CN113856633B - Bimetallic coordination polymer adsorbent, preparation method and application thereof - Google Patents
Bimetallic coordination polymer adsorbent, preparation method and application thereof Download PDFInfo
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- CN113856633B CN113856633B CN202110862084.XA CN202110862084A CN113856633B CN 113856633 B CN113856633 B CN 113856633B CN 202110862084 A CN202110862084 A CN 202110862084A CN 113856633 B CN113856633 B CN 113856633B
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 37
- 239000013256 coordination polymer Substances 0.000 title claims abstract description 36
- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 78
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000011259 mixed solution Substances 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 20
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- YYGZWQNDFRCZIF-UHFFFAOYSA-N 2,5-bis(sulfanyl)terephthalic acid Chemical compound OC(=O)C1=CC(S)=C(C(O)=O)C=C1S YYGZWQNDFRCZIF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 150000002500 ions Chemical class 0.000 claims description 13
- 239000010936 titanium Substances 0.000 claims description 11
- 238000001179 sorption measurement Methods 0.000 abstract description 25
- 239000013335 mesoporous material Substances 0.000 abstract description 6
- 238000004090 dissolution Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 description 18
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 12
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 10
- 238000003795 desorption Methods 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 229920001661 Chitosan Polymers 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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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
- B01J20/223—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
- C02F2101/20—Heavy metals or heavy metal compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention relates to a bimetallic coordination polymer adsorbent, a preparation method and application thereof, and belongs to the technical field of mesoporous material preparation. Mixing 2, 5-dimercapto terephthalic acid, zirconium chloride and DMF, and stirring the mixture at room temperature until complete dissolution; dropwise adding titanium isopropoxide into the mixed solution A, continuously stirring until the titanium isopropoxide is completely mixed in the dropwise adding process, adding methanol into the mixture, stirring to obtain a mixed solution B, carrying out hydrothermal reaction at 130-150 ℃, washing the obtained solid with DMF and methanol for two times respectively to remove unreacted parts, respectively soaking the washed solid in DMF and methanol solution, and finally drying the solid in vacuum to obtain the bimetallic coordination polymer adsorbent. The bimetallic coordination polymer adsorbent is applied to the adsorption recovery of lead in a solution.
Description
Technical Field
The invention relates to a bimetallic coordination polymer adsorbent, a preparation method and application thereof, and belongs to the technical field of mesoporous material preparation.
Background
Lead has the advantages of ductility, corrosion resistance, easy alloying with other metals, and the like, and is widely applied to national defense and science and technology. However, with the rapid development of world economy and the continual innovation in related technical fields, the demand for lead is increasing. The supply of lead cannot meet the requirements of the related art due to the over-exploitation of primary lead ores. Second, industrial production produces a large amount of wastewater containing lead ions. The lead-containing ion wastewater not only pollutes the ecological environment, but also can harm the health of human bodies. Therefore, the development of a green and efficient lead ion treatment technology and a wastewater remediation technology has great significance for human development.
The adsorption method has the advantages of low cost, easy regeneration, flexibility, no secondary pollution and the like, and is widely concerned. A variety of adsorption materials including graphene oxide, cellulose, activated carbon, and chitosan have been used to remove heavy metals from wastewater. Most of the adsorption materials lack structural and functional adjustability and have low adsorption capacity, which motivates people to find novel efficient materials. Metal coordination polymers are mixed inorganic-organic materials composed of metal ions and ligands. The advantages of high porosity, unique structure, large specific surface area, customizable functions before and after synthesis and the like are brought into wide attention. However, it is still difficult to synthesize bimetallic coordination polymers with tailored properties, high efficiency and selectivity.
Disclosure of Invention
Aiming at the problems and the defects existing in the prior art, the invention provides a bimetallic coordination polymer adsorbent, a preparation method and application thereof. The bimetallic coordination polymer is used for efficiently and selectively recovering lead ions in a solution, and has the advantages of low process cost, easiness in regeneration, simplicity in preparation and excellent selective reusability. The invention is realized by the following technical scheme.
A bimetallic coordination polymer adsorbent having the structural formula:
。
a preparation method of a bimetallic coordination polymer adsorbent comprises the following specific steps:
step 1, mixing 2, 5-dimercapto terephthalic acid, zirconium chloride and DMF, and stirring the mixture at room temperature until the mixture is completely dissolved; dropwise adding titanium isopropoxide into the mixed solution A, continuously stirring until the titanium isopropoxide is completely mixed in the dropwise adding process, adding methanol into the mixture, and stirring to obtain a mixed solution B;
and 2, carrying out hydrothermal reaction on the mixed solution B obtained in the step 1 at 130-150 ℃, washing the obtained solid twice with DMF and methanol respectively to remove unreacted parts, soaking the washed solid in DMF and methanol solution respectively, and finally drying the solid in vacuum to obtain the bimetallic coordination polymer adsorbent which is named as Ti/Zr-DBMD.
The ratio of 2, 5-dimercapto terephthalic acid, zirconium chloride and DMF in step 1 was 8.69:0.57:50mmol/mmol/mL.
