CN110194504A - The preparation method of superhydrophilic superoleophobic water-oil separating sponge - Google Patents
The preparation method of superhydrophilic superoleophobic water-oil separating sponge Download PDFInfo
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- CN110194504A CN110194504A CN201910567692.0A CN201910567692A CN110194504A CN 110194504 A CN110194504 A CN 110194504A CN 201910567692 A CN201910567692 A CN 201910567692A CN 110194504 A CN110194504 A CN 110194504A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The present invention provides a kind of preparation method of superhydrophilic superoleophobic water-oil separating sponge, includes the following steps: that Dopamine hydrochloride is dissolved in deionized water by (1) and be uniformly mixed, be configured to the reaction solution that concentration is 0.01~0.02mol/L;(2) sponge is immersed in step (1) in configured reaction solution, the ethylene polyamine of final concentration of 0.005~0.01mol/L is added, room temperature decentralization is set after sealing, takes out sponge, and sponge is immersed in the water spare by washing;(3) sponge obtained by step (2) is immersed in silver nitrate solution, water-oil separating sponge is made in washing.Preparation method low cost provided by the invention, preparation is simple, the water-oil separating sponge of this method preparation with super hydrophilic underwater superoleophobic property and can be catalyzed small organic molecule in reductive water, have the advantages that separate and catalytic reduction efficiency is high, stable, reusable.
Description
Technical field
The present invention relates to functional material technical fields, and in particular to a kind of system of superhydrophilic superoleophobic water-oil separating sponge
Preparation Method.
Background technique
The rapid development of industry, results in the discharge of a large amount of oily waste waters.Oily waste water seriously endanger people's health and
Life security pollutes environment, has caused great concern.In face of serious water pollution, water-oil separating, which becomes, solves water body
One of key technology of pollution.How low in cost, environmental-friendly, separative efficiency height, the grease point of high recycling rate are found
Off-network film has caused the great interest and extensive concern of research field.
Oil-water separation mesh film with special wellability is divided into super-hydrophobic super-oleophylic separation nethike embrane and superhydrophilic superoleophobic point
Off-network film.For super-hydrophobic super-oleophylic separation nethike embrane for, the lipophilicity having since itself is potential, cause oil droplet or other
Impurity is easily adsorbed on film, causes the pollution of separation nethike embrane, reduces water-oil separating efficiency, causes the reusability difference and two of film
Secondary pollution.And opposite superhydrophilic superoleophobic separation nethike embrane can be comparatively fast by being blocked in top for oil, so that oil is not due to water
It is directly contacted with nethike embrane, so as to avoid membrane pollution problem by favor.
In addition, oil is immiscible with water, so fuel-displaced phase and water phase are readily viewed in oily waste water, but in addition to oily waste water
Other than water, a large amount of small organic molecule is also dissolved in sewage, some are not that naked eyes are visible.Wherein 4- nitrophenol is as one
The important organic synthesis raw material of kind, is widely used in the intermediate of organic synthetic dye, medicine and pesticide, also indicates as soda acid
Agent is used as leather preservative.4- nitrophenol toxicity is big, it is difficult to which it is useless to generate a large amount of industry in use for biodegrade
Water causes serious water pollution.The 4- nitrophenol how degraded in water becomes one of urgent problem to be solved instantly, efficiently,
The novel process technology of low cost is always the direction that water treatment field is made great efforts.
Summary of the invention
The present invention provides a kind of preparation method of superhydrophilic superoleophobic water-oil separating sponge, solves and lacks in the prior art
Use wellability separation nethike embrane that water make when water-oil separating processing to degrade while passing through nethike embrane small organic molecule in water
Effective ways.
