CN106283894B - A kind of graphene oxide is modified filter paper and preparation method and application - Google Patents
A kind of graphene oxide is modified filter paper and preparation method and application Download PDFInfo
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- CN106283894B CN106283894B CN201610643771.1A CN201610643771A CN106283894B CN 106283894 B CN106283894 B CN 106283894B CN 201610643771 A CN201610643771 A CN 201610643771A CN 106283894 B CN106283894 B CN 106283894B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/08—Filter paper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/13—Silicon-containing compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/71—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes
- D21H17/74—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes of organic and inorganic material
Abstract
Filter paper and preparation method and application is modified the invention discloses a kind of graphene oxide, is to use dip coating, by filter paper impregnation in the mixed solution of graphene oxide and silane coupler, ultrasonic disperse, then take out, put and dry naturally at room temperature, produce graphene oxide and be modified filter paper.Graphene oxide modification filter paper preparation method disclosed by the invention is simple, cost is low, obtained filter paper stability is good, has good separating effect to oil water mixture, having a extensive future in profit quick separating and oiliness sewage treatment.
Description
Technical field
Filter paper and preparation method and application is modified the present invention relates to a kind of graphene oxide, belongs to organo-mineral complexing work(
Can field of material technology.
Background technology
Oily waste water essentially from oil exploitation, crude oil leakage, ship ballast water and chemical industry, steel, food, weaving,
The industries such as machining, the oil-polluted water destruction ecological balance, endanger human health.Oil-polluted water is handled, is conducive to water
The improvement of environment；The impurity such as the moisture in product oil can remove by water-oil separating, oil quality is improved.Utilize the special of material
Wellability realizes water-oil separating to the different interface interactions of oil and water, has become and promotes the important of oily water separation technique development
Breach, compared with traditional water-oil separating material, the water-oil separating material with special wellability has high efficiency and Gao Xuan
Selecting property.At present, the water-oil separating material with special wellability mainly includes two classes of oil removing and water removal.As people are to oil-containing water
Processing and the continuous improvement of water-oil separating requirement, new challenge is proposed to oily water separation technique and material.
Graphene oxide itself has the specific surface area and loose structure of super large, changed as a kind of new nano material
Learn property stable.Graphene oxide has superior dispersiveness because of it in water, is considered as hydroaropic substance, but oxygen for a long time
Graphite alkene is of virtually amphipathic, hydrophilic to hydrophobic property distribution is presented from graphene platelet edge to center, therefore
Graphene oxide can generally there are interface such as interfacial agent, and reduce the energy between interface.In view of its property, oxidation
Graphene presents good application prospect in water-oil separating field.Application of the graphene oxide in water-oil separating mainly has two
The approach of kind：One is that graphene oxide is made into film or other carrier surfaces are carried on, and utilizes the super parent of graphene oxide in itself
Water and superoleophobic property realizes water-oil separating under water；Two be that graphene oxide is reduced into graphene, utilizes the super-hydrophobic of graphene
Property realizes water-oil separating.Chinese patent CN103768960A discloses a kind of preparation method of graphene basement membrane and its in profit point
Application from, it forms gel by graphene oxide and crosslinking agent, dries, and is reduced after being compacted under 10~200 kPas of pressure
Obtain.Chinese patent CN104815608A discloses a kind of system based on the multi-functional water-oil separating material of stannic oxide/graphene nano band
Preparation Method, using oxidizing process cutting function stannic oxide/graphene nano band, then prepares graphite oxide by vacuum filtration method
Alkene nanobelt porous membrane.Chinese patent CN103623709A discloses graphene oxide and is modified superhydrophilic superoleophobic water-oil separating
Film and preparation method and application, the agent of hydrophilic polymer water-sensitive, crosslinking film forming agent, Nano silica sol are mixed, with graphene oxide
