CN110041531A - The method of one step solvent structure Zn-MOF or Zn-Sn-MOF metal organic framework - Google Patents
The method of one step solvent structure Zn-MOF or Zn-Sn-MOF metal organic framework Download PDFInfo
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- CN110041531A CN110041531A CN201910416703.5A CN201910416703A CN110041531A CN 110041531 A CN110041531 A CN 110041531A CN 201910416703 A CN201910416703 A CN 201910416703A CN 110041531 A CN110041531 A CN 110041531A
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Abstract
The invention discloses the methods of step solvent structure Zn-MOF or Zn-Sn-MOF a metal organic framework, belong to the preparation technical field of metal organic framework.Organic molecules-ligands 2-methylimidazole and inorganic salts zinc nitrate are dissolved in methanol solvate respectively, the Tin tetrachloride pentahydrate solution of various concentration is added after two kinds of solution are mixed again, zinc ion and 2-methylimidazole are combined into the Zn-Sn-MOF metal organic frame with different-shape.The present invention has at low cost, and device is simple, and operation is simple, highly controllable, in preparation process without using toxic reagent and it is environmentally friendly the advantages that.
Description
Technical field
The invention belongs to the preparation technical fields of metal organic framework, and in particular to one step solvent structure Zn- of one kind
The method of MOF or Zn-Sn-MOF metal organic framework.
Background technique
Metal organic framework is that one kind by metal center or metal cluster and organic ligand connects shape in the form of coordinate bond
At the porous material with special topological structure and regular aperture.Compared to other porous materials, there is bigger specific surface
Product, structure, porosity and pore structure can also be regulated and controled with the difference of metal or ligand, while can also carry out function
Change modification, these excellent characteristics make material absorption with separate, be catalyzed and the fields such as sensor have it is good dive
In application value.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of simple processes, a step solvent low in cost and highly controllable
The method of thermal method synthesis Zn-MOF or Zn-Sn-MOF metal organic framework.
The present invention adopts the following technical scheme that a step solvent structure Zn-MOF metal has to solve above-mentioned technical problem
The method of machine skeleton, it is characterised in that specific steps are as follows: be added separately to 1.098g zinc nitrate and 3.300g 2-methylimidazole
It in 40mL methanol solution and stirs to being completely dissolved to obtain solution A and solution B, wherein the mass ratio of zinc nitrate and 2-methylimidazole
It for 1:3.3, is uniformly mixed solution A and solution B to obtain solution C, solution C is placed in 100-180 DEG C of autoclave
1-3h is reacted, after reaction, cooled to room temperature is centrifugated after taking out product, is dried to obtain the flower-shaped Zn- of silk ball
MOF metal organic framework.
The method of step solvent structure Zn-Sn-MOF metal organic framework of the present invention, it is characterised in that tool
Body step are as follows: 1.098g zinc nitrate and 3.300g 2-methylimidazole are added separately in 40mL methanol solution and stirred to complete
Fully dissolved obtains solution A and solution B, and wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, and solution A and solution B are stirred
It mixes to be uniformly mixed and obtains solution C, be placed on 100-180 DEG C of autoclave for Tin tetrachloride pentahydrate solution is added in solution C
Middle reaction 1-3h, wherein the mass ratio of Tin tetrachloride pentahydrate and zinc nitrate is 3:1, after reaction cooled to room temperature,
It is centrifugated after product is taken out, is dried to obtain spherical Zn-Sn-MOF metal organic framework.
The method of step solvent structure Zn-Sn-MOF metal organic framework of the present invention, it is characterised in that tool
Body step are as follows: 1.098g zinc nitrate and 3.300g 2-methylimidazole are added separately in 40mL methanol solution and stirred to complete
Fully dissolved obtains solution A and solution B, and wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, and solution A and solution B are stirred
It mixes to be uniformly mixed and obtains solution C, Tin tetrachloride pentahydrate solution is added in solution C and is placed on 100-180 DEG C of autoclave
Middle reaction 1-3h, wherein the mass ratio of Tin tetrachloride pentahydrate and zinc nitrate is 0.3:1, naturally cools to room after reaction
Temperature is centrifugated after taking out product, is dried to obtain spherical Zn-Sn-MOF metal organic framework.
