CN109081394A - A kind of preparation method of the magnetic nanoparticle for sewage treatment - Google Patents
A kind of preparation method of the magnetic nanoparticle for sewage treatment Download PDFInfo
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- CN109081394A CN109081394A CN201811050455.9A CN201811050455A CN109081394A CN 109081394 A CN109081394 A CN 109081394A CN 201811050455 A CN201811050455 A CN 201811050455A CN 109081394 A CN109081394 A CN 109081394A
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- magnetic nanoparticle
- preparation
- added
- aliphatic chain
- nanoparticle
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Classifications
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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
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
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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
-
- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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
Abstract
The present invention provides a kind of preparation methods of magnetic nanoparticle for sewage treatment, the described method comprises the following steps: (1) Fe3O4Magnetic nanoparticle is handled with alkaline solution；(2) magnetic nanoparticle made from step (1) is modified with tetramethoxy-silicane, (3) coupling of magnetic nanoparticle made from step (1) is had to the PEG polymer of photoreactive groups and aliphatic chain, obtained scion grafting has the magnetic nanoparticle of the PEG of aliphatic chain.Magnetic nanoparticle prepared by the present invention has hydrophilic, hydrophobic dual structure, and good and dispersed and oiliness pollutant can be kept to have good compatibility in aqueous solution, has the advantages that be easily achieved that quickly clean oil droplet, oil removal rate high.Magnetic nanoparticle scion grafting stable structure prepared by the present invention simultaneously can be recycled for multiple times after recycling washing, its cycle-index is up to 15-20 times after actual measurement.
Description
Technical field
The present invention relates to synthesize a kind of magnetic nanoparticle that can be applied to sewage treatment, and in particular to a kind of surface scion grafting
The Fe of PEG molecule with aliphatic chain3O4Magnetic nanoparticle.
Background technique
Magnetic nanoparticle has a good application prospect in sewage treatment field, existing technology mainly by using
Amphiphilic polymers are to Fe3O4Nanoparticle carries out surface grafting modification, makes polymer and the affine absorption of oiliness pollutant, in turn
The quick separating of magnetic nanoparticle in water is realized under the action of an external magnetic field.Oiliness pollution of this kind of technology in processing sewage
Object has many advantages, such as simple process, high-efficient, easy recycling, recycling, for solving oil exploitation, transport, in process
Water pollution problems have huge help.However, the existing magnetic nanoparticle with efficient degreasing effect often faces work
Complicated, at high cost, stability the is poor problem of skill limits its a large amount of popularization and application.
Summary of the invention
Above of the existing technology in order to solve the problems, such as, the purpose of the present invention is to provide a kind of for sewage treatment
Magnetic nanoparticle preparation method simplifies the preparation process of existing magnetic nanoparticle, reduces production cost, improves nano-magnetic
The stability of particle.
It is relatively easy that the present invention provides a kind of preparation process, it is easy to accomplish the magnetic nanoparticle preparation side being prepared on a large scale
Method, technical solution are as follows:
A kind of preparation method of the magnetic nanoparticle for sewage treatment, the described method comprises the following steps:
(1) by Fe3O4Magnetic nanoparticle is added in alkaline aqueous solution, and heating stirring 1h is added to percent by volume after filtering
For in the ethanol water of 40%-60%；
(2) above-mentioned suspension is adjusted to acidity, ultrasonic disperse 15min, N using pH adjusting agent2It protects lower heating stirring and is added dropwise
Tetramethoxy-silicane stirs 12h at 55-65 DEG C after being added dropwise, is cleaned after filtering with ether or acetone, and vacuum is dry at room temperature
It is dry；
(3) magnetic nanoparticle after drying is added in deionized water, mass percent 0.5-2% is added has light reaction
The PEG polymer of group and aliphatic chain, N2The lower stirring of protection, and using the ultraviolet light 1h of wavelength 240-300nm, it collects
Fe3O4Particle, scion grafting, which can be obtained, the magnetic nanoparticle of PEG of aliphatic chain.
