CN104815608A - Preparation method of multifunctional oil-water separation material based on graphene oxide nanobelt - Google Patents
Preparation method of multifunctional oil-water separation material based on graphene oxide nanobelt Download PDFInfo
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- CN104815608A CN104815608A CN201510220548.1A CN201510220548A CN104815608A CN 104815608 A CN104815608 A CN 104815608A CN 201510220548 A CN201510220548 A CN 201510220548A CN 104815608 A CN104815608 A CN 104815608A
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Abstract
The invention discloses a preparation method of a multifunctional oil-water separation material based on graphene oxide nanobelts, wherein the preparation method includes following steps: (1) cutting functionalized graphene oxide nanobelts in an oxidizing manner; and (2) preparing a graphene oxide nanobelt porous thin film through a vacuum-suction filtering method. The porous screen multifunctional oil-water separation thin film is 38 +/- 2 cm<2> in area and is 5-200 nm in pore size. The multifunctional oil-water separation material screen film can simultaneously perform oil-water separation and heavy metal adsorption to a mixture containing oil and water and heavy metal ions and the like components which are insoluble to each other. The integrated water-purifying renewable film has very important significance on protecting environment and maintaining ecologic system balance.
Description
Technical field
The present invention relates to a kind of preparation method of multi-functional graduation porous compound nethike embrane.
Background technology
Oil spills and oil-containing industrial water discharge have been worldwide problems, this brings many noxious materials to ocean, be delivered to by marine food chain and comprise in each species body of the mankind from rudimentary plant algae to higher mammal, organism species and human health are on the hazard.And except containing insoluble oil in industrial wastewater, contain a large amount of dispersion emulsion and heavy metal ion toward contact, due to its toxicity and carcinogenesis, heavy metal is considered to " killer " that pose a health risk.Along with the increase of population and the scarcity of freshwater resources, preparation stable circulation can use, become a urgent demand for the multi-functional diffusion barrier removing the oil of different conditions in water and heavy metal ion.
Traditional weight-driven water-oil separating film can only separating emulsions or immiscible oil water mixture, can not separate dissolved metal ion in the solution.With regard to existing oil-water separation mesh film and sorbing material, separation process and adsorption process are carried out all respectively, and the rear water of separation needs to carry out after-treatment and just can re-use.Therefore needing to prepare can function match, carry out the diffusion barrier of water-oil separating and heavy metal adsorption, and diffusion barrier can realize automatically cleaning after a procedure, anti-oil pollution simultaneously, continues to recycle.
Summary of the invention
The object of this invention is to provide a kind of preparation method based on the multi-functional water-oil separating material of stannic oxide/graphene nano band; multi-functional water-oil separating material web prepared by the method can carry out water-oil separating and heavy metal adsorption to containing the multi-component mixture such as profit, metal ion that do not dissolve each other simultaneously; this one body swimming purification renewable membrane, has very important significance to protection of the environment, maintenance ecosystem balance.
The object of the invention is to be achieved through the following technical solutions:
Based on a preparation method for the multi-functional water-oil separating material of stannic oxide/graphene nano band, adopt oxidizing process in conjunction with vacuum filtration legal system for multi-functional graduation water-oil separating material, concrete steps are as follows:
One, oxidizing process cutting function stannic oxide/graphene nano band:
(1) measuring 2-50mL phosphoric acid solution joins in the round-bottomed flask of 500mL, adds the 20-400mL concentrated sulfuric acid, stirs;
(2) taking 0.1-10g CNT joins in the mixed acid liquid of step (1), stirs 0.1-5h;
(3) divided by 0.1-50g potassium permanganate 3 steps slowly to join in the mixed liquor of step (2), stir 0.5-1h;
(4) above-mentioned reaction system is moved in the oil bath pan of 30-70 DEG C, after stirring reaction 5-48h, be cooled to room temperature;
(5) solution of step (4) is poured in the frozen water mixed liquor containing 2-50mL hydrogen peroxide (30%) into the 5-48h that condenses, now solution become blackish green explanation reaction complete;
(6) hydrochloric acid and 100-300mL deionized water filtration washing on poly tetrafluoroethylene that 50-200mL concentration is 1-30% will be added after ultrasonic for solution process;
(7) dry in vacuum drying chamber, obtain stannic oxide/graphene nano band (GONRs), ultrasonic 2-50min obtains the GONRs suspension of homogenization;
(8) 0.1-10g IPDI is added in GONRs suspension, under nitrogen protection stirring reaction 20-30h, finally obtain product carrene and DMF washing 4-6 time, freeze drying obtains functional graphene oxide nanobelt.