For inorganic crosslinking agent, ultrasonic disperse, coated in silk screen film forming, drying crosslinking obtains the superoleophobic water-oil separating of super-hydrophilic and underwater
Nethike embrane.Chinese patent CN104841287A discloses a kind of preparation method of multi-functional graduation water-oil separating composite film material,
Holey Cu films are prepared using bubble hydrogen template, by infusion process porous C u film surfaces prepare chitosan (CS) and
Graphene oxide (GO) composite coating.Chinese patent CN104828817A discloses a kind of oxygen with high efficiency oil-water separating capacity
Graphite alkene nethike embrane and preparation method thereof, graphene oxide water solution is dipped into by the stainless (steel) wire that surface has a large amount of defects
In, graphene oxide is covered stainless (steel) wire twine surface, obtain a kind of graphene oxide nethike embrane.Chinese patent
CN105396466A disclose a kind of cellulose nano-fibrous-graphene oxide hydridization of high water flux composite hyperfiltration membrane and its
Preparation method, its structure includes at least one layer of cellulose nano-fibrous filter layer with graphene oxide hydridization, and at least one layer of
Microfiltration membranes support layer or electrostatic spinning nano fiber support layer, the composite hyperfiltration membrane have good resist in oil water separation process
Pollute fouling performance and pressure-resistant performance.Chinese patent CN103626171A discloses a kind of preparation method of water-oil separating material,
Sponge material is soaked in graphene oxide solution, graphene oxide cladding sponge material is obtained, in the presence of reducing agent
Reduction reaction is carried out, water-oil separating material is obtained.Chinese patent CN103432994A discloses a kind of graphene-based suction of magnetic
The preparation method of oil whip composite, will obtain graphene oxide water solution, and adds carbon receiving after graphite oxide ultrasonic disperse
Mitron, through suction filtration film forming, graphene-based foamed material is obtained by hydrothermal reduction method, by chemical method in its area load oxygen
Change iron standby magnetic graphite alkenyl foamed composite.
On the premise of high water-oil separating efficiency is kept, selection versatile material improves steady as matrix, process simplification
It is qualitative, cost is reduced, it is the development in the field to realize extensive preparation and application of the graphene oxide in water-oil separating material
Direction.Compared with metal nethike embrane or other hard materials, paper base material has the advantages that softness, easily shaped, and prepares water-oil separating
Material has unique advantage, but the report of paper substrate graphene oxide composite material is less.Chinese patent CN105254920A is disclosed
A kind of preparation method of graphene paper prepreg, miillpore filter vacuum mistake is used by the uniform graphene suspension of ultrasonic disperse
Filter, graphene film material is dried together with filter paper, screening is taken off from miillpore filter, subsequently heat-treated to remove dispersant,
So as to obtain the graphene paper-like material of self-supporting, it is placed in the mixed liquor of epoxy resin and solvent and impregnates, obtain resin
The graphene paper prepreg of dipping.Chinese patent CN103086373A discloses a kind of titanium dioxide-graphene composite nano paper
And preparation method thereof, its key component is titanium dioxide nano-belts and graphene or titanium dioxide nano-belts, graphene and added
Plus agent, prepare main including processes such as synthesis-compound-scattered-suction filtration-dryings.
Graphene oxide is coated on matrix surface, can be effectively improved by increasing graphene oxide and basal body binding force
The performance of material and life-span.Chinese patent CN105214512A discloses a kind of preparation of carrier surface graphene oxide membrane
Method, introduces amino active group in carrier surface first, graphene oxide uniform load then is obtained into oxygen to carrier surface
Graphite alkene film, because the oxy radical in graphene oxide and amino react, enhances graphene oxide membrane and carrier
Between adhesion.Chinese patent CN103788413A discloses a kind of method of graphene oxide chemical modification inorganic filler, adopts
Graphene oxide is connected to inorganic filler surface with chemical modification method, makes to produce firm Covalent bonding together therebetween.Profit
The adhesion between graphene oxide and filter paper can be increased with " bridging effect " of coupling agent, graphene oxide can be not only improved
The performance of modified filter paper, while being created conditions for the extensive use that graphene oxide is modified filter paper.
The content of the invention
Filter paper and preparation method and application is modified it is an object of the invention to provide a kind of graphene oxide.