Technical scheme is as follows:
A kind of preparation method of superhydrophilic superoleophobic water-oil separating sponge, includes the following steps:
(1) Dopamine hydrochloride is dissolved in deionized water and is uniformly mixed, being configured to concentration is the anti-of 0.01~0.02mol/L
Answer solution;
(2) sponge is immersed in step (1) in configured reaction solution, addition final concentration of 0.005~
The ethylene polyamine of 0.01mol/L, room temperature decentralization is set after sealing, takes out sponge, and sponge is immersed in the water spare by washing;
(3) sponge obtained by step (2) is immersed in silver nitrate solution, water-oil separating sponge is made in washing.
Preferably, the processing step before further including base before the step (1), by mandruka as needed shape into
Row is cut.
Preferably, the sponge is melamine sponge, polyurethane sponge or polyvinylalcohol sponge.
Preferably, it is uniformly mixed solution by ultrasound in the step (1), ultrasonic time is 10~20min.
Preferably, it before ethylene polyamine being added in the step (2), is ultrasonically treated, ultrasonic time is 10~20min.
Preferably, solution places 30~50h at room temperature after sealing in the step (2).
Preferably, silver nitrate solution concentration is 0.3~1mg/mL in the step (3).
Preferably, the time that sponge is immersed in silver nitrate solution in the step (3) is 5~15min.
Another technical solution of the invention is as follows:
A kind of superhydrophilic superoleophobic water-oil separating sponge is made by any of the above-described kind of preparation method.
The utility model has the advantages that
Preparation method provided by the invention is easy to operate, low in cost, and can be mass-produced preparation.The method of the present invention preparation
Water-oil separating sponge out is super hydrophilic in air, underwater superoleophobic, and being capable of organic small point in simultaneous catalytic reduction water
Son, the compound sponge separative efficiency is high, and water can be blocked by oil faster in water-oil separating experiment, and to difference
Oils have excellent separating effect;Also, water-oil separating sponge of the present invention is environmental-friendly, and easy cleaning is easy to maintain, repeats
It utilizes, there is preferable stability.This at the same time, water-oil separating sponge of the present invention also restores in the catalysis of 4- nitrophenol real
Excellent performance is played in testing, due to in-situ reducing of the Nano silver grain on sponge, so that water is while passing through sponge,
The 4- nitrophenol dissolved in water is degraded under the catalytic action of Nano silver grain by sodium borohydride reduction, is in water treatment field
Sewage treatment provides more effective approach.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph a) of unmodified sponge substrate used in the embodiment of the present invention 1 and prepares multi-functional
The scanning electron microscope (SEM) photograph b) of sponge;
Fig. 2 be the embodiment of the present invention 1 prepared by sponge in air in water contact angle photo a) and water with gasoline liquid
Drip contact angle photo b);
Fig. 3 is that the Multifunctional sponge of 1-3 of embodiment of the present invention preparation is used for the experimental provision of oil-water separation mixture and divides
From effect photo;
Fig. 4 is experimental result picture of the Multifunctional sponge of 1-3 of embodiment of the present invention preparation for paranitrophenol catalysis reduction.
It wherein marks are as follows: 1- Multifunctional sponge;The mixture of 2- oil and water;Oil after 3- separation;Water after 4- separation.
Specific embodiment
The source of all raw materials is not particularly limited in following embodiment, raw material used is commercially available.
The present invention provides a kind of preparation method of superhydrophilic superoleophobic water-oil separating sponge, includes the following steps:
(1) mandruka is cut into suitable shape;
(2) Dopamine hydrochloride and deionized water are added in beaker and form solution;
(3) sponge is dipped in above-mentioned mixed solution, is ultrasonically treated lower dropwise addition ethylene polyamine;This step provides alkaline ring
Border, make dopamine complete auto polymerization and with the copolymerization of polyethylene polyamine and;
(4) beaker is sealed and placed in certain time at room temperature, is washed after taking out sponge, and be soaked in spare in water;Sea
Silk floss saves under water environment, avoids dehydration from air-drying, is conducive to the maintenance of hydrophilic and oleophobic property;
(5) above-mentioned sponge is soaked in silver nitrate solution at room temperature, is then washed with water, obtain the water-oil separating
Sponge;By the reduction reaction to silver nitrate, by modified by silver nanoparticles to sponge substrate, silver nano-grain is realized to nitre
The catalyst of base phenol reduction.