Two, stannic oxide/graphene nano band porous membrane is prepared by vacuum filtration method:
(1) stannic oxide/graphene nano band to be dispersed in 100-1000mL deionized water and ultrasonic process, prepare uniform stannic oxide/graphene nano band suspension, controlling total ultrasonic time is 0.2-5 hour, but its time is not continuous print, and 5s is ultrasonic, 5s stops, simultaneously, the intensity of ultrasonic process is 100-200W, and frequency is 10-30 KHZ, and voltage is 100-220V;
(2) the stannic oxide/graphene nano band suspension of acquisition is filtered one deck filter membrane by vacuum filtration, the pore size using filter paper is 30-50 μm, and film diameter is 7cm, and area is 38.46cm
2, consequent film is pliable and tough, can prejudicially not depart from filter paper easily.
For the multi-functional nethike embrane of stannic oxide/graphene nano band, undertaken heavy metal ion adsorbed by its surface functional group, its mechanism of action is as follows:
。
Tool of the present invention has the following advantages:
1, the present invention utilizes high length-diameter ratio micro-nano-scale material to carry out vacuum filtration legal system for porous material is a kind of simple, the method that convenient, cost is low, parameter is controlled, and prepared stannic oxide/graphene nano band netting gear has, and good super hydrophilic under water super oleophobic is low sticks character, can automatically cleaning be realized, prevent oil pollution in separation process.
2, graphene oxide has a large amount of functional groups due to its surface, its heavy metal ion has good suction-operated, therefore graphene oxide composite material is a kind of outstanding and heavy metal ion adsorbing material, and it has amphiphilic, is a kind of promising water-oil separating material.
3, the high draw ratio of stannic oxide/graphene nano band is utilized can to form porous network structure from overlap joint, prepare holey stannic oxide/graphene nano band and can realize heavy metal adsorption and water-oil separating double process simultaneously, and stannic oxide/graphene nano band there is high specific area can simultaneously chelating many kinds of metal ions, there is the advantage that adsorption capacity is large.
4, traditional oil water separation process, can not be separated with the heavy metal ion in water the oil in sewage simultaneously, stannic oxide/graphene nano band nethike embrane prepared by the present invention can be applied simultaneously in Adsorption of Heavy Metal Ions and water-oil separating, solve the problems such as the after-treatment in the process of disposing of sewage, have a good application prospect.
5, graphene oxide has amphiphilic, and in air, hydrophilic and oleophilic super oleophobic under water, carries out the infiltration of water before carrying out water-oil separating by stannic oxide/graphene nano band nethike embrane, forms water membrane, can effectively stop oil to infiltrate in oil water separation process.
6, the area of Multifunctional oil moisture scrapping off film that prepared by the present invention is 38 ± 2cm
2, holey membrane pore size is 5-200nm.
7, this preparation method is simple to operate, and experiment parameter is controlled, and cost is low, can be used for manufacturing water-oil separating and heavy metal adsorption multifunctional material, and this material has hydrophilic and oleophilic super oleophobic properties under water in air, good mechanical stability.
