CN109225144A - A kind of preparation method of fluoroquinolone antibiotics adsorbent - Google Patents
A kind of preparation method of fluoroquinolone antibiotics adsorbent Download PDFInfo
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- 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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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- 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
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- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
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- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/36—Organic compounds containing halogen
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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
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Abstract
The invention discloses a kind of preparation methods of fluoroquinolone antibiotics adsorbent, comprising the following steps: 1), metal salt and organic ligand are dissolved in n,N-Dimethylformamide obtain solution A；2), turn solution A to enter in hydrothermal reaction kettle, after reacting 20h-30h under the conditions of 100 DEG C -160 DEG C, be cooled to room temperature, obtain intermediate product after centrifugation, washing, drying；3), intermediate product and cobaltous sulfate are dissolved in organic solvent, are cooled to room temperature after magnetic agitation, dry the quinolone antibiotics adsorbent after centrifugation.The adsorbent aperture is 1.5-3.2nm, specific surface area 698-1143m2/g.Preparation step of the invention is simple, at low cost, high to the removal efficiency of quinolone antibiotics pollutant, has a extensive future.
Description
Technical field
The present invention relates to the applications of metal organic framework (MOF) material, and in particular to a kind of cobaltous sulfate-UIO material to
Remove the technical field of fluoroquinolone antibiotics adsorbent preparation.
Background technique
Fluoroquinolone antibiotics are a kind of artificial synthesized class antibacterials, and because of its good anti-bacterial effect, effect is strong, are easy quilt
It absorbs, is widely used in clinic.As a kind of common drug, fluoroquinolone antibiotics are once by mankind or animal
It is unable to be absorbed completely after intake, remaining part is most to enter environment by human waste in the form of substance, causes dirt
Dye.Because it is long-term it is unreasonable use such drug, lead to its residual and accumulation in the environment, to endanger environmental health.Therefore,
A kind of new trend will necessarily be become to the Adsorption of fluoquinolone pollutant.
Metal-organic framework materials are by metal ion or metallic compound and organic ligand by being self-assembly of orderly
The novel skeletal porous material of one kind of structure, type are broadly divided into ZIF series, MIL series and UIO series.Wherein UIO system
Column framework material has more activated adoption sites, provides more touch opportunities for pollutant because of large specific surface area, because
This, UIO series framework material is considered as a kind of good adsorbent material.But in practical applications, UIO series framework material pair
The removal efficiency of fluoroquinolone antibiotics is only capable of reaching 50% or so.Therefore, UIO series framework material is improved to fluorine in environment
The Adsorption efficiency of quinolone antibiotics is of great significance.
Summary of the invention
The technical problem to be solved by the present invention is to overcome metal-organic framework materials in the prior art to fluoroquinolones
The removal efficiency of antibiotic is only capable of reaching 50% defect, provides a kind of preparation method of fluoroquinolone antibiotics adsorbent.
In order to solve the above-mentioned technical problems, the present invention provides the following technical solutions:
A kind of preparation method of fluoroquinolone antibiotics adsorbent, comprising the following steps:
1), metal salt and organic ligand are dissolved in n,N-Dimethylformamide and obtain solution A；
2), turn solution A to enter in hydrothermal reaction kettle, after reacting 20h-30h under the conditions of 100 DEG C -160 DEG C, be cooled to room temperature,
Intermediate product are obtained after centrifugation, washing, drying；
3), intermediate product and cobaltous sulfate are dissolved in organic solvent, are cooled to room temperature after magnetic agitation, it is dry after centrifugation
Obtain the quinolone antibiotics adsorbent.
Further, the metal salt be zirconium chloride, the organic ligand be terephthalic acid (TPA), zirconium chloride with it is right
The molar ratio of phthalic acid is 1:1-3.
Further, the organic solvent is methanol, one of ethyl alcohol or acetonitrile.
Further, the mass ratio of intermediate product and cobaltous sulfate is 1:0.1-1 in the step 3).
Further, the temperature of magnetic agitation is 25 DEG C -50 DEG C in the step 3).
Further, drying temperature is 60 DEG C -100 DEG C in the step 3), drying time 12h-24h.
