CN108273472A - A kind of preparation method of efficient selective absorption selenite radical adsorbent - Google Patents
A kind of preparation method of efficient selective absorption selenite radical adsorbent Download PDFInfo
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- CN108273472A CN108273472A CN201810044075.8A CN201810044075A CN108273472A CN 108273472 A CN108273472 A CN 108273472A CN 201810044075 A CN201810044075 A CN 201810044075A CN 108273472 A CN108273472 A CN 108273472A
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- adsorbent
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- 229940082569 selenite Drugs 0.000 title claims abstract description 26
- 239000003463 adsorbent Substances 0.000 title claims abstract description 22
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 5
- 238000011026 diafiltration Methods 0.000 claims description 5
- 238000002474 experimental method Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000002798 spectrophotometry method Methods 0.000 claims description 5
- 150000001621 bismuth Chemical class 0.000 claims description 4
- 239000003446 ligand Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 239000011669 selenium Substances 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 239000007795 chemical reaction product Substances 0.000 claims 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims 1
- XWNOTOKFKBDMAP-UHFFFAOYSA-N [Bi].[N+](=O)(O)[O-] Chemical compound [Bi].[N+](=O)(O)[O-] XWNOTOKFKBDMAP-UHFFFAOYSA-N 0.000 claims 1
- 229910052786 argon Inorganic materials 0.000 claims 1
- 238000001354 calcination Methods 0.000 claims 1
- 238000003763 carbonization Methods 0.000 claims 1
- 235000019253 formic acid Nutrition 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- -1 selenite radical Chemical class 0.000 abstract description 27
- 239000012621 metal-organic framework Substances 0.000 abstract description 19
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 abstract description 10
- 239000012922 MOF pore Substances 0.000 abstract description 7
- 239000010865 sewage Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 229920006395 saturated elastomer Polymers 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000002594 sorbent Substances 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- 238000000151 deposition Methods 0.000 abstract 1
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- BDSBMINFNXSZQP-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid;methanol Chemical compound OC.OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 BDSBMINFNXSZQP-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000012467 final product Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- MCAHWIHFGHIESP-UHFFFAOYSA-N selenous acid Chemical compound O[Se](O)=O MCAHWIHFGHIESP-UHFFFAOYSA-N 0.000 description 2
- 229910001051 Magnalium Inorganic materials 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- 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
- B01J20/223—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]
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/106—Selenium compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses the preparation methods that a kind of efficient selective adsorbs selenite radical adsorbent, belong to sewage treatment field.The adsorbent is using five water bismuth nitrates and trimesic acid as raw material, with abundant active adsorption sites, special organic metal framework object (MOFs) micropore canals structure, there is higher adsorbance when this material is used for selenite radical adsorbent (saturated extent of adsorption can reach 255.3mg/g).Traditional selenite radical adsorbent is depositing many defects, and selectivity is relatively low, and saturated extent of adsorption is smaller, the relatively narrow pH scope of applications, and principle is low in the presence of the competing ions of larger concentration.Therefore, one kind is developed efficiently, with ph stability, the adsorbent of highly selective selenite radical ion has great importance.In the present invention, the preparation of bismuthino MOF (BI MOF) adsorbent is very simple and convenient, and its special MOF pore passage structure having can further ensure its efficient absorption property, is very promising selenite radical sorbent material.
Description
Technical field
The invention belongs to sewage treatment fields, and in particular to a kind of preparation of efficient selective absorption selenite radical adsorbent
Method.