Accompanying drawing explanation
Fig. 1 is stannic oxide/graphene nano band porous web pattern and application process schematic diagram;
Fig. 2 is stannic oxide/graphene nano band porous web automatically cleaning process schematic.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Detailed description of the invention one: present embodiment prepares multi-functional water-oil separating material in accordance with the following steps:
One, oxidizing process cutting function stannic oxide/graphene nano band:
(1) measuring 2-50mL phosphoric acid solution joins in the round-bottomed flask of 500mL, adds the 20-400mL concentrated sulfuric acid, stirs under the rotating speed of 15000-30000rpm;
(2) taking 0.1-10g CNT joins in the mixed acid liquid of step (1), stirs 0.1-5h;
(3) divided by 0.1-50g potassium permanganate 3 steps slowly to join in the mixed liquor of step (2), stir 0.5-1h;
(4) above-mentioned reaction system is moved in the oil bath pan of 30-70 DEG C, under the rotating speed of 15000-30000rpm, be cooled to room temperature after stirring reaction 5-48h;
(5) solution of step (4) is poured in the frozen water mixed liquor containing 2-50mL hydrogen peroxide (30%) into the 5-48h that condenses, now solution become blackish green explanation reaction complete;
(6) solution is added the hydrochloric acid and 100-300mL deionized water filtration washing on poly tetrafluoroethylene that 50-200mL concentration is 1-30% after ultrasonic process 20-30min under 30-50Hz condition;
(7) dry 20-30h in the vacuum drying chamber of 50-80 DEG C, obtains stannic oxide/graphene nano band (GONRs), and ultrasonic 2-50min obtains the GONRs suspension of homogenization;
(8) 0.1-10g IPDI is added in GONRs suspension; stirring reaction 20-30h(mixing speed is 15000-30000rpm under nitrogen protection); finally obtain product carrene and DMF washing 4-6 time, freeze drying obtains functional graphene oxide nanobelt.
Two, stannic oxide/graphene nano band porous membrane is prepared by vacuum filtration method:
(1) stannic oxide/graphene nano band to be dispersed in 100-1000mL deionized water and ultrasonic process, prepare uniform stannic oxide/graphene nano band suspension, controlling total ultrasonic time is 0.2-5 hour, but its time is not continuous print, and 5s is ultrasonic, 5s stops, simultaneously, the intensity of ultrasonic process is 100-200W, and frequency is 10-30 KHZ, and voltage is 100-220V;
(2) the stannic oxide/graphene nano band suspension of acquisition is filtered one deck filter membrane by vacuum filtration, the pore size using filter paper is 30-50 μm, and film diameter is 7cm, and area is 38.46cm
2, consequent film is pliable and tough, can prejudicially not depart from filter paper easily.
Three, heavy metal ion adsorbed and water-oil separating application process:
Preparation heavy metal ion solution is as model pollutant, and stannic oxide/graphene nano band nethike embrane is contained on oily-water seperating equipment, is separated by Action of Gravity Field.Oil water mixture and heavy metal ion are passed through oily-water seperating equipment, through the multi-functional GONRs nethike embrane of preparation simultaneously.Utilize oily-water seperating equipment to test for water-oil separating separative efficiency nethike embrane respectively, after being separated, liquid is measured its oil content by Infrared Oil Determination Instrument and Atomic Absorption Spectrometer (AAS) and is recorded disengaging time.As shown in Figure 1, Adsorption of Heavy Metal Ions and oil, by 100mL10% salt acid soak, are carried out wash-out, for subsequent applications (Fig. 2) by separating oil and Adsorption of Heavy Metals caudacoria.
The area of Multifunctional oil moisture scrapping off film prepared by the present invention is 38 ± 2cm
2, holey membrane pore size is 5-200nm.
Detailed description of the invention two: present embodiment prepares Multifunctional oil moisture scrapping off film in accordance with the following steps:
One, oxidizing process cutting function stannic oxide/graphene nano band;
(1) measuring 20mL phosphoric acid solution joins in the round-bottomed flask of 500mL, then adds the 180mL concentrated sulfuric acid and stirs under rotating speed is 30000rpm;
(2) take 1g CNT to join in above mixed acid liquid and stir 1h;
(3) divided by 6g potassium permanganate 3 steps slowly to join in above mixed liquor and stir 30min;
(4) above-mentioned reaction system being moved in the oil bath pan of 45 DEG C, is be cooled to room temperature after stirring reaction 24h under the condition of 30000rpm at rotating speed;
(5) pour in the frozen water mixed liquor containing 10mL hydrogen peroxide (30%) 24h that condenses into, now solution become blackish green explanation reaction complete;
(6) hydrochloric acid and 150mL deionized water filtration washing on poly tetrafluoroethylene that 100mL concentration is 10% will be added after ultrasonic for solution process;
(7) in the vacuum drying chamber of 60 DEG C, dry 24h obtains stannic oxide/graphene nano band (GONRs), and ultrasonic 10min obtains the GONRs suspension of homogenization;
(8) added by 2g IPDI, under nitrogen protection stirring reaction 24h, finally obtain product carrene and DMF washs 5 times, freeze drying obtains functional graphene oxide nanobelt.