The beneficial effects obtained by the present invention are as follows being: fluoroquinolone antibiotics adsorbent uniform particle sizes produced by the present invention,
Mechanicalness is strong, and high to fluoroquinolones antibiosis adsorption efficiency in environment, adsorption capacity is big, the fluoquinolone in adsorption treatment environment
There are bright prospects in the application of class antibiotic.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the scanning electron microscope schematic diagram of the resulting fluoroquinolone antibiotics adsorbent of the embodiment of the present invention 1；
Fig. 2 is the infrared spectroscopy schematic diagram of the resulting fluoroquinolone antibiotics adsorbent of the embodiment of the present invention 1；
Fig. 3 is the X-ray diffraction schematic diagram of the resulting fluoroquinolone antibiotics adsorbent of the embodiment of the present invention 1.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1
A kind of preparation method of fluoroquinolone antibiotics adsorbent, comprising the following steps:
1) zirconium chloride, is weighed by the molar ratio of 1:1 and terephthalic acid (TPA) is dissolved in the n,N-Dimethylformamide of 40mL
In obtain solution A；
2), turn solution A to enter in hydrothermal reaction kettle, after being reacted for 24 hours under the conditions of 120 DEG C, be cooled to room temperature, be centrifuged, washed
It washs, drying obtains intermediate product afterwards for 24 hours at 80 DEG C；
3) intermediate product and cobaltous sulfate are dissolved in methanol by the mass ratio of 1:0.5, and obtain B solution, by solution B at 40 DEG C
Magnetic agitation 1h；
4), be cooled to room temperature, be centrifuged, through at 80 DEG C it is dry for 24 hours the fluoroquinolone antibiotics adsorbent.
Embodiment 2
A kind of preparation method of fluoroquinolone antibiotics adsorbent, comprising the following steps:
1) zirconium chloride, is weighed by the molar ratio of 1:2 and terephthalic acid (TPA) is dissolved in the n,N-Dimethylformamide of 40mL
In obtain solution A；
2), turn solution A to enter in hydrothermal reaction kettle, after being reacted for 24 hours under the conditions of 120 DEG C, be cooled to room temperature, be centrifuged, washed
It washs, drying obtains intermediate product afterwards for 24 hours at 80 DEG C；
3) intermediate product and cobaltous sulfate are dissolved in methanol by the mass ratio of 1:1, and obtain B solution, by solution B in 40 DEG C of magnetic
Power stirs 1h；
4), be cooled to room temperature, be centrifuged, through at 80 DEG C it is dry for 24 hours the fluoroquinolone antibiotics adsorbent.
Embodiment 3
A kind of preparation method of fluoroquinolone antibiotics adsorbent, comprising the following steps:
1) zirconium chloride, is weighed by the molar ratio of 1:3 and terephthalic acid (TPA) is dissolved in the n,N-Dimethylformamide of 40mL
In obtain solution A；
2), turn solution A to enter in hydrothermal reaction kettle, after being reacted for 24 hours under the conditions of 120 DEG C, be cooled to room temperature, be centrifuged, washed
It washs, drying obtains intermediate product afterwards for 24 hours at 80 DEG C；
3) intermediate product and cobaltous sulfate are dissolved in ethyl alcohol by the mass ratio of 1:0.8, and obtain B solution, by solution B at 25 DEG C
Magnetic agitation 1h；
4), be cooled to room temperature, be centrifuged, through at 60 DEG C it is dry for 24 hours the fluoroquinolone antibiotics adsorbent.
Embodiment 4
A kind of preparation method of fluoroquinolone antibiotics adsorbent, comprising the following steps:
1) zirconium chloride, is weighed by the molar ratio of 1:1 and terephthalic acid (TPA) is dissolved in the n,N-Dimethylformamide of 30mL
In obtain solution A；
2), turn solution A to enter in hydrothermal reaction kettle, after being reacted for 24 hours under the conditions of 120 DEG C, be cooled to room temperature, be centrifuged, washed
It washs, drying obtains intermediate product afterwards for 24 hours at 80 DEG C；
3) intermediate product and cobaltous sulfate are dissolved in acetonitrile by the mass ratio of 1:0.1, and obtain B solution, by solution B at 50 DEG C
Magnetic agitation 1h；
4), be cooled to room temperature, be centrifuged, through at 80 DEG C it is dry for 24 hours the fluoroquinolone antibiotics adsorbent.
Embodiment 5
A kind of preparation method of fluoroquinolone antibiotics adsorbent, comprising the following steps:
1) zirconium chloride, is weighed by the molar ratio of 1:2 and terephthalic acid (TPA) is dissolved in the n,N-Dimethylformamide of 60mL
In obtain solution A；
2), turn solution A to enter in hydrothermal reaction kettle, after being reacted for 24 hours under the conditions of 120 DEG C, be cooled to room temperature, be centrifuged, washed
It washs, drying obtains intermediate product afterwards for 24 hours at 80 DEG C；
3) intermediate product and cobaltous sulfate are dissolved in methanol by the mass ratio of 1:0.2, and obtain B solution, by solution B at 40 DEG C
Magnetic agitation 1h；
4), be cooled to room temperature, be centrifuged, through at 100 DEG C it is dry for 24 hours the fluoroquinolone antibiotics adsorbent.