Background technology
Selenium in sewage mainly in the form of selenite radical ion and selenic acid radical ion existing for, but due to relatively low
The toxicity of the selenite radical ion of valence state is better than selenic acid radical ion, therefore the selenite radical ion in treated sewage has
Higher priority.And the mode for commonly using processing selenite radical ion at present has：Sedimentation, filtering, ion exchange, UF membrane and
Absorption.However, for other several processing means, adsorption treatment mode seems more efficiently, economic and practical and suction
Attached dose is more prone to synthesize.So absorption is the optimal selection of selenite radical ion in current treated sewage.It is common to inhale
Attached dose has several classes：(ferrimanganic bimetallic aoxidizes for metal oxide (aluminium oxide, iron oxide, calcium oxide), bimetallic oxide
Object) and double-metal hydroxide (magnalium double-metal hydroxide).However, because there is apparent lack in above several adsorbents
Sunken and insufficient (low-down saturated extent of adsorption, slower adsorption equilibrium, the unstability under inclined strong acid and strong base environment, and
Low-down selectivity).Therefore, it develops one kind efficiently, there is extraordinary stability, highly selective selenous acid
Root adsorbent is very urgent for the selenite radical in treated sewage.Based on the bismuth oxide of business for selenous acid
Root has certain absorption property, however because its specific surface area is smaller, pore passage structure is undeveloped, is unfavorable for selenite radical and its
Active adsorption sites adequately contact.Therefore it is solution to develop a kind of novel bismuthino adsorbent for having more bigger serface
The certainly key of this problem.And this special materials of Bi-MOF meet above all kinds of requirements, and it is real by adsorbing
Demonstrate its remarkable absorption property.Therefore, one kind that this kind of material will be irreplaceable in sewage treatment field is novel
Material.
Invention content
The present invention is prepared for can be used as the tool of selenite radical adsorbent using the bismuth salt of abundance and ligand as raw material
There is the sorbent material Bi-MOF of special pore passage structure.
Preparation process of the present invention is simple, does not need expensive device, and products obtained therefrom quality high-performance is good, and stability is good, selection
Property by force future selenite radical and the application of other Anion-adsorptions in there is bright foreground.
A kind of preparation method of efficient selective absorption selenite radical adsorbent, manufacturing process include the following steps：
1) Bi that configuration 30mL mass concentrations are 2.5mg/mL3+Methanol solution, addition 30mL mass concentrations are 12.5 mg/
The trimesic acid methanol solution of mL, Bi is obtained after stirring3+Trimesic acid mixed solution；
2) mixed solution is heated to reaction in constant temperature oven, by 100 DEG C -180 DEG C, the reaction time is at 12h-48h
Reason, obtains product A；
3) by after above-mentioned product A absolute methanol diafiltrations, 60 DEG C are dried to obtain final product Bi-MOF；
4) above-mentioned adsorbent B i-MOF is used as in selenite radical adsorption experiment, and is surveyed with NITRATE BY FLAME ATOMIC spectrophotometry
Try its absorption property.
The raw material that the present invention uses is mainly bismuth salt, and amount of storage is big in the earth's crust, and synthesizes and amplify economic and practical, production
Amount is big.
Adsorbent with special MOF pore passage structures prepared by the method for the present invention is with highest selenite radical so far
Absorption property has very fast adsorption equilibrium characteristic, and absorption property is highly stable under pH 4-11 environment, Yi Ji
Also has extraordinary selectivity in the environment of counter anion under very big concentration.
Description of the drawings
Fig. 1 is the SEM figures for the Bi-MOF with special MOF pore passage structures that specific embodiment 1 obtains.
Fig. 2 is the XRD diagram for the Bi-MOF with special MOF pore passage structures that specific embodiment 1 obtains.
Fig. 3 is that specific embodiment 1 obtains the stability diagram in pH 4-11 with the Bi-MOF of special MOF pore passage structures,
It is not influenced the absorption property of selenite radical by pH value variation substantially, also demonstrates its outstanding absorption stability.
Fig. 4 is that specific embodiment 1 obtains the selectivity with the Bi-MOF of special MOF pore passage structures, is in concentration ratio
In the presence of 2000 competing ions, there is extraordinary selectivity.
Fig. 5 is that specific embodiment 1 obtains the isothermal adsorption concentration curve with the Bi-MOF of special MOF pore passage structures, Bi-MOF
A more satisfactory maximum saturation adsorbance can be reached.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, the common skill in this field
The every other embodiment that art personnel are obtained under the premise of without creative work, shall fall within the protection scope of the present invention.
