CN108114752A - A kind of preparation method of ZIFs packages inorganic oxide core-shell material - Google Patents

A kind of preparation method of ZIFs packages inorganic oxide core-shell material Download PDF

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CN108114752A
CN108114752A CN201611056748.9A CN201611056748A CN108114752A CN 108114752 A CN108114752 A CN 108114752A CN 201611056748 A CN201611056748 A CN 201611056748A CN 108114752 A CN108114752 A CN 108114752A
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zifs
product
methanol
milliliters
metal salt
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徐杰
王天龙
马红
高进
孙志强
苗虹
聂鑫
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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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
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
    • B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
    • 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]
    • 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
    • B01J20/28014—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
    • B01J20/28016—Particle form
    • B01J20/28019—Spherical, ellipsoidal or cylindrical
    • 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
    • B01J20/28014—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
    • B01J20/28016—Particle form
    • B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • 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
    • B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
    • B01J2531/20—Complexes comprising metals of Group II (IIA or IIB) as the central metal
    • B01J2531/26—Zinc
    • 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
    • B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
    • B01J2531/80—Complexes comprising metals of Group VIII as the central metal
    • B01J2531/84—Metals of the iron group
    • B01J2531/845—Cobalt

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

A kind of method for preparing class zeolitic imidazolate framework material (ZIFs) package inorganic oxide core-shell material, this method is using cuprous oxide or silica as nuclear material, make imidazoles organic ligand and metal salt that coordination polymerization occur on nuclear material surface, continuity ZIFs shells are formed, obtain the Core-shell structure material of ZIFs shells package.This method is simple, mild condition, and universality is strong, has important application value.