(6) sponge of above-mentioned preparation is for water-oil separating experiment and the reduction experiment of 4- nitrophenol.
In above-mentioned steps (1), the mandruka can be polyvinyl alcohol (PVA) sponge, melamine sponge, polyurethane
Sponge, cutting sponge diameter is 4~7cm, concretely 4cm, 5cm, 6cm or 7cm.
In above-mentioned steps (2), the concentration of the Dopamine hydrochloride is 0.01~0.02mol/L, concretely 0.01mol/
L、0.015mol/L、0.02mol/L。
In above-mentioned steps (3), the concentration of the ethylene polyamine is 0.005~0.01mol/L, concretely 0.005mol/
L、0.006mol/L、0.007mol/L、0.008mol/L、0.009mol/L、0.01mol/L。
In above-mentioned steps (3), ultrasonic time be 10~20min, concretely 10min, 12min, 15min, 18min,
20min。
In above-mentioned steps (4), time of repose is 30~50h at room temperature, concretely 30h, 35h, 40h, 45h, 50h.
In above-mentioned preparation method, step (5) in silver nitrate concentration be 0.3~1mg/mL, concretely 0.3mg/mL,
0.6mg/mL, 0.7mg/mL, 0.8mg/mL or 1mg/mL.
Above-mentioned steps (5) in, soaking time is 5~15min, specially 5min, 10min, 15min.
Implementation column 1
The present embodiment provides a kind of preparation methods of superhydrophilic superoleophobic water-oil separating sponge, include the following steps:
(1) PVA sponge is cut into the circle that diameter is 5cm;
(2) sponge is immersed in the beaker containing 250mL deionized water and 0.75g Dopamine hydrochloride, is ultrasonically treated 10min
To obtain homogeneous solution, the concentration of Dopamine hydrochloride is 0.015mol/L at this time;
(3) 0.25g ethylene polyamine is added dropwise under the ultrasonic treatment in step (2), the concentration of ethylene polyamine is at this time
0.006mol/L;
(4) above-mentioned beaker is sealed with paraffin, is placed 40 hours at room temperature, obtain PDA/PEPA sponge, taken out sponge and wash
It washs, is soaked in spare in water;
(5) sponge that step (4) obtains is immersed into 10min in the silver nitrate solution of 0.5mg/mL at room temperature, obtains Ag@
PDA/PEPA sponge is washed with water clean.
(6) sponge made from is tested for water-oil separating and the reduction experiment of 4- nitrophenol, as the result is shown sea obtained
Silk floss is greater than 150 ° in air to the contact angle of water close to 0 °, to the contact angle of oil.
As shown in Figure 1, wherein left side a) show the scanning electron microscope of unmodified sponge substrate used in the present embodiment 1
Figure, right side b) show the scanning electron microscope (SEM) photograph of the Multifunctional sponge of 1 method of the present embodiment preparation.It is in figure as it can be seen that unmodified
Sponge surface is more smooth, has non-uniform micron-sized aperture;The sponge surface of modified is more coarse, and surface is poly- more
Bar amine and polyethylene polyamine polymer bumps and silver nano-grain.
As shown in Fig. 2, wherein left side a) show sponge prepared by the present embodiment 1 in air with water contact angle figure,
Right side b) show sponge prepared by the present embodiment 1 in water with gasoline liquid-drop contact angle photo.Water-oil separating of the invention
The contact angle of sponge and water is close to 0 °, thus water energy is enough easily across water-oil separating sponge;Oily connecing on sponge simultaneously
Feeler is greater than 150 °, i.e. oil droplet cannot be infiltrated thus be cannot pass through in the water-oil separating sponge surface.