Further, Fe described in step (1)3O4Nanoparticle is prepared by the following method: under inert gas shielding, will be rubbed
You are than the FeCl for 1:22•4H2O and FeCl3•6H2O is dissolved in water, then 80-90 DEG C of stirring is added concentrated ammonia liquor and is adjusted to pH
8.5-9.5 reaction 2h obtains Fe3O4Nanoparticle.
Preferably, alkaline aqueous solution described in step (1) be sodium hydroxide, potassium hydroxide, sodium acetate, ammonium hydroxide, phosphate,
The combination of one or more of carbonate, organic amine, alkaline aqueous solution pH are 8.5-9.5.
Preferably, step (1) heating temperature is 55-65 DEG C.
Preferably, step (2) pH adjusting agent is the combination of one or more of hydrochloric acid, acetic acid, sulfuric acid, phosphoric acid, is adjusted
PH is 4.0-4.5 after section.
Preferably, step (2) heating temperature is 55-65 DEG C.
Preferably, the addition quality of step (2) described tetramethoxy-silicane is Fe3O4The 0.1-0.2% of quality.
Further, PEG polymer described in step (3) has the following structure:
,
Wherein R1 、R2For the aliphatic chain C with phenyl ring and/or ester bond2-C30Aliphatic chain, n=20-40.
Preferably, the additive amount of PEG polymer is Fe3O4The 0.5-2% of quality.
Preferably, the oiliness pollutant includes at least one of crude oil, diesel oil, gasoline, vegetable oil, organosilane ester,
The sewage pH is between 3-11.
The utility model has the advantages that the present invention provides a kind of magnetic nanoparticle preparation method for sewage treatment, system of the present invention
Standby magnetic nanometer has the advantage that 1. magnetic nanoparticles prepared by the present invention have hydrophilic, hydrophobic dual structure,
It can keep good and dispersed in aqueous solution and oiliness pollutant has good compatibility, have and be easily achieved
Quickly clean the high advantage of oil droplet, oil removal rate；2. magnetic nanoparticle scion grafting stable structure prepared by the present invention, after recycling washing
It can be recycled for multiple times, its cycle-index is up to 15-20 times after actual measurement.
Specific embodiment
The invention will now be further described with reference to specific embodiments, but examples are merely exemplary, not to this hair
Bright range constitutes any restrictions.It will be understood by those skilled in the art that without departing from the spirit and scope of the invention
Can with the details and forms of the technical scheme of the invention are modified or replaced, but these modification and replacement each fall within it is of the invention
In protection scope.
Embodiment 1
By 25g Fe3O4The NaOH aqueous solution of pH=9.0 of 100mL, 60 DEG C of heating stirring 1h, filtering is added in magnetic nanoparticle
It is added to isometric ethanol solution afterwards.Above-mentioned suspension is adjusted to pH=4.0, ultrasonic disperse 15min, N using glacial acetic acid2It protects
It protects lower 60 DEG C of heating stirrings and 0.25g tetramethoxy-silicane is added dropwise, 12h is stirred after being added dropwise at 60 DEG C, with third after filtering
Ketone cleaning, is dried in vacuo at room temperature.Magnetic nanoparticle after drying is added in deionized water, 0.5g 1- nitrine second is added
Ester group polyethylene glycol monooleate (the ethylene glycol degree of polymerization is 30), N2The lower stirring of protection, and use the ultraviolet lighting of wavelength 280nm
1h is penetrated, Fe is collected3O4Particle.The magnetic nanoparticle of preparation is used to emulsify edible oily sewage disposal, pH=7, turbidity=
900NTU, particle dosage are 200mg/L, and removal rate is greater than 95%, and cycle-index is more than 20 times.