A kind of graphene oxide of the present invention is modified the preparation method of filter paper, is to use dip coating, by filter paper impregnation in
In the mixed solution of graphene oxide and silane coupler, ultrasonic disperse then takes out, and puts and dries naturally at room temperature, produces oxygen
Graphite alkene is modified filter paper；
It is characterized in that：
The filter paper is the qualitative or quantitative filter paper of common middling speed that average pore size is 1~50 micron；
The mixed solution of the graphene oxide and silane coupler is made according to the following ratio, graphene oxide:Silane is even
Join agent:Deionized water:Absolute ethyl alcohol is 1g~5g:0.05g~0.5g:20mL~30mL:70mL~80mL；
The condition of the ultrasonic disperse is：Ultrasonic power 200W~400W, 25 DEG C~35 DEG C of ultrasonic temperature, ultrasonic time 1
~3 hours；
Naturally the time dried is 12~36 hours.
Above-mentioned graphene oxide is modified in the preparation method of filter paper：It is micro- for 30~50 that the filter paper is preferably average pore size
The qualitative or quantitative filter paper of common middling speed of rice.
Above-mentioned graphene oxide is modified in the preparation method of filter paper：The mixing of the graphene oxide and silane coupler
Solution is preferably made according to the following ratio, graphene oxide:Silane coupler:Deionized water:Absolute ethyl alcohol is 1g~2g:0.05g
~0.2g:20mL:80mL.
Above-mentioned graphene oxide is modified in the preparation method of filter paper：The silane coupler is 3- aminopropyl-triethoxies
Silane, trade name KH550.
Above-mentioned graphene oxide is modified the preparation method of filter paper：The condition of the ultrasonic disperse is preferably：Ultrasonic power
250W~300W, 25 DEG C~30 DEG C of ultrasonic temperature, ultrasonic time 2~3 hours.
Above-mentioned graphene oxide is modified the preparation method of filter paper：Naturally the time dried is preferably 24~36 small
When.
Graphene oxide prepared by the method for the invention is modified filter paper.
Graphene oxide of the present invention is modified application of the filter paper in profit quick separating and oiliness sewage treatment.
It is experimentally confirmed that graphene oxide of the present invention, which is modified filter paper, can realize profit quick separating, separative efficiency can
Reach more than 98%.The filter paper stability is good, repeats and utilizes.
There is the present invention prominent effect to be：
(1) present invention proposes a kind of graphene oxide and is modified filter paper and preparation method thereof, and technique is simple and convenient, can advise greatly
Prepared by mould, be conducive to expanding application of the graphene oxide in water-oil separating.
(2) using " bridging effect " of coupling agent, the adhesion between graphene oxide and filter paper is increased by covalent bond,
It effectively prevent graphene oxide coming off from filter paper top layer, it is further to improve the performance that graphene oxide is modified filter paper.
(3) graphene oxide that the present invention is provided is modified low filter paper cost, physical and chemical performance stabilization, can freely cut simultaneously
Reuse, discarded filter paper can centralized burning processing, it is to avoid secondary pollution.
Embodiment
To be easy to further understand the present invention, the present invention is further elaborated for the following example.These embodiments have
There is certain representativeness, but all examples can not be included, be only used for clearly illustrating the present invention, rather than limit this hair
Bright scope.
Embodiment 1
(1) 1g graphene oxides and 0.05g Silane coupling agent KH550s are dissolved in 20mL deionized waters and 80mL absolute ethyl alcohols
Mixed solution in, ultrasonic disperse is uniform, and (condition of ultrasonic disperse is：Ultrasonic power 300W, 30 DEG C of ultrasonic temperature, ultrasonic time
2 hours).Common qualitative filter paper (30~50 microns of average pore size) is impregnated in above-mentioned mixed liquor, ultrasonic disperse 1 hour, room
The lower nature of temperature dries 24 hours, that is, obtains graphene oxide and be modified filter paper.
(2) water-oil separating is carried out using common filter, graphene oxide, which is modified folded filter paper funnel, inserts
In filter tunnel.At room temperature (25 DEG C), by petroleum ether (60~90 DEG C of boiling point) and deionized water by volume 1:3 ratio is mixed
Close, ultrasonic disperse is quickly poured into filter paper into oil water mixture, profit quick separating can be achieved, separative efficiency can reach 98%
More than.The filter paper stability is good, repeats and utilizes.