Two, stannic oxide/graphene nano band porous membrane is prepared by vacuum filtration method:
(1) 0.008mol stannic oxide/graphene nano band to be dispersed in 400mL deionized water and ultrasonic process, to prepare uniform stannic oxide/graphene nano band suspension.Arranging total ultrasonic time is 1.0 hours, but its time is not continuous print, and 5s is ultrasonic, and 5s stops.The effective time of ultrasonic process is 0.5 hour.Meanwhile, the intensity of ultrasonic process is 150W, 20 KHZ frequency and voltage 203V.
(2) the nanobelt suspension of acquisition is filtered one deck filter membrane by vacuum filtration, the pore size using filter paper is 30-50 μm, and film diameter is 7cm, and area is 38.46cm
2.Consequent film is pliable and tough, can prejudicially not depart from filter paper easily.
Three, heavy metal ion adsorbed and water-oil separating application process:
Preparation heavy metal ion solution is as model pollutant, and stannic oxide/graphene nano band nethike embrane is contained on oily-water seperating equipment, is separated by Action of Gravity Field.Oil water mixture and heavy metal ion are passed through oily-water seperating equipment, through the multi-functional GONRs nethike embrane of preparation simultaneously.Oily-water seperating equipment is utilized to test for water-oil separating separative efficiency nethike embrane respectively, after being separated, liquid is measured its oil content by Infrared Oil Determination Instrument and Atomic Absorption Spectrometer (AAS) and is recorded disengaging time, separative efficiency 95 ± 4%, Adsorption of Heavy Metal Ions 90 ± 5%.
The area of Multifunctional oil moisture scrapping off film prepared by present embodiment is 38 ± 2cm
2, holey membrane pore size is 100 ± 20nm, and thickness is 2mm.
Detailed description of the invention three: present embodiment prepares Multifunctional oil moisture scrapping off film in accordance with the following steps:
One, oxidizing process cutting function stannic oxide/graphene nano band:
(1) measuring 20mL phosphoric acid solution joins in the round-bottomed flask of 500mL, then adds the 180mL concentrated sulfuric acid and is stir under the condition of 30000rpm at rotating speed;
(2) take 3g CNT to join in above mixed acid liquid and stir 1h;
(3) divided by 6g potassium permanganate 3 steps slowly to join in above mixed liquor and stir 30min;
(4) above-mentioned reaction system being moved in the oil bath pan of 45 DEG C, is be cooled to room temperature after stirring reaction 24h under the condition of 30000rpm at rotating speed;
(5) pour in the frozen water mixed liquor containing 10mL hydrogen peroxide (30%) 24h that condenses into, now solution become blackish green explanation reaction complete;
(6) hydrochloric acid and 150mL deionized water filtration washing on poly tetrafluoroethylene that 100mL concentration is 10% will be added after ultrasonic for solution process;
(7) in the vacuum drying chamber of 60 DEG C, dry 24h obtains stannic oxide/graphene nano band (GONRs), and ultrasonic 10min obtains the GONRs suspension of homogenization;
(8) added by 2g IPDI, under nitrogen protection stirring reaction 24h, finally obtain product carrene and DMF washs 5 times, freeze drying obtains functional graphene oxide nanobelt.
Two, stannic oxide/graphene nano band porous membrane is prepared by vacuum filtration method:
(1) 0.008mol stannic oxide/graphene nano band to be dispersed in 400mL deionized water and ultrasonic process, to prepare uniform stannic oxide/graphene nano band suspension.Arranging total ultrasonic time is 1.0 hours, but its time is not continuous print, and 5s is ultrasonic, and 5s stops.The effective time of ultrasonic process is 0.5 hour.Meanwhile, the intensity of ultrasonic process is 150W, 20 KHZ frequency and voltage 203V.