Embodiment 2
The present embodiment provides a kind of preparation methods of superhydrophilic superoleophobic water-oil separating sponge, include the following steps:
(1) melamine sponge is cut into the circle of diameter 5cm;
(2) sponge is immersed in the beaker containing 250mL deionized water and 0.95g Dopamine hydrochloride, is ultrasonically treated 10 points
Clock is to obtain homogeneous solution, and the concentration of Dopamine hydrochloride is 0.02mol/L at this time;
(3) 0.30g polyethylene polyamine is added dropwise under the ultrasonic treatment in step (2), the concentration of polyethylene polyamine is at this time
0.007mol/L;
(4) above-mentioned beaker is sealed with paraffin, is placed 45 hours at room temperature, obtain PDA/PEPA sponge, taken out sponge and wash
It washs, is soaked in spare in water;
(5) sponge that step (4) obtains is immersed in the silver nitrate solution of 0.8mg/mL 5 minutes at room temperature, obtains Ag@
PDA/PEPA sponge is washed with water clean.
(6) sponge made from is tested for water-oil separating and the reduction experiment of 4- nitrophenol, as the result is shown sea obtained
Silk floss is greater than 150 ° in air to the contact angle of water close to 0 °, to the contact angle of oil.
Embodiment 3
The present embodiment provides a kind of preparation methods of superhydrophilic superoleophobic water-oil separating sponge, include the following steps:
(1) polyurethane sponge is cut into the circle of diameter 5cm;
(2) sponge is immersed in the beaker containing 250mL deionized water and 0.47g Dopamine hydrochloride, is ultrasonically treated 10 points
Clock is to obtain homogeneous solution, and the concentration of Dopamine hydrochloride is 0.01mol/L at this time.
(3) 0.23g polyethylene polyamine is added dropwise under the ultrasonic treatment in step (2), the concentration of polyethylene polyamine is at this time
0.005mol/L;
(4) above-mentioned beaker is sealed with paraffin, is placed 30 hours at room temperature, obtain PDA/PEPA sponge, take out sponge
Washing, is soaked in spare in water;
(5) sponge that step (4) obtains is immersed in the silver nitrate solution of 0.3mg/mL 15 minutes at room temperature, obtains
Ag@PDA/PEPA sponge is washed with water clean.
(6) sponge made from is tested for water-oil separating and the reduction experiment of 4- nitrophenol, as the result is shown sea obtained
Silk floss is greater than 150 ° in air to the contact angle of water close to 0 °, to the contact angle of oil.
It is real that water-oil separating sponge made from the preparation method of 1-3 of the embodiment of the present invention carries out water-oil separating experiment catalysis reduction
It tests as follows:
(1) water-oil separating is tested
As shown in figure 3, carrying out oil-water separation test by shown Suction filtration device, above-mentioned obtained sponge is fixed on dress
Centre is set, upper and lower is respectively the glass container that feeds and discharge, and the mixture of toluene and water is passed through to the feed glass container of top
It is poured on above-mentioned water-oil separating sponge, water can rapidly be flowed into the mistake of lower section by water-oil separating sponge under the effect of gravity
In filter flask, while toluene is blocked in the top of water-oil separating sponge, the water after toluene and separation after being separated, to reach
To the purpose of water-oil separating.
(2) it is catalyzed reduction experiment
Catalysis reduction experiment is carried out using above-mentioned same apparatus, sponge is fixed among above-mentioned Suction filtration device, then
Configured certain density 4- nitrophenol solution is poured on sponge by the glass container of top, water is under the effect of gravity
It can be flowed by sponge in the filtering flask of lower section.Since under the catalytic action of Nano silver grain, sodium borohydride can be restored
4- nitrophenol in water so that solution eventually become it is colourless, to have the function that sewage purification.Fig. 4 is shown, molten after reaction
Liquid eventually becomes colourless, and sewage is purified.