Embodiment 2
(1) 1g graphene oxides and 0.1g Silane coupling agent KH550s are dissolved in 20mL deionized waters and 80mL absolute ethyl alcohols
Mixed solution in, ultrasonic disperse is uniform, and (condition of ultrasonic disperse is：Ultrasonic power 250W, 25 DEG C of ultrasonic temperature, ultrasonic time
3 hours).Common qualitative filter paper (30~50 microns of average pore size) is impregnated in above-mentioned mixed liquor, ultrasonic disperse 2 hours, room
The lower nature of temperature dries 24 hours, that is, obtains graphene oxide and be modified filter paper.
(2) water-oil separating is carried out using common filter, graphene oxide, which is modified folded filter paper funnel, inserts
In filter tunnel.At room temperature (25 DEG C), by kerosene and deionized water by volume 1:2 ratio mixing, ultrasonic disperse is into profit
Mixture, is quickly poured into filter paper, and profit quick separating can be achieved, and separative efficiency can reach more than 99%.The filter paper stability
It is good, repeat and utilize.
Embodiment 3
(1) 2g graphene oxides and 0.1g Silane coupling agent KH550s are dissolved in 30mL deionized waters and 70mL absolute ethyl alcohols
Mixed solution in, ultrasonic disperse is uniform, and (condition of ultrasonic disperse is：Ultrasonic power 400W, 35 DEG C of ultrasonic temperature, ultrasonic time
1 hour).Common quantitative filter paper (30~50 microns of average pore size) is impregnated in above-mentioned mixed liquor, ultrasonic disperse 3 hours, room
The lower nature of temperature dries 36 hours, that is, obtains graphene oxide and be modified filter paper.
(2) water-oil separating is carried out using common filter, graphene oxide, which is modified folded filter paper funnel, inserts
In filter tunnel.At room temperature (25 DEG C), by kerosene and deionized water by volume 1:4 ratio mixing, ultrasonic disperse is into profit
Mixture, is quickly poured into filter paper, and profit quick separating can be achieved, and separative efficiency can reach more than 99%.The filter paper stability
It is good, repeat and utilize.
Embodiment 4
(1) 1g graphene oxide 0.1g Silane coupling agent KH550s are dissolved in 20mL deionized waters and 80mL absolute ethyl alcohols
In mixed solution, ultrasonic disperse is uniform, and (condition of ultrasonic disperse is：Ultrasonic power 200W, 25 DEG C of ultrasonic temperature, ultrasonic time 3
Hour).Common middling speed qualitative filter paper (30-50 microns of average pore size) is impregnated in above-mentioned mixed liquor, ultrasonic disperse 2 hours,
Dry naturally at room temperature 36 hours, that is, obtain graphene oxide and be modified filter paper.
(2) water-oil separating is carried out using common filter, graphene oxide, which is modified folded filter paper funnel, inserts
In filter tunnel.At room temperature (25 DEG C), by kerosene and deionized water by volume 1:3 ratio mixing, ultrasonic disperse is into profit
Mixture, is quickly poured into filter paper, and profit quick separating can be achieved, and separative efficiency can reach more than 99%.The filter paper stability
It is good, repeat and utilize.
Embodiment 5
(1) 2g graphene oxides and 0.2g Silane coupling agent KH550s are dissolved in 20mL deionized waters and 80mL absolute ethyl alcohols
Mixed solution in, ultrasonic disperse is uniform, and (condition of ultrasonic disperse is：Ultrasonic power 350W, 30 DEG C of ultrasonic temperature, ultrasonic time
2 hours).Common middling speed qualitative filter paper (30-50 microns of average pore size) is impregnated in above-mentioned mixed liquor, ultrasonic disperse 2 hours,
Dry naturally at room temperature 36 hours, that is, obtain graphene oxide and be modified filter paper.
(2) water-oil separating is carried out using common filter, graphene oxide, which is modified folded filter paper funnel, inserts
In filter tunnel.At room temperature (25 DEG C), by kerosene and deionized water by volume 1:2 ratio mixing, ultrasonic disperse is into profit
Mixture, is quickly poured into filter paper, and profit quick separating can be achieved, and separative efficiency can reach more than 99%.The filter paper stability
It is good, repeat and utilize.