Embodiment 2
By 25g Fe3O4The NaOH aqueous solution of pH=9.0 of 100mL, 60 DEG C of heating stirring 1h, filtering is added in magnetic nanoparticle
It is added to isometric ethanol solution afterwards.Above-mentioned suspension is adjusted to pH=4.0, ultrasonic disperse 15min, N using glacial acetic acid2It protects
It protects lower 60 DEG C of heating stirrings and 0.25g tetramethoxy-silicane is added dropwise, 12h is stirred after being added dropwise at 60 DEG C, with third after filtering
Ketone cleaning, is dried in vacuo at room temperature.Magnetic nanoparticle after drying is added in deionized water, 0.5g1- nitrine ethyl ester is added
Base polyethylene glycol monooleate (the ethylene glycol degree of polymerization is 30), N2The lower stirring of protection, and use the ultraviolet light of wavelength 280nm
1h collects Fe3O4Particle.The magnetic nanoparticle of preparation is used to emulsify edible oily sewage disposal, pH=11, turbidity=900NTU,
Particle dosage is 200mg/L, and removal rate is greater than 95%, and cycle-index is more than 15 times.
Embodiment 3
By 25g Fe3O4The ammonia spirit of pH=9.0 of 100mL, 60 DEG C of heating stirring 1h, after filtering are added in magnetic nanoparticle
It is added to isometric ethanol solution.Above-mentioned suspension is adjusted to pH=4.0, ultrasonic disperse 15min, N using hydrochloric acid2Under protection
Simultaneously 0.25g tetramethoxy-silicane is added dropwise in 60 DEG C of heating stirrings, stirs 12h at 60 DEG C after being added dropwise, clear with acetone after filtering
It washes, is dried in vacuo at room temperature.Magnetic nanoparticle after drying is added in deionized water, it is poly- that 0.5g1- nitrine ethoxycarbonyl is added
Ethylene glycol docosane ester (the ethylene glycol degree of polymerization is 20), N2The lower stirring of protection, and use the ultraviolet light of wavelength 280nm
1h collects Fe3O4Particle.The magnetic nanoparticle of preparation is used for emulsified crude oil sewage treatment, pH=5, turbidity=1000NTU, grain
Sub- dosage is 200mg/L, and removal rate is greater than 95%, and cycle-index is more than 17 times.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, that is done any repairs
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the magnetic nanoparticle for sewage treatment, which is characterized in that the method includes following steps
It is rapid:
(1) by Fe3O4Magnetic nanoparticle is added in alkaline aqueous solution, and heating stirring 1h, being added to percent by volume after filtering is
In the ethanol water of 40-60%；
(2) above-mentioned suspension is adjusted to acidity, ultrasonic disperse 15min, N using pH adjusting agent2It protects lower heating stirring and is added dropwise four
Methoxy silane stirs 12h at 55-65 DEG C after being added dropwise, is cleaned after filtering with ether or acetone, and vacuum is dry at room temperature
It is dry；
(3) magnetic nanoparticle after drying is added in deionized water, mass percent 0.5-2% is added has light reaction
The PEG polymer of group and aliphatic chain, N2The lower stirring of protection, and using the ultraviolet light 1h of wavelength 240-300nm, it collects
Fe3O4Particle, scion grafting, which can be obtained, the magnetic nanoparticle of PEG of aliphatic chain.
2. preparation method according to claim 1, which is characterized in that Fe described in step (1)3O4Nanoparticle is by as follows
Method preparation: under inert gas shielding, the FeCl for being 1:2 by molar ratio2•4H2O and FeCl3•6H2O is dissolved in water, and 80-90 DEG C is stirred
It mixes, concentrated ammonia liquor is then added by pH and is adjusted to 8.5-9.5, reaction 2h obtains Fe3O4Nanoparticle.
3. preparation method according to claim 1, which is characterized in that alkaline aqueous solution described in step (1) is hydroxide
The combination of one or more of sodium, potassium hydroxide, sodium acetate, ammonium hydroxide, phosphate, carbonate, organic amine, alkaline aqueous solution pH are
8.5-9.5。
4. preparation method according to claim 1, which is characterized in that step (1) heating temperature is 55-65 DEG C.
