐城工学院 | Preparation method of super-hydrophobic and super-oleophylic polymer sponge material |
| CN115155536A (en) * | 2022-07-12 | 2022-10-11 | 湖北大学 | Preparation method of super-hydrophobic flame-retardant sponge for selective adsorption |
| WO2023098008A1 (en) * | 2021-12-03 | 2023-06-08 | 江南大学 | High-strength starch frozen gel having super-hydrophobicity and preparation method therefor |
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| CN111410767A (en) * | 2020-04-20 | 2020-07-14 | 南京工业大学 | Carborane-based super-hydrophobic material and preparation method and application thereof |
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| CN113980347B (en) * | 2021-09-09 | 2023-02-24 | 盐城工学院 | Preparation method of super-hydrophobic super-oleophylic polymer sponge material |
| WO2023098008A1 (en) * | 2021-12-03 | 2023-06-08 | 江南大学 | High-strength starch frozen gel having super-hydrophobicity and preparation method therefor |
| CN115155536A (en) * | 2022-07-12 | 2022-10-11 | 湖北大学 | Preparation method of super-hydrophobic flame-retardant sponge for selective adsorption |
| CN115155536B (en) * | 2022-07-12 | 2023-04-07 | 湖北大学 | Preparation method of super-hydrophobic flame-retardant sponge for selective adsorption |
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Application publication date: 20180831 |