The mol ratio of the zirconium chloride to the titanium isopropoxide in the step 1 is 0.57:3.78.
The ratio of titanium isopropoxide to methanol in the step 1 is 3.78:50mmol/mL.
A bimetallic coordination polymer adsorbent is applied to the adsorption recovery of lead in solution.
The above-mentioned organic and inorganic reagents, which are not shown in concentrations, are commercially available analytical products.
The beneficial effects of the invention are as follows:
(1) The bimetallic coordination polymer adsorbent prepared by the invention is mainly used for adsorbing and recovering lead ions from a solution, and has good adsorption capacity on the lead ions.
(2) The preparation method of the invention is simple, flexible and low in cost, and has good economic and practical application values.
(3) The bimetallic coordination polymer adsorbent disclosed by the invention is nontoxic and harmless, has high performance, is easy to separate, has good selectivity and can be repeatedly used, and does not cause secondary pollution to the environment.
In conclusion, the mesoporous material adsorbent for adsorbing and recovering lead has great potential in the aspect of adsorbing and recovering lead ions.
Detailed Description
The invention will be further described with reference to the following specific embodiments.
Example 1
The bimetallic coordination polymer adsorbent has the structural formula:
。
the preparation method of the bimetallic coordination polymer adsorbent comprises the following specific steps:
step 1, 8.69 mmole of 2, 5-dimercapto terephthalic acid, 0.57 mmole of zirconium chloride and 50 mmole of LDMF are mixed, and the mixture is stirred at room temperature until complete dissolution; 3.78mmol of titanium isopropoxide is added into 50mL of mixed solution A (the dropping speed is 10 drops/min, each 10 drops is 1 mL), the mixture is continuously stirred until the mixture is completely mixed during the dropping process, and then methanol is added into the mixture and stirred to obtain mixed solution B; wherein the ratio of 2, 5-dimercapto terephthalic acid, zirconium chloride and DMF is 8.69:0.57:50mmol/mmol/mL; the mol ratio of the zirconium chloride to the titanium isopropoxide is 0.57:3.78; the ratio of titanium isopropoxide to methanol is 3.78:50mmol/mL;
and 2, carrying out hydrothermal reaction on the mixed solution B obtained in the step 1 for 24 hours at 130 ℃, washing the obtained solid twice with DMF and methanol respectively to remove unreacted parts, soaking the washed solid in 100mL of methanol solution for 24 hours and 100mL of methanol solution for 24 hours respectively, and finally drying the solid in vacuum to prepare the bimetallic coordination polymer adsorbent which is named as Ti/Zr-DBMD.
And (3) measuring the lead ion adsorption performance:
40mg of Ti/Zr-DBMD was added to 40mL of a lead solution for adsorption experiments, the pH of the lead ion solution was 4, the lead ion concentration was 10mg/L, and five repetition experiments were performed. All repeatability experiments use mixed solution (mixed according to the volume ratio of 1:1) with thiourea and hydrochloric acid concentration as desorbing agent, desorb lead ions on the adsorbent by the desorbing agent after each adsorption experiment is finished, and carry out next adsorption experiment on the eluted solid. The desorption time is 24 hours, the solid products after desorption are respectively washed for 3 times by thiourea and distilled water, and the next adsorption experiment is carried out after vacuum drying. The concentration of the remaining lead ions in the filtrate was 0.36mg/L as measured by ICP-OES, the adsorption rate was 96.4%, and the desorption rate was 82.7%. The invention shows that the bimetallic coordination polymer mesoporous material adsorbent Ti/Zr-DBMD can be recycled.
Example 2
The bimetallic coordination polymer adsorbent has the structural formula:
。
the preparation method of the bimetallic coordination polymer adsorbent comprises the following specific steps:
step 1, 8.69 mmole of 2, 5-dimercapto terephthalic acid, 0.57 mmole of zirconium chloride and 50 mmole of LDMF are mixed, and the mixture is stirred at room temperature until complete dissolution; 3.78mmol of titanium isopropoxide is dripped into 50mL of mixed solution A (the dripping speed is 10 drops/min, each 10 drops is 1 mL), the mixture is continuously stirred until the mixture is completely mixed during the dripping process, and then methanol is added into the mixture and the obtained mixed solution B is stirred; wherein the ratio of 2, 5-dimercapto terephthalic acid, zirconium chloride and DMF is 8.69:0.57:50mmol/mmol/mL; the mol ratio of the zirconium chloride to the titanium isopropoxide is 0.57:3.78; the ratio of titanium isopropoxide to methanol is 3.78:50mmol/mL;
and 2, carrying out hydrothermal reaction on the mixed solution B obtained in the step 1 for 48 hours at 150 ℃, washing the obtained solid twice with DMF and methanol respectively to remove unreacted parts, soaking the washed solid in 200mL of methanol solution for 24 hours and 200mL of methanol solution for 24 hours respectively, and finally drying the solid in vacuum to prepare the bimetallic coordination polymer adsorbent which is named as Ti/Zr-DBMD.
