CN106588781A - Preparation of nanomaterial ZIF-67 and application thereof in quick adsorption of anionic dye - Google Patents
Preparation of nanomaterial ZIF-67 and application thereof in quick adsorption of anionic dye Download PDFInfo
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- CN106588781A CN106588781A CN201611190135.4A CN201611190135A CN106588781A CN 106588781 A CN106588781 A CN 106588781A CN 201611190135 A CN201611190135 A CN 201611190135A CN 106588781 A CN106588781 A CN 106588781A
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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]
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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
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/56—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
- C07D233/58—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring nitrogen atoms
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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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for preparing a microporous nanomaterial ZIF-67and an application of the ZIF-67 in quick adsorption of dye. The material is prepared by reacting divalent metal cobalt salt with a 2-methylimidazole ligand at the room temperature so as to produce a nanoscale microporous crystal adopting a similar topology structure. The prepared nanomaterial ZIF-67 is dispersed in a dye aqueous solution and can be used as a novel adsorbent to efficiently and quickly remove anionic dye in water; the adsorption capacity is 91.69 mg/g for 1 h, which is close to the equilibrium adsorption capacity, and the removal rate can reach 90.91%. The nanomaterial ZIF-67 is expected to be further used for adsorbing other pollutants in water and combined with other adsorbing materials for preparation of ZIF-67-based composite materials.
Description
Technical field
The present invention relates to method and ZIF-67 that micropore nanophase materials ZIF-67 is prepared under a kind of room temperature are used for quick suction
The application of attached dye, belongs to nano material and adsorption technology field.
Background technology
Metal-organic framework materials（MOFs）Also referred to as Porous coordination polymer organic and inorganic heterozygosis framework material, by mistake
The multiple tooth organic ligand (mostly polybase and fragrant polyacid) for crossing metal ion or metal cluster and nitrogenous, oxygen etc. is constituted using self assembly
With the periodically netted class zeolitic material of multidimensional, it is a kind of using boundless novel porous materials.Why can cause
The broad interest of people, be on the one hand because metal-organic framework materials possess special hole shape size controllability and can
Modified, the features such as specific surface area is very big, is on the other hand have gentle preparation factor due to MOFs, and preparation process is simply easy
Control, structure it is diversified, unique so that MOFs gas store and separation, optics, magnetics, catalysis, molecular recognition, host and guest
The aspects such as body assembling, chemical sensitisation technology and medical treatment have open market.The pore passage structure of metal-organic framework materials is
It is connected formed by coordination with organo-functional group by inorganic metal ion center, different organic ligands and metal ligand can be made
The metal-organic framework materials of standby Different Pore Structures.It has been found that metal-organic framework materials as adsorbing material compared to
Traditional adsorbing material shows obvious advantage.
The discovery of metal-organic framework materials is derived from early 1990s, has by different metal ions and dentation
Machine ligands are combined, and Robson and Hoskins et al. prepare the material that many possesses special construction first.Nineteen ninety,
Robson et al. has synthesized a kind of novel porous structure material, and anion can be swapped.MOFs materials now
Design is prepared, metal ion concentrates on divalent transition metal ion, and organic ligand is headed by neutral pyridines and its derivant.
But the structure constructed using these metal ions, organic ligand has certain limitation, coordination site is few, coordination mode
Single, the stability of material of formation is poor, so as to constrain further research and the commercial Application of material.
Class zeolite imidazole ester framework compound（Zeolitic imidazolate frameworks, ZIFs）It is a kind of new
The MOFs materials of type, ZIFs are that the N atoms on imidazole ring are complexed to the one kind formed in divalent transition metal ion to have
The porous crystalline material of zeolite topological, can just form different structure by the interaction between modulation part or part
ZIFs, becomes a kind of new porous material because of the advantage which combines MOFs and traditional zeolite.ZIFs is except possessing skeleton
Outside multiformity and novelty, also with some other outstanding characteristics.Because the interaction between imidazoles chain and metal ion is higher,
So ZIFs generally has higher heat stability than other MOFs materials（>400℃）.ZIFs also has higher chemistry steady
It is qualitative, ZIF-8 is put in water, benzene, methanol and is flowed back 1-7 days, remain to the relatively stable of holding structure, this is wide for such material
General application is laid a good foundation, and it is good that research also finds that this kind of material is shown at aspects such as catalysis, magnetic, gas storage and separation
Good performance.
And ZIF-67 is similar with ZIF-8 structures, be by divalent cobalt and 2-methylimidazole at room temperature, alcoholic solution or water
The high-purity crystals that quick production is stirred in solution have the heat stability of height simultaneously.Recently, ZIF-67 is received widely
Pay close attention to and have substantial amounts of experiment and research developing its application.