Embodiment 5
(1) 2g graphene oxides and 0.1g Silane coupling agent KH550s are dissolved in 20mL deionized waters and 80mL absolute ethyl alcohols
Mixed solution in, ultrasonic disperse is uniform, and (condition of ultrasonic disperse is：Ultrasonic power 250W, 30 DEG C of ultrasonic temperature, ultrasonic time
3 hours).Common middling speed qualitative filter paper (30-50 microns of average pore size) is impregnated in above-mentioned mixed liquor, ultrasonic disperse 2 hours,
Dry naturally at room temperature 36 hours, that is, obtain graphene oxide and be modified filter paper.
(2) water-oil separating is carried out using common filter, graphene oxide, which is modified folded filter paper funnel, inserts
In filter tunnel.At room temperature (25 DEG C), by petroleum ether (60~90 DEG C of boiling point) and deionized water by volume 1:4 ratio is mixed
Close, ultrasonic disperse is quickly poured into filter paper into oil water mixture, profit quick separating can be achieved, separative efficiency can reach 99%
More than.The filter paper stability is good, repeats and utilizes.
Embodiment 6
(1) 2g graphene oxides and 0.1g Silane coupling agent KH550s are dissolved in 20mL deionized waters and 80mL absolute ethyl alcohols
Mixed solution in, ultrasonic disperse is uniform, and (condition of ultrasonic disperse is：Ultrasonic power 250W, 30 DEG C of ultrasonic temperature, ultrasonic time
3 hours).Common middling speed qualitative filter paper (30-50 microns of average pore size) is impregnated in above-mentioned mixed liquor, ultrasonic disperse 2 hours,
Dry naturally at room temperature 36 hours, that is, obtain graphene oxide and be modified filter paper.
(2) water-oil separating is carried out using common filter, graphene oxide, which is modified folded filter paper funnel, inserts
In filter tunnel.At room temperature (25 DEG C), by n-hexane and deionized water by volume 1:3 ratio mixing, ultrasonic disperse is into oil
Aqueous mixtures, are quickly poured into filter paper, and profit quick separating can be achieved, and separative efficiency can reach more than 99%.The filter paper is stable
Property it is good, repeat and utilize.
Claims (3)
- To use dip coating 1. a kind of graphene oxide is modified the preparation method of filter paper, by filter paper impregnation in graphene oxide with In the mixed solution of silane coupler, ultrasonic disperse then takes out, and puts and dries naturally at room temperature, produces graphene oxide modification Filter paper；Wherein, the filter paper is the qualitative or quantitative filter paper of common middling speed that average pore size is 1~50 micron；The ultrasonic disperse Condition be：Ultrasonic power 200W~400W, 25 DEG C~35 DEG C of ultrasonic temperature, ultrasonic time 1~3 hour；It is described to dry naturally Time be 12~36 hoursIt is characterized in that：The mixed solution of the graphene oxide and silane coupler is made according to the following ratio, graphene oxide:Silane coupler: Deionized water:Absolute ethyl alcohol is 1g~5g:0.05g~0.5g:20mL~30mL:70mL~80mL.
- 2. graphene oxide according to claim 1 is modified the preparation method of filter paper, it is characterised in that：The graphite oxide The mixed solution of alkene and silane coupler is made according to the following ratio, graphene oxide:Silane coupler:Deionized water:Anhydrous second Alcohol is 1g~2g:0.05g~0.2g:20mL:80mL.
- 3. graphene oxide according to claim 1 or 2 is modified the preparation method of filter paper, it is characterised in that：The silane Coupling agent is 3- aminopropyl triethoxysilanes, trade name KH550.
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| US11607652B2 (en) * | 2018-02-07 | 2023-03-21 | National University Corporation Kobe University | Composite separation membrane |
| CN110079358B (en) * | 2019-05-24 | 2021-03-30 | 上海贵通新材料科技有限公司 | Preparation method of demulsifier material |
| GB202000280D0 (en) | 2020-01-09 | 2020-02-26 | Institute Of Tech Sligo | Filter |
| CN113802412B (en) * | 2021-08-19 | 2022-07-26 | 江苏众立生包装科技有限公司 | Anti-wrinkle and anti-wet tipping paper |
| CN115160652B (en) * | 2022-07-29 | 2023-04-07 | 华南理工大学 | Magnetic nanocellulose-carbon composite aerogel and preparation method and application thereof |
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