1 fluoroquinolone antibiotics adsorbent specific surface area performance indicator of table
| Embodiment | Specific surface area (m2/g) | Aperture (nm) |
| Embodiment 1 | 1143 | 1.6 |
| Embodiment 2 | 911 | 1.5 |
| Embodiment 3 | 1032 | 3.2 |
| Embodiment 4 | 698 | 2.7 |
| Embodiment 5 | 1102 | 2.8 |
The fluoroquinolone antibiotics adsorbent prepared in 0.01g embodiment 1-5 is weighed respectively, and 10mL is added and contains
In the lavo-ofloxacin hydrochloride aqueous solution of 100mg/L, 1h are shaken in 25 DEG C of water-baths, to obtain clear liquid new through T6 after being filtered, being diluted
The test of century ultraviolet-visible spectrophotometer, adsorbance are calculated by formula.
The fluoroquinolone antibiotics adsorbent prepared in 3 parts of 0.01g embodiments 1 is weighed, 10mL is separately added into and contains
The hydrochloric acid Ba Luo that the hydrochloric acid sand that Ciprofloxacin Hydrochloride, the 10mL of 100mg/L contains 50mg/L replaces husky star and 10mL to contain 50mg/L
Sha Xingzhong shakes 1h in 25 DEG C of water-baths, filtered, dilute after obtain clear liquid and surveyed through T6 new century ultraviolet-visible spectrophotometer
Examination, adsorbance are calculated by formula.
The adsorption capacity of the 2 resulting adsorbent of embodiment 1-5 of table
Table 2 the result shows that, the fluoroquinolone antibiotics adsorbent that the present invention prepares is to fluoroquinolone antibiotics
Adsorption efficiency it is high, especially to lavo-ofloxacin hydrochloride adsorbance with higher, adsorbance is up to 70.21mg/g.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (7)
1. a kind of preparation method of fluoroquinolone antibiotics adsorbent, which comprises the following steps:
1), metal salt and organic ligand are dissolved in n,N-Dimethylformamide and obtain solution A；
2), turn solution A to enter in hydrothermal reaction kettle, under the conditions of 100 DEG C -160 DEG C react 20h-30h after, be cooled to room temperature, through from
Intermediate product are obtained after the heart, washing, drying；
3), intermediate product and cobaltous sulfate are dissolved in organic solvent, are cooled to room temperature after magnetic agitation, dry institute after centrifugation
State quinolone antibiotics adsorbent.
2. the method according to claim 1, wherein the metal salt is zirconium chloride, the organic ligand
For terephthalic acid (TPA), the molar ratio of zirconium chloride and terephthalic acid (TPA) is 1:1-3.
3. method according to claim 1 or 2, which is characterized in that the organic solvent is methanol, in ethyl alcohol or acetonitrile
One kind.
4. the method according to claim 1, wherein the mass ratio of intermediate product and cobaltous sulfate is in the step 3)
1:0.1-1.
5. the method according to claim 1, wherein the temperature of magnetic agitation is 25 DEG C -50 in the step 3)
℃。
6. being done the method according to claim 1, wherein drying temperature is 60 DEG C -100 DEG C in the step 3)
The dry time is 12h-24h.
7. the method according to claim 1, wherein the resulting adsorbent aperture of step 1) be 1.5-3.2nm, than
Surface area is 698-1143m2/g。
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Cited By (5)
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| CN109704432A (en) * | 2019-01-23 | 2019-05-03 | 河南师范大学 | One kettle way prepares UIO-66-NH2The method of/functional monomer composite material and its application in absorption antibiotic |
| CN110075814A (en) * | 2019-05-06 | 2019-08-02 | 苏州科技大学 | A kind of two dimension N doping magnetic ionic liquids class zeolite imidazole ester nano material and preparation method thereof, purposes |
| CN115582100A (en) * | 2022-11-07 | 2023-01-10 | 安徽农业大学 | Preparation method and application of three-dimensional bimetal MOFs (metal-organic frameworks) macroscopic microbead material |
| CN116284811A (en) * | 2023-02-05 | 2023-06-23 | 吉林大学 | Preparation method and application of Ga-MOGs |
| CN116272893A (en) * | 2023-01-13 | 2023-06-23 | 昆明理工大学 | Adsorbent for efficiently removing ciprofloxacin in water and preparation method thereof |
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| CN116272893A (en) * | 2023-01-13 | 2023-06-23 | 昆明理工大学 | Adsorbent for efficiently removing ciprofloxacin in water and preparation method thereof |
| CN116284811A (en) * | 2023-02-05 | 2023-06-23 | 吉林大学 | Preparation method and application of Ga-MOGs |
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Application publication date: 20190118 |