The content of the invention
It is an object of the invention to provide a kind of preparation method of metal-organic framework materials-ZIF-67, prepared material
Material can preferably be scattered in aqueous solution with nano-grade size, and with the organic-inorganic ligands acted on dye molecule, because
And can be used as adsorbent fast and efficiently adsorbing separation ionic dyes from water.
To reach above-mentioned purpose, present invention firstly provides a kind of preparation side of metal-organic framework materials-ZIF-67
Method, which comprises the following steps：A certain amount of divalent cobalt is added the ligand solution that divalent cobalt is formed in solvent, Jing ultrasounds point
Certain hour is reacted at room temperature with after mixing containing 2-methylimidazole ligand solution again after being dissipated to uniformly.It is after reaction terminates, high
Speed is collected by centrifugation the violet solid in reactant liquor, and with solvent, repeatedly immersion and centrifugation obtain solid product, vacuum dried to obtain
To ZIF-67.ZIF-67 adds aqueous dye solutions by a certain percentage as adsorbent, has been capable of achieving after static adsorption certain hour
The ionic dyes that effect is gone in eliminating water.
In the preparation method of above-mentioned micropore nanophase materials ZIF-67, it is preferable that the divalent cobalt for being adopted can be nitre
Sour cobalt, cobaltous acetate, cobaltous sulfate, one kind of cobaltous chloride.
In the preparation method of above-mentioned micropore nanophase materials ZIF-67, it is preferable that solvent is DMF, first
Alcohol, one kind or mixture of deionized water.
In the preparation method of above-mentioned micropore nanophase materials ZIF-67, it is preferable that the mol ratio of divalent cobalt and imidazoles is：
1:0.05~1:0.8。
In the preparation method of above-mentioned micropore nanophase materials ZIF-67, it is preferable that cobalt salt solution concentration is：0.05~
0.6mol/L；Imidazole solution concentration is：0.5 ~ 2mol/L, response time are 20 ~ 24h.
In the preparation method of above-mentioned micropore nanophase materials ZIF-67, it is preferable that centrifugal speed is 2000-4000r/min；
Product cleaning solvent is dehydrated alcohol or absolute methanol or deionized water, and baking temperature is 60-110 DEG C；Drying time be 12 ~
24h。
In the preparation method of above-mentioned micropore nanophase materials ZIF-67, it is preferable that adsorbent addition is 0.5 ~ 5 g/mL,
Scope dye strength scope is 20 ~ 300 g/mL, and Longer absorption times are 10 ~ 600 min.
Beneficial effect：ZIF-67 prepared by the present invention is with the bivalence Co ion and π π that electrostatic interaction is produced with dyestuff
The glyoxaline structure of conjugation, the material can be used for the ionic dyes in adsorption aqueous solution.
Description of the drawings
Fig. 1 is the XRD figure of ZIF-67 nanoparticles prepared by embodiment 1.
Fig. 2 is the BET figures of ZIF-67 nanoparticles prepared by embodiment 1.
Specific embodiment
With reference to embodiment, the present invention is further illustrated, but it is not intended that can practical range to of the invention
Restriction.
Embodiment 1
1.91g Co(NO3)2·6H2O obtains cobalt salt solution, 9.8g2- methyl in being dissolved in 100mL deionized waters and methyl alcohol mixed liquor
Imidazoles is made into 2-methylimidazole solution in being dissolved in 100mL methanol, cobalt salt solution is stirred in the constant temperature oscillator of 150r/min at 30 DEG C
24h is mixed, is added 2-methylimidazole solution to continue stirring 24h and is obtained ZIF-67 dispersion liquids.High speed centrifugation collects gained ZIF-67 grains
Son, is repeatedly overnight soaked to be centrifuged with dehydrated alcohol again and obtains purification ZIF-67, the available purple powder of 80 °C of lower vacuum drying 24h
Last shape ZIF-67.
Test the ZIF-67 for preparing as adsorbent for static adsorption, evaluate and test the performance of absorbing dye in its water,
Dyestuff used is light blue.Aqueous dye solutions of the compound concentration for 100mg/L, weigh the dye that 0.01g adsorbents add 10ml respectively
Material solution, is placed in constant temperature oscillator and keeps frequency of oscillation to be 150 r/min.After adsorbing different time at 30 DEG C, centrifugation
Separating adsorbent and solution, take the dyes concentration after upper solution ultraviolet spectrophotometer determines absorption, by following fixed
Adopted formula calculates dye adsorption amount and clearance of the adsorbent under the adsorption conditionses.The surveyed absorption result is shown in Table 1,
q=(C0-Ct)V/m
R=[(C0-Ct)/ C0]*100%
In formula, q is adsorbance, mg/g；C0With CtSolution concentration before respectively adsorbing and after absorption, mg/L；V absorption used is molten
Liquid is accumulated, L；M be sorbent used quality, g.