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
1) Bi that configuration 30mL mass concentrations are 2.5mg/mL3+Methanol solution, addition 30mL mass concentrations are 12.5 mg/
The trimesic acid methanol solution of mL, Bi is obtained after stirring3+Trimesic acid mixed solution；
2) mixed solution is heated to reaction in constant temperature oven, by 120 DEG C, the reaction time is to handle for 24 hours, obtains product
A；
3) by after above-mentioned product A absolute methanol diafiltrations, 60 DEG C are dried to obtain final product Bi-MOF；
4) above-mentioned adsorbent B i-MOF is used as in selenite radical adsorption experiment, and is surveyed with NITRATE BY FLAME ATOMIC spectrophotometry
Try its absorption property.
Embodiment 2
1) Bi that configuration 30mL mass concentrations are 2.5mg/mL3+Methanol solution, addition 30mL mass concentrations are 12.5 mg/
The trimesic acid methanol solution of mL, Bi is obtained after stirring3+Trimesic acid mixed solution；
2) mixed solution is heated to reaction in constant temperature oven, by 150 DEG C, the reaction time is to handle for 24 hours, obtains product
A；
3) by after above-mentioned product A absolute methanol diafiltrations, 60 DEG C are dried to obtain final product Bi-MOF；
4) above-mentioned adsorbent B i-MOF is used as in selenite radical adsorption experiment, and is surveyed with NITRATE BY FLAME ATOMIC spectrophotometry
Try its absorption property.
Embodiment 3
1) Bi that configuration 30mL mass concentrations are 2.5mg/mL3+Methanol solution, addition 30mL mass concentrations are 12.5 mg/
The trimesic acid methanol solution of mL, Bi is obtained after stirring3+Trimesic acid mixed solution；
2) mixed solution is heated to reaction in constant temperature oven, by 100,110,130,140,160,170,180 DEG C,
Reaction time be 12h, for 24 hours, 36h, 48h processing, obtain product A；
3) by after above-mentioned product A absolute methanol diafiltrations, 60 DEG C are dried to obtain final product Bi-MOF；
4) above-mentioned adsorbent B i-MOF is used as in selenite radical adsorption experiment, and is surveyed with NITRATE BY FLAME ATOMIC spectrophotometry
Try its absorption property.
It should be understood that although with reference to its illustrative embodiment, particularly shown and description is carried out to the present invention,
It should be understood by those skilled in the art that without departing substantially from by it is as defined in the claims the present invention spirit and
Under conditions of range, the variation of various forms and details can be carried out wherein, can carry out arbitrary group of various embodiments
It closes.
Claims (5)
1. a kind of preparation method of efficient selective absorption selenite radical adsorbent, it is characterised in that the method includes following steps
Suddenly：
1) a certain amount of bismuth salt is dissolved into a certain amount of absolute methanol, Bi is obtained after stirring3+Methanol solution；
2) a certain amount of ligand is dissolved into a certain amount of absolute methanol, ligand methanol solution is obtained after stirring；
3) above two solution is mixed, obtains mixed solution, handle to obtain reaction product A by hydro-thermal reaction；
4) by above-mentioned reaction product A absolute methanol diafiltrations repeatedly, it is dried to obtain product B, product B is this novel sub- selenium
Acid group adsorbent B i-MOF；
5) above-mentioned adsorbent B i-MOF is used as in selenite radical adsorption experiment, and it is tested with NITRATE BY FLAME ATOMIC spectrophotometry
Absorption property.
2. preparation method according to claim 1, which is characterized in that the bismuth salt described in step 1) is five water nitric acid
Bismuth, solution temperature are room temperature, and the mass concentration of addition is 2.5mg/mL.