Description

A kind of preparation method of ZIFs packages inorganic oxide core-shell material
Technical field
The present invention relates to Material Fields, and in particular to a kind of side for preparing ZIFs package inorganic oxide Core-shell structure materials Method.
Background technology
It is organic that ZIF materials are that the metal with different topology structure to be formed is complexed with imidazoles organic ligand for metal ion Coordination polymer.ZIFs has porosity, adjustability of structure, functional diversity and good thermal stability and chemical stabilization Property, therefore there is a potential using value in many fields, such as catalysis, gas absorption with separating, optical electro-chemistry, drug conduct, Microreactor, sewage disposal etc..
In order to further enhance ZIFs materials in the application of numerous areas, the pattern of material can be adjusted, prepares different dimensional Degree material is achieved.By material preparation into nucleocapsid be efficiently use shape characteristic improve material property one kind have efficacious prescriptions Method.At present, ZIFs Core-shell structure materials are applied in fields such as photocatalysis, molecular size selective, absorption.ZIFs cores Shell structure material traditional preparation methods include droplet stream method, the seed law, self-template, curvature diffusion method.These methods synthesize nucleocapsid All there is certain deficiencies for structure.For example, preparation condition is harsh, apparatus for preparation is complicated, product separation difficulty etc..With right The concern and attention of ZIFs core-shell materials develop mild mode and prepare ZIFs nucleocapsids new method instead of conventional method, tool There are important application value and application prospect.
Compared with having been reported, this synthetic method has the advantage that：(1) this synthetic method is realized carries out core under temperate condition The preparation of shell structure material can avoid, using special synthetic instrument, simplifying complicated synthesis step, solve core-shell material and ZIFs Crystallize mixed questions.(2) the present invention provides suitable in silica and cuprous oxide as mould material, cobalt, copper or zinc The ZIFs systems that ion is formed with 2-methylimidazole have applicability and creativeness.
The content of the invention
It is a kind of by controlling feed way present invention aims at providing, prepare ZIFs package inorganic oxide nucleocapsids The new method of material by the way that feed way ZIFs is controlled to form continuity shell on mould material surface, obtains nucleocapsid knot Structure material, and avoid the ZIFs Crystallizations that largely dissociate in system.
Synthetic method provided by the invention is：(20-40 DEG C) in a mild condition, by controlling feed way, with oxidation Cuprous and silica passes through metal ion and organic ligand 2-methylimidazole coordination polymerization single step reaction system as mould material Obtain ZIFs Core-shell structure materials.Cuprous oxide used includes solid spherical cuprous oxide；Hollow cuprous oxide is spherical, more for individual layer Layer is spherical.Silica used is solid spherical structure.Due to hollow cuprous oxide, dispersion effect is preferable in methyl alcohol, hollow list Layer or the spherical cuprous oxide effect of multilayer are better than solid spherical cuprous oxide.
0.04-0.065 grams of the dosage of cuprous oxide template in the present invention；Silica content is 0.04-0.05 grams.
Solvent for use of the present invention is methanol or ethyl alcohol；Methanol has good dispersion performance and dissolving to template and presoma Property, methanol addition is 30-40 milliliters in template；Methanol addition is 10-30 milliliters in presoma.
Reaction is carried out in three-necked flask at room temperature, at a normal, required presoma cobalt nitrate or zinc nitrate and 2-methylimidazole Methanol solution needs slowly to add in into different templates agent dispersing liquid simultaneously, rapidly joins predecessor, it is possible to create largely free to match somebody with somebody Object is closed, nucleocapsid can not be obtained.Therefore, the optimal charging process of optimization adds in predecessor, optimum response for controlling simultaneously Condition is room temperature, and optimum reacting time 1-2h, charging rate is to be slowly added to simultaneously.Presoma 2-methylimidazole and metal salt Molar ratio is about 4:1-8:1.
Compared with traditional route, route provided by the invention has the following advantages：
1st, the present invention proposes a kind of variation route by the way that feed way is controlled to prepare ZIFs Core-shell structure materials, condition temperature With, it is easy to operate, it is the variation route of a control synthesis ZIFs nucleocapsid.
2nd, the present invention has certain universality.Compared with the traditional production method of ZIFs nucleocapsids, the present invention is not using Nucleocapsid is prepared with template and two kinds of different metal ions, there is preferable universality.
The present invention is described in detail with embodiment below.
Description of the drawings
Fig. 1 is the infrared spectrum of 1 product of example.
Fig. 2 is that the TEM and SEM of 1 product of example scheme.
Fig. 3 is the infrared spectrum of 2 product of example.
Fig. 4 is that the TEM of 2 product of example schemes.
Fig. 5 is that the TEM of 3 product of example schemes.
Fig. 6 is the infrared spectrum of 3 product of example.
Fig. 7 is the infrared spectrum of 4 product of example.
Fig. 8 is the infrared spectrum of 5 product of example.
Fig. 9 is the infrared spectrum of 6 product of example.
Figure 10 is that the TEM of 7 product of example schemes.
Figure 11 is the infrared spectrum of 7 product of example.
Figure 12 is the infrared spectrum of 8 product of example.
Figure 13 is that the TEM of 8 product of example schemes.
Figure 14 is that the TEM of 9 product of example schemes.
Figure 15 is the infrared spectrum of 9 product of example.
Figure 16 is the infrared spectrum of 10 product of example.
Specific embodiment
Embodiment 1：By 0.065 gram of stratiform spherical hollow cuprous oxide, 30 milliliters of methanol is added to 100 milliliters In three-necked flask, by 2-methylimidazole (0.17~0.22 gram) methanol solution and the methanol solution of cobalt nitrate (0.08~0.11 gram) Flask is slowly added to, is stirred simultaneously, stirring holding 1-8h under room temperature normal pressure.Then stop stirring, total overall reaction mixed liquor is turned Move to centrifuge tube.4500rpm is centrifuged, and solid product with methanol is washed for several times, product is put into 80 DEG C of oven dryings 12h collects solid product.Then infrared analysis (FT-IR, Fig. 1) is sampled, observation absorbs peak position.By TEM and SEM to sample Product pattern and size are observed (SEM and TEM, Fig. 2).The result shows that product be Cu2O (hollow)@ZIFs cores Shell structure.