(2) the nanobelt suspension of acquisition is filtered one deck filter membrane by vacuum filtration; The pore size using filter paper is 30-50 μm.Film diameter is 7cm, and area is 38.46cm
2.Consequent film is pliable and tough, can prejudicially not depart from filter paper easily.
Three, heavy metal ion adsorbed and water-oil separating application process:
Preparation heavy metal ion solution is as model pollutant, and stannic oxide/graphene nano band nethike embrane is contained on oily-water seperating equipment, is separated by Action of Gravity Field.Oil water mixture and heavy metal ion are passed through oily-water seperating equipment, through the multi-functional GONRs nethike embrane of preparation simultaneously.Utilize oily-water seperating equipment to test for water-oil separating separative efficiency nethike embrane respectively, after being separated, liquid is measured its oil content by Infrared Oil Determination Instrument and Atomic Absorption Spectrometer (AAS) and is recorded disengaging time.
The area of Multifunctional oil moisture scrapping off film prepared by present embodiment is 38 ± 2cm
2, holey membrane pore size is 20 ± 10nm, and thickness is 5mm.
Claims (6)
1., based on a preparation method for the multi-functional water-oil separating material of stannic oxide/graphene nano band, it is characterized in that described method step is as follows:
One, oxidizing process cutting function stannic oxide/graphene nano band:
(1) measuring 2-50mL phosphoric acid solution joins in the round-bottomed flask of 500mL, adds the 20-400mL concentrated sulfuric acid, stirs;
(2) taking 0.1-10g CNT joins in the mixed acid liquid of step (1), stirs 0.1-5h;
(3) divided by 0.1-50g potassium permanganate 3 steps slowly to join in the mixed liquor of step (2), stir 0.5-1h;
(4) above-mentioned reaction system is moved in the oil bath pan of 30-70 DEG C, after stirring reaction 5-48h, be cooled to room temperature;
(5) solution of step (4) is poured in the frozen water mixed liquor containing 2-50mL hydrogen peroxide into the 5-48h that condenses, now solution become blackish green explanation reaction complete;
(6) 50-200mL hydrochloric acid and 100-300mL deionized water filtration washing on poly tetrafluoroethylene will be added after ultrasonic for solution process;
(7) dry in vacuum drying chamber, obtain GONRs, ultrasonic 2-50min obtains the GONRs suspension of homogenization;
(8) 0.1-10g IPDI is added in GONRs suspension, under nitrogen protection stirring reaction 20-30h, finally obtain product carrene and DMF washing 4-6 time, freeze drying obtains functional graphene oxide nanobelt;
Two, stannic oxide/graphene nano band porous membrane is prepared by vacuum filtration method:
(1) functional graphene oxide nanobelt to be dispersed in 100-1000mL deionized water and ultrasonic process, to prepare uniform stannic oxide/graphene nano band suspension;
(2) the stannic oxide/graphene nano band suspension of acquisition is filtered one deck filter membrane by vacuum filtration.
2. the preparation method based on stannic oxide/graphene nano band multifunctional water parting material according to claim 1, is characterized in that the concentration of described hydrogen peroxide is 30%.
3. the preparation method based on stannic oxide/graphene nano band multifunctional water parting material according to claim 1, is characterized in that the concentration of described hydrochloric acid is 1-30%.
4. the preparation method based on stannic oxide/graphene nano band multifunctional water parting material according to claim 1, is characterized in that in described step 2 (1), and the intensity of ultrasonic process is 100-200W, and frequency is 10-30 KHZ, and voltage is 100-220V.
5. the preparation method based on stannic oxide/graphene nano band multifunctional water parting material according to claim 1, is characterized in that, in described step 2 (1), total ultrasonic time is that 0.2-5 hour, 5s are ultrasonic, and 5s stops.
6. the preparation method based on stannic oxide/graphene nano band multifunctional water parting material according to claim 1, it is characterized in that the filter paper pore size that described vacuum filtration uses is 30-50 μm, film diameter is 7cm, and area is 38.46cm
2.
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