Embodiment 2
The micropore nanophase materials ZIF-67 for preparing is used for static adsorption as adsorbent to test with embodiment 1, adsorbs 1 h,
Dye solution wherein used is Congo red aqueous solution, and absorption result is shown in Table 2.
Embodiment 3
The micropore nanophase materials ZIF-67 for preparing is used for static adsorption as adsorbent to test with embodiment 1, adsorbs 1h, its
In dye solution used be crystal violet aqueous solution, absorption result is shown in Table 2.
From figure 1 it appears that experiment presents highly consistent with the crest location and intensity distributions simulated in collection of illustrative plates, say
The bright nanoparticle that obtains is ZIF-67 and purity is higher.Fig. 2 can be seen that adsorption curve urgency when relative pressure is less than 0.05
It is acute to rise, and absorption/desorption curve presents a little stagnant ring, shows that ZIF-67 nanoparticles possess microcellular structure.Say Fig. 1 ~ 2
The bright ZIF-67 for obtaining is provided simultaneously with crystal structure and microcellular structure.
Absorption property can be seen that the adsorbance of 60 min adsorption times in above-described embodiment can reach 120 as shown in Table 1
More than the 98% of min adsorption times, as the increase absorption content of adsorption time gradually rises and tends to be steady, in 180 min
Almost adsorption equilibrium, show adsorbent ZIF-67 can quickly, efficient absorption light blue.
Absorption property can be seen that ZIF-67 is far longer than crystal violet to the clearance of light blue and Congo red as shown in Table 2
Dye solution.As light blue and Congo red belong to anionic dyes, and crystal violet is then cationic dyes, so ZIF-67
The main cause of energy quick adsorption light blue is the SO of dyestuff3 2-With the CO in ZIF-672+Generation electrostatic interaction.Additionally, on dyestuff
Phenyl ring is also beneficial to absorption, but π pi-conjugated effects during quick adsorption with the pi-conjugated effects of imidazoles phenyl ring generation π on ZIF-67
It is weaker than electrostatic interaction.
The sorbent used adsorbance under different adsorption times in 1 embodiment 1 of table.
。
Adsorb the adsorbance under different dyes solution in 2 embodiment of table.
Claims (7)
1.ZIF-67 the preparation of nano material, its preparation method comprise the steps：By divalent cobalt solution and 2-methylimidazole
Certain hour is reacted in solution mixing at room temperature；After reaction terminates, high speed centrifugation collects purple solid product, many times of Jing immersions and
It is vacuum dried after centrifugation again；Gained ZIF-67 nano materials can be as adsorbent efficiently, in quick adsorption water ionic dyes.
2. preparation method according to claim 1, it is characterised in that the divalent cobalt part is cobalt nitrate, cobaltous acetate,
Cobaltous sulfate, one kind of cobaltous chloride.
3. preparation method according to claim 1, it is characterised in that the solvent of the ligand solution is N, N- dimethyl methyls
Amide, methanol, one kind of deionized water or mixture.
4. preparation method according to claim 1, it is characterised in that the mol ratio of divalent cobalt and 2-methylimidazole is：
1:0.05~1:0.8。
5. preparation method according to claim 1, it is characterised in that the divalent cobalt solution concentration is：0.05~
0.6mol/L；2-methylimidazole solution concentration is：0.5 ~ 6mol/L, response time are 2 ~ 24h.
6. preparation method according to claim 1, it is characterised in that centrifugal speed is 2000-8000r/min；It is dried temperature
Spend for 60-110 DEG C；Drying time is 12 ~ 24h.
7. preparation method according to claim 1, it is characterised in that adsorbent addition is 0.5 ~ 5 g/mL, scope dye
Material concentration range is 20 ~ 300 g/mL, and Longer absorption times are 10 ~ 600 min.
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| CN114247430A (en) * | 2022-01-05 | 2022-03-29 | 天津工业大学 | Active dye adsorbent and preparation method thereof |
| CN114505057A (en) * | 2021-12-31 | 2022-05-17 | 石家庄循环化工研究院 | ZIF-8/67 composite crystal adsorbent, preparation method thereof and wastewater purification method |
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