Embodiment 2：By the cuprous oxide of 0.065 gram of solid spherical shape, 30 milliliters of methanol is added to three mouthfuls of 100 milliliters It is in flask, the methanol solution of 2-methylimidazole (0.17~0.22 gram) methanol solution and cobalt nitrate (0.08~0.11 gram) is slow Flask is added in, is stirred simultaneously, stirring holding 1-8h under room temperature normal pressure.Then stop stirring, total overall reaction mixed liquor is transferred to Centrifuge tube.4500rpm is centrifuged, and solid product with methanol is washed for several times, product is put into 80 DEG C of oven drying 12h, is received Collect solid product.Then infrared analysis (FT-IR, Fig. 3) is sampled, observation absorbs peak position.By TEM Fig. 4 to sample topography and Size is observed.Confirmation obtains product as Core-shell structure material.The result shows that product be Cu2O (solid)@ZIFs Nucleocapsid.
Embodiment 3：By the cuprous oxide of 0.065 gram of hollow stratiform spherical shape, 30 milliliters of methanol is added to 100 milliliters In three-necked flask, by 2-methylimidazole (0.17~0.22 gram) methanol solution and the methanol solution of cobalt nitrate (0.08~0.11 gram) Flask is rapidly joined, is stirred simultaneously, stirring holding 1-8h under room temperature normal pressure.Then stop stirring, total overall reaction mixed liquor is turned Move to centrifuge tube.4500rpm is centrifuged, and solid product with methanol is washed for several times, product is put into 80 DEG C of oven dryings 12h collects product and does not obtain ZIFs nucleocapsids.By tem observation product (TEM, Fig. 5) and it is infrared to product analysis not Form nucleocapsid (FT-IR, Fig. 6).
Embodiment 4：By the cuprous oxide of 0.065 gram of hollow stratiform spherical shape, 30 milliliters of methanol is added to 250 milliliters In three-necked flask, by the first of 30 milliliters of 20 ml methanol solution of 2-methylimidazole (0.6225 gram) and cobalt nitrate (0.134 gram) Alcoholic solution is stirred under room temperature normal pressure by being successively slowly added to flask, and keeps 1-8h.Then stirring is stopped, it will be all anti- Mixed liquor is answered to be transferred to centrifuge tube.4500rpm is centrifuged, and solid product with methanol is washed for several times, product is put into 80 DEG C Oven drying 12h collects solid product.Nucleocapsid (FT-IR, Fig. 7) is not formed by infrared analysis product.
Embodiment 5：By the cuprous oxide of 0.065 gram of hollow stratiform spherical shape, 30 milliliters of methanol is added to 100 milliliters In three-necked flask, by 10 ml methanol solution of 2-methylimidazole (0.34 gram) and the methanol of 10 milliliters of cobalt nitrate (0.145 gram) Solution is slowly added to flask, while is stirred under room temperature normal pressure, and keeps 1-8h.Then stirring is stopped, by total overall reaction mixed liquor It is transferred to centrifuge tube.4500rpm is centrifuged, and solid product with methanol is washed for several times, product is put into 80 DEG C of oven dryings 12h collects solid product.Nucleocapsid (FT-IR, Fig. 8) is not formed by infrared analysis product.
Embodiment 6：By the cuprous oxide of 0.065 gram of hollow stratiform spherical shape, 30 milliliters of methanol is added to 100 milliliters In three-necked flask, by the first of 10 milliliters of 10 ml methanol solution of 2-methylimidazole (0.0907 gram) and cobalt nitrate (0.0425 gram) Alcoholic solution is slowly added to flask, stirs simultaneously, is stirred under room temperature normal pressure, and keeps 1-8h.Then stirring is stopped, by total overall reaction Mixed liquor is transferred to centrifuge tube.4500rpm is centrifuged, and solid product with methanol is washed for several times, product is put into 80 DEG C of bakings Case dries 12h, collects solid product.Nucleocapsid (FT-IR, Fig. 9) is not formed by infrared analysis product.
Embodiment 7：By the cuprous oxide of 0.065 gram of solid spherical shape, 30 milliliters of methanol is added to three mouthfuls of 100 milliliters It is in flask, the methanol solution of methylimidazole (0.17~0.22 gram) methanol solution and zinc nitrate (0.08~0.11 gram) is slow Flask is added in, is stirred simultaneously, is stirred under room temperature normal pressure, and keep 1-2h.Then stop stirring, total overall reaction mixed liquor is shifted To centrifuge tube.4500rpm is centrifuged, and solid product with methanol is washed for several times, product is put into 80 DEG C of oven drying 12h, Collection product is ZIFs nucleocapsids.By tem observation product morphology (TEM, Figure 10) and it is infrared to product analysis (FT-IR, figure 11).The result shows that product be Cu2O (solid)@ZIFs nucleocapsids.
Embodiment 8：By the cuprous oxide of 0.065 gram of hollow stratiform spherical shape, 30 milliliters of methanol is added to 100 milliliters In three-necked flask, by methylimidazole (0.17~0.21 gram) methanol solution and the methanol solution of zinc nitrate (0.08~0.11 gram) Flask is slowly added to, is stirred simultaneously, is stirred under room temperature normal pressure, and keeps 1-2h.Then stirring is stopped, by total overall reaction mixed liquor It is transferred to centrifuge tube.4500rpm is centrifuged, and solid product with methanol is washed for several times, product is put into 80 DEG C of oven dryings 12h collects solid product.Then infrared analysis (FT-IR, Figure 12) is sampled, observation absorbs peak position.By TEM Figure 13 to sample Product pattern and size are confirmed.The result shows that product be Cu2O (hollow)@ZIFs nucleocapsids.
Embodiment 9：By the silica of 0.044 gram of solid spherical shape, 30 milliliters of methanol is added to three mouthfuls of 100 milliliters It is in flask, the methanol solution of methylimidazole (0.17~0.21 gram) methanol solution and zinc nitrate (0.08~0.10 gram) is slow Flask is added in, is stirred simultaneously, is stirred under room temperature normal pressure, and keep 1-8h.Then stop stirring, total overall reaction mixed liquor is shifted To centrifuge tube.4500rpm is centrifuged, and solid product with methanol is washed for several times, product is put into 80 DEG C of oven drying 12h, Collect solid product.Sample topography and size are observed by TEM Figure 14.Then sample infrared analysis (FT-IR, Figure 15), observation absorbs peak position.The result shows that product be SiO2@ZIFs nucleocapsids.
Embodiment 10：By the silica of 0.044 gram of solid spherical shape, 30 milliliters of methanol is added to three mouthfuls of 100 milliliters It is in flask, the methanol solution of methylimidazole (0.17~0.21 gram) methanol solution and cobalt nitrate (0.08~0.10 gram) is slow Flask is added in, is stirred simultaneously, is stirred under room temperature normal pressure, and keep 1-8h.Then stop stirring, total overall reaction mixed liquor is shifted To centrifuge tube.
4500rpm is centrifuged, and solid product with methanol is washed for several times, product is put into 80 DEG C of oven drying 12h, is collected solid Body product.Then infrared analysis (FT-IR, Figure 16) is sampled, observation absorbs peak position.Fail to obtain Core-shell structure material.