And (3) measuring the lead ion adsorption performance:
40mg of Ti/Zr-DBMD was added to 40mL of a lead solution for adsorption experiments, the pH of the lead ion solution was 4, the lead ion concentration was 10mg/L, and five repetition experiments were performed. All repeatability experiments use mixed solution (mixed according to the volume ratio of 1:1) with thiourea and hydrochloric acid concentration as desorbing agent, desorb lead ions on the adsorbent by the desorbing agent after each adsorption experiment is finished, and carry out next adsorption experiment on the eluted solid. The desorption time is 24 hours, the solid products after desorption are respectively washed for 3 times by thiourea and distilled water, and the next adsorption experiment is carried out after vacuum drying. The concentration of the remaining lead ions in the filtrate was determined by ICP-OES to be 0.13mg/L, the adsorption rate was 98.7%, and the desorption rate was 96.1%. The invention shows that the bimetallic coordination polymer mesoporous material adsorbent Ti/Zr-DBMD can be recycled.
Example 3
The bimetallic coordination polymer adsorbent has the structural formula:
。
the preparation method of the bimetallic coordination polymer adsorbent comprises the following specific steps:
step 1, 8.69 mmole of 2, 5-dimercapto terephthalic acid, 0.57 mmole of zirconium chloride and 50 mmole of LDMF are mixed, and the mixture is stirred at room temperature until complete dissolution; 3.78mmol of titanium isopropoxide is dripped into 50mL of mixed solution A (the dripping speed is 10 drops/min, each 10 drops is 1 mL), the mixture is continuously stirred until the mixture is completely mixed during the dripping process, and then methanol is added into the mixture and the obtained mixed solution B is stirred; wherein the ratio of 2, 5-dimercapto terephthalic acid, zirconium chloride and DMF is 8.69:0.57:50mmol/mmol/mL; the mol ratio of the zirconium chloride to the titanium isopropoxide is 0.57:3.78; the ratio of titanium isopropoxide to methanol is 3.78:50mmol/mL;
and 2, carrying out hydrothermal reaction on the mixed solution B obtained in the step 1 at 140 ℃ for 36h, washing the obtained solid twice with DMF and methanol respectively to remove unreacted parts, soaking the washed solid in 150mL of methanol solution for 24h and 150mL of methanol solution for 24h respectively, and finally drying the solid in vacuum to obtain the bimetallic coordination polymer adsorbent which is named as Ti/Zr-DBMD.
And (3) measuring the lead ion adsorption performance:
40mg of Ti/Zr-DBMD was added to 40mL of a lead solution for adsorption experiments, the pH of the lead ion solution was 4, the lead ion concentration was 10mg/L, and five repetition experiments were performed. All repeatability experiments use mixed solution (mixed according to the volume ratio of 1:1) with thiourea and hydrochloric acid concentration as desorbing agent, desorb lead ions on the adsorbent by the desorbing agent after each adsorption experiment is finished, and carry out next adsorption experiment on the eluted solid. The desorption time is 24 hours, the solid products after desorption are respectively washed for 3 times by thiourea and distilled water, and the next adsorption experiment is carried out after vacuum drying. The concentration of the remaining lead ions in the filtrate was determined by ICP-OES to be 0.22mg/L, the adsorption rate was 97.8%, and the desorption rate was 84.5%. The invention shows that the bimetallic coordination polymer mesoporous material adsorbent Ti/Zr-DBMD can be recycled.
While the specific embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes may be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (5)
1. A preparation method of a bimetallic coordination polymer adsorbent is characterized in that: the method comprises the following specific steps:
step 1, mixing 2, 5-dimercapto terephthalic acid, zirconium chloride and DMF, and stirring the mixture at room temperature until the mixture is completely dissolved to obtain a mixed solution A; dropwise adding titanium isopropoxide into the mixed solution A, continuously stirring until the titanium isopropoxide is completely mixed in the dropwise adding process, adding methanol into the mixture, and stirring to obtain a mixed solution B;
step 2, carrying out hydrothermal reaction on the mixed solution B obtained in the step 1 in a baking oven at 130-150 ℃, washing the obtained solid with DMF and methanol for two times to remove unreacted parts, respectively soaking the washed solid in DMF and methanol solution, and finally drying the solid in vacuum to prepare the bimetallic coordination polymer adsorbent which is named as Ti/Zr-DBMD;
the structural formula of the bimetallic coordination polymer adsorbent is as follows:
。
2. the method for preparing the bimetallic coordination polymer adsorbent as set forth in claim 1, wherein: the ratio of 2, 5-dimercapto terephthalic acid, zirconium chloride and DMF in step 1 was 8.69:0.57:50mmol/mmol/mL.
3. The method for preparing the bimetallic coordination polymer adsorbent as set forth in claim 1, wherein: the molar ratio of zirconium chloride to titanium isopropoxide in step 1 was 0.57:3.78.
4. The method for preparing the bimetallic coordination polymer adsorbent as set forth in claim 1, wherein: the ratio of titanium isopropoxide to methanol in step 1 was 3.78:50mmol/mL.
5. Use of a bimetallic coordination polymer adsorbent prepared by the method for preparing a bimetallic coordination polymer adsorbent according to claim 1 for adsorbing and recovering lead ions in solution.
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