5. preparation method according to claim 1, which is characterized in that step (2) pH adjusting agent be hydrochloric acid, acetic acid,
The combination of one or more of sulfuric acid, phosphoric acid, pH is 4.0-4.5 after adjusting.
6. preparation method according to claim 1, which is characterized in that step (2) heating temperature is 55-65 DEG C.
7. preparation method according to claim 1, which is characterized in that the addition matter of step (2) described tetramethoxy-silicane
Amount is Fe3O4The 0.1-0.2% of quality.
8. preparation method according to claim 1, which is characterized in that PEG polymer described in step (3) has following knot
Structure:
,
Wherein R1 、R2For the aliphatic chain C with phenyl ring and/or ester bond2-C30Aliphatic chain, n=20-40.
9. preparation method according to claim 1, which is characterized in that the additive amount of PEG polymer is Fe3O4Quality
0.5-2%。
10. the magnetic nanoparticle purposes after the scion grafting that preparation method according to claim 1 obtains is to separate sewage
In oiliness pollutant, the oiliness pollutant includes at least one of crude oil, diesel oil, gasoline, vegetable oil, organosilane ester,
The sewage pH is between 3-11.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811050455.9A CN109081394A (en) | 2018-09-10 | 2018-09-10 | A kind of preparation method of the magnetic nanoparticle for sewage treatment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811050455.9A CN109081394A (en) | 2018-09-10 | 2018-09-10 | A kind of preparation method of the magnetic nanoparticle for sewage treatment |
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| CN109081394A true CN109081394A (en) | 2018-12-25 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103736433A (en) * | 2014-01-24 | 2014-04-23 | 福州大学 | Hydrophobic magnetic mesoporous microsphere as well as preparation method and application thereof |
| CN103937478A (en) * | 2014-04-16 | 2014-07-23 | 东北石油大学 | Preparation method of nanofluid for improving oil recovery |
| EP2804186A1 (en) * | 2013-05-14 | 2014-11-19 | King Saud University | Coated magnetite nanoparticles, method for the preparation thereof and their use |
| CN106497599A (en) * | 2016-11-16 | 2017-03-15 | 杭州电子科技大学 | Surface charge and the preparation method and application of the controllable pH responsive type magnetic demulsifiers of hydrophilic and hydrophobic |
| CN108246280A (en) * | 2018-02-01 | 2018-07-06 | 王建伟 | A kind for the treatment of process of ozone catalytic degradation of dye waste water |
| CN108384573A (en) * | 2018-01-31 | 2018-08-10 | 天津大学 | A kind of preparation method and application of hydrophilic magnetic Nano material |
-
2018
- 2018-09-10 CN CN201811050455.9A patent/CN109081394A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2804186A1 (en) * | 2013-05-14 | 2014-11-19 | King Saud University | Coated magnetite nanoparticles, method for the preparation thereof and their use |
| CN103736433A (en) * | 2014-01-24 | 2014-04-23 | 福州大学 | Hydrophobic magnetic mesoporous microsphere as well as preparation method and application thereof |
| CN103937478A (en) * | 2014-04-16 | 2014-07-23 | 东北石油大学 | Preparation method of nanofluid for improving oil recovery |
| CN106497599A (en) * | 2016-11-16 | 2017-03-15 | 杭州电子科技大学 | Surface charge and the preparation method and application of the controllable pH responsive type magnetic demulsifiers of hydrophilic and hydrophobic |
| CN108384573A (en) * | 2018-01-31 | 2018-08-10 | 天津大学 | A kind of preparation method and application of hydrophilic magnetic Nano material |
| CN108246280A (en) * | 2018-02-01 | 2018-07-06 | 王建伟 | A kind for the treatment of process of ozone catalytic degradation of dye waste water |
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Application publication date: 20181225 |
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