Claims (7)

  1. A kind of 1. method for preparing ZIFs package inorganic oxide core-shell materials, it is characterised in that：It controls metal salt solution and matches somebody with somebody The feed way of liquid solution so that metal ion and ligand are formed continuous in inorganic oxide mould material surface coordination ZIFs shells obtain ZIFs package inorganic oxide Core-shell structure materials.
  2. 2. according to the method for claim 1, it is characterised in that：By metal salt and ligand be dissolved in respectively 10~30 milliliters it is specific Solvent is added in the dispersion liquid of 30~40 milliliters of mould materials, by the processing such as centrifuging, being dried in vacuo, obtains ZIFs package nothings Machine oxide core shell structural material.
  3. 3. according to the method for claim 1, it is characterised in that：Mould material is cuprous oxide and silica.Oxidation is sub- Copper product can be solid spherical structure, hollow single-layer or multi-layer spherical structure, and earth silicon material is solid spherical structure.
  4. 4. according to the method for claim 1, it is characterised in that：Used to prepare in raw material, metal salt is cobalt nitrate, chlorine Change cobalt, cobalt acetate, acetylacetonate cobalt, zinc nitrate, zinc chloride, zinc acetate, one kind of zinc acetylacetonate or mixture, ligand For 2-methylimidazole, metal salt and ligand molar ratio are 1:4~1:8.
  5. 5. according to the method for claim 2, it is characterised in that：ZIFs Core-shell structure materials synthesis solvent for use for methanol, Ethyl alcohol, methanol are optimum solvents；The methanol solution molar concentration of original metal salt for 14.6~49.8 mmoles/liter；The first of ligand Alcoholic solution molar concentration for 110~414.1 mmoles/liter；0.03~0.08 gram of mould material is dispersed in 30~40 ml methanols Form uniform dispersion.
  6. 6. according to the method for claim 2, it is characterised in that：Reaction temperature is 20-40 DEG C, mixing time 1-4h.
  7. 7. according to the method for claim 2, it is characterised in that：The charging rate of metal salt solution and ligand solution is 0.32 ~1.5 milliliters/min；Feed time is 25~45min；Optimal charging sequence is to add in simultaneously.
CN201611056748.9A 2016-11-26 2016-11-26 A kind of preparation method of ZIFs packages inorganic oxide core-shell material Pending CN108114752A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN110105583A (en) * 2019-05-08 2019-08-09 中国科学技术大学 A kind of metal oxide/ZIF composite material, preparation method and application
CN112397690A (en) * 2019-08-12 2021-02-23 中国科学院化学研究所 Method for in-situ construction of surface coating layer based on metal-organic framework material
CN112826832A (en) * 2019-11-25 2021-05-25 中国科学院大连化学物理研究所 Nano reactor, preparation method and application thereof
CN114260027A (en) * 2020-09-16 2022-04-01 四川大学 Method for preparing metal oxide @ metal organic framework core-shell material

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110105583A (en) * 2019-05-08 2019-08-09 中国科学技术大学 A kind of metal oxide/ZIF composite material, preparation method and application
CN112397690A (en) * 2019-08-12 2021-02-23 中国科学院化学研究所 Method for in-situ construction of surface coating layer based on metal-organic framework material
CN112826832A (en) * 2019-11-25 2021-05-25 中国科学院大连化学物理研究所 Nano reactor, preparation method and application thereof
CN112826832B (en) * 2019-11-25 2022-05-17 中国科学院大连化学物理研究所 Nano reactor, preparation method and application thereof
CN114260027A (en) * 2020-09-16 2022-04-01 四川大学 Method for preparing metal oxide @ metal organic framework core-shell material
CN114260027B (en) * 2020-09-16 2023-04-25 四川大学 Method for preparing metal oxide@metal organic framework core-shell material

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Application publication date: 20180605