3. preparation method according to claim 1, which is characterized in that the equal benzene three that the ligand described in step 2) uses
Formic acid, solution temperature are room temperature, and the mass concentration of addition is 12.5mg/mL.Carbonization technique is calcined 1 hour for 600-1000 DEG C,
Calcination atmosphere is argon gas.
4. preparation method according to claim 1, which is characterized in that the hydrothermal temperature range described in step 3)
It is 100 DEG C -180 DEG C, reaction time 12h-48h.
5. preparation method according to claim 1, which is characterized in that described in step 4), in vacuum drying oven, 60 DEG C
Desciccate A obtains Bi-MOF.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810044075.8A CN108273472B (en) | 2018-01-10 | 2018-01-10 | Preparation method of adsorbent capable of efficiently and selectively adsorbing selenious acid roots |
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|---|---|---|---|
| CN201810044075.8A CN108273472B (en) | 2018-01-10 | 2018-01-10 | Preparation method of adsorbent capable of efficiently and selectively adsorbing selenious acid roots |
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| Publication Number | Publication Date |
|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109888206A (en) * | 2019-01-23 | 2019-06-14 | 江苏理工学院 | A kind of lithium ion battery negative material Bi/Bi2O3/ C and its preparation and application |
| CN111729662A (en) * | 2020-06-23 | 2020-10-02 | 东莞理工学院 | Preparation method and application of MXene membrane material for in-situ growth of Bi-MOF |
| CN113333002A (en) * | 2021-06-12 | 2021-09-03 | 景德镇陶瓷大学 | Preparation method of CdS quantum dot-loaded bismuth oxide composite visible light catalytic material and product prepared by same |
| CN113351226A (en) * | 2021-06-12 | 2021-09-07 | 景德镇陶瓷大学 | Petal-shaped loaded ZnIn2S4Preparation method of bismuth oxide composite visible light catalytic material and product prepared by same |
| CN114835233A (en) * | 2022-06-01 | 2022-08-02 | 闽江学院 | Method for rapidly removing chloride ions in wastewater by using bismuth-based metal organic framework material |
| CN114904498A (en) * | 2022-05-30 | 2022-08-16 | 天津城建大学 | Preparation method and application of adsorption material PEHA-CAU-17 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109888206A (en) * | 2019-01-23 | 2019-06-14 | 江苏理工学院 | A kind of lithium ion battery negative material Bi/Bi2O3/ C and its preparation and application |
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| CN111729662A (en) * | 2020-06-23 | 2020-10-02 | 东莞理工学院 | Preparation method and application of MXene membrane material for in-situ growth of Bi-MOF |
| CN113333002A (en) * | 2021-06-12 | 2021-09-03 | 景德镇陶瓷大学 | Preparation method of CdS quantum dot-loaded bismuth oxide composite visible light catalytic material and product prepared by same |
| CN113351226A (en) * | 2021-06-12 | 2021-09-07 | 景德镇陶瓷大学 | Petal-shaped loaded ZnIn2S4Preparation method of bismuth oxide composite visible light catalytic material and product prepared by same |
| CN113333002B (en) * | 2021-06-12 | 2023-03-03 | 景德镇陶瓷大学 | Preparation method of CdS quantum dot-loaded bismuth oxide composite visible light catalytic material and product prepared by same |
| CN113351226B (en) * | 2021-06-12 | 2023-04-18 | 景德镇陶瓷大学 | Petal-shaped loaded ZnIn 2 S 4 Preparation method of bismuth oxide composite visible light catalytic material and product prepared by same |
| CN114904498A (en) * | 2022-05-30 | 2022-08-16 | 天津城建大学 | Preparation method and application of adsorption material PEHA-CAU-17 |
| CN114835233A (en) * | 2022-06-01 | 2022-08-02 | 闽江学院 | Method for rapidly removing chloride ions in wastewater by using bismuth-based metal organic framework material |
| CN114835233B (en) * | 2022-06-01 | 2023-09-12 | 闽江学院 | Method for rapidly removing chloride ions in wastewater by bismuth-based metal organic framework material |
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