Experimental result show that the contact angle of water-oil separating sponge and water of the invention is close to 0 °, thus water
Water-oil separating sponge can easily be passed through;Contact angle of the oil on sponge is greater than 150 ° simultaneously, i.e., oil droplet is in the grease
Separation sponge surface cannot be infiltrated thus be cannot pass through.Oil water mixture is poured into and is fixed with water-oil separating sponge of the invention
In the glass container being disposed vertically, quickly, while pass through oil is blocked fully above sponge water under the effect of gravity,
Achieve the effect that water-oil separating.Since the water-oil separating sponge has extremely low adhesiveness to oil droplet, oil droplet is in sponge table
Face does not infiltrate completely, so cleaning is easy;Solution containing 4- nitrophenol is in the 4- nitro by being dissolved after sponge in water
Phenol reacts under the catalytic action of Nano silver grain with sodium borohydride, realizes the efficient also original place of small organic molecule in water
Reason;And the sponge performance prepared is stablized, can Reusability, do not need complicated Conservation environment, be later water treatment field
Provide new idea and method.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from
In the case where mind and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of superhydrophilic superoleophobic water-oil separating sponge, which comprises the steps of:
(1) Dopamine hydrochloride is dissolved in deionized water and is uniformly mixed, it is molten to be configured to the reaction that concentration is 0.01~0.02mol/L
Liquid;
(2) sponge is immersed in step (1) in configured reaction solution, is added final concentration of 0.005~0.01mol/L's
Ethylene polyamine, room temperature decentralization is set after sealing, takes out sponge, and sponge is immersed in the water spare by washing;
(3) sponge obtained by step (2) is immersed in silver nitrate solution, water-oil separating sponge is made in washing.
2. the preparation method of superhydrophilic superoleophobic water-oil separating sponge according to claim 1, which is characterized in that described
It further include the processing step before substrate before step (1), by mandruka, shape is cut as needed.
3. the preparation method of superhydrophilic superoleophobic water-oil separating sponge according to claim 1, which is characterized in that the sea
Silk floss is melamine sponge, polyurethane sponge or polyvinylalcohol sponge.
4. the preparation method of superhydrophilic superoleophobic water-oil separating sponge according to claim 1, which is characterized in that the step
It is uniformly mixed solution by ultrasound in (1), ultrasonic time is 10~20min suddenly.
5. the preparation method of superhydrophilic superoleophobic water-oil separating sponge according to claim 1, which is characterized in that the step
Suddenly it before ethylene polyamine being added in (2), is ultrasonically treated, ultrasonic time is 10~20min.
6. the preparation method of superhydrophilic superoleophobic water-oil separating sponge according to claim 1, which is characterized in that the step
Suddenly solution places 30~50h at room temperature after sealing in (2).
7. the preparation method of superhydrophilic superoleophobic water-oil separating sponge according to claim 1, which is characterized in that the step
Suddenly silver nitrate solution concentration is 0.3~1mg/mL in (3).
8. the preparation method of superhydrophilic superoleophobic water-oil separating sponge according to claim 1, which is characterized in that the step
Suddenly the time that sponge is immersed in silver nitrate solution in (3) is 5~15min.
9. a kind of superhydrophilic superoleophobic water-oil separating sponge, which is characterized in that pass through any preparation of claim 1 to 8
Method is made.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111841514A (en) * | 2020-08-06 | 2020-10-30 | 四川大学 | High-performance underwater super-oleophobic recycled foam and preparation method thereof |
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CN104190111A (en) * | 2014-09-05 | 2014-12-10 | 清华大学 | Oil-water separation screen membrane with lead ion responsiveness and preparation method of membrane |
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Cited By (2)
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CN111841514A (en) * | 2020-08-06 | 2020-10-30 | 四川大学 | High-performance underwater super-oleophobic recycled foam and preparation method thereof |
CN111841514B (en) * | 2020-08-06 | 2022-03-29 | 四川大学 | High-performance underwater super-oleophobic recycled foam and preparation method thereof |
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