The method of step solvent structure Zn-Sn-MOF metal organic framework of the present invention, it is characterised in that tool
Body step are as follows: 1.098g zinc nitrate and 3.300g 2-methylimidazole are added separately in 40mL methanol solution and stirred to complete
Fully dissolved obtains solution A and solution B, and wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, and solution A and solution B are stirred
It mixes to be uniformly mixed and obtains solution C, Tin tetrachloride pentahydrate solution is added in solution C and is placed on 100-180 DEG C of autoclave
Middle reaction 1-3h, wherein the mass ratio of Tin tetrachloride pentahydrate and zinc nitrate is 1:3, after reaction cooled to room temperature,
It is centrifugated after product is taken out, is dried to obtain polyhedron pattern Zn-Sn-MOF metal organic framework.
The present invention is with low in cost, device is simple, operation is simple, highly controllable, does not use toxic examination in preparation process
Different-shape can be obtained by the material proportion of control zinc nitrate and Tin tetrachloride pentahydrate in agent and advantages of environment protection
Zn-Sn-MOF metal organic framework.
Detailed description of the invention
Fig. 1 is the SEM figure that the flower-shaped Zn-MOF metal organic framework of silk ball is made in embodiment 1；
Fig. 2 is the SEM figure that spherical shape Zn-Sn-MOF metal organic framework is made in embodiment 2；
Fig. 3 is the SEM figure that spherical shape Zn-Sn-MOF metal organic framework is made in embodiment 3；
Fig. 4 is the SEM figure that polyhedron shape Zn-Sn-MOF metal organic framework is made in embodiment 4.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
1.098g zinc nitrate and 3.300g 2-methylimidazole are added separately in 40mL methanol solution and stirred to being completely dissolved
Solution A and solution B are obtained, wherein the mass ratio of zinc nitrate and 2-methylimidazole is 1:3.3, and solution A and solution B are stirred
Solution C uniformly is obtained, solution C is placed in 160 DEG C of autoclaves and reacts 2h, after reaction, cooled to room temperature will
Product is centrifugated after taking out, is dried to obtain the flower-shaped Zn-MOF metal organic framework of silk ball, and SEM figure is as shown in Figure 1.
Embodiment 2
1.098g zinc nitrate and 3.300g 2-methylimidazole are added separately in 40mL methanol solution and stirred to being completely dissolved
Solution A and solution B are obtained, wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, and solution A and solution B are stirred
Solution C uniformly is obtained, Tin tetrachloride pentahydrate solution is added in solution C and is placed in 160 DEG C of autoclaves and reacts 2h,
The mass ratio of middle Tin tetrachloride pentahydrate and zinc nitrate is 3:1, cooled to room temperature after reaction, after product is taken out from
Heart separation is dried to obtain spherical Zn-Sn-MOF metal organic framework, and SEM figure is as shown in Figure 2.
Embodiment 3
1.098g zinc nitrate and 3.300g 2-methylimidazole are added separately in 40mL methanol solution and stirred to being completely dissolved
Solution A and solution B are obtained, wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, and solution A and solution B are stirred
Solution C uniformly is obtained, Tin tetrachloride pentahydrate solution is added in solution C and is placed in 160 DEG C of autoclaves and reacts 2h,
The mass ratio of middle Tin tetrachloride pentahydrate and zinc nitrate is 0.3:1, after reaction cooled to room temperature, after product is taken out
It is centrifugated, is dried to obtain spherical Zn-Sn-MOF metal organic framework, SEM figure is as shown in Figure 3.
Embodiment 4
1.098g zinc nitrate and 3.300g 2-methylimidazole are added separately in 40mL methanol solution and stirred to being completely dissolved
Solution A and solution B are obtained, wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, and solution A and solution B are stirred
Solution C uniformly is obtained, Tin tetrachloride pentahydrate solution is added in solution C and is placed in 160 DEG C of autoclaves and reacts 2h,
The mass ratio of middle Tin tetrachloride pentahydrate and zinc nitrate is 1:3, cooled to room temperature after reaction, after product is taken out from
Heart separation is dried to obtain polyhedron shape Zn-Sn-MOF metal organic framework, and SEM figure is as shown in Figure 4.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (4)
1. the method for a step solvent structure Zn-MOF metal organic framework, it is characterised in that specific steps are as follows: by 1.098g
Zinc nitrate and 3.300g 2-methylimidazole be added separately in 40mL methanol solution and stir to be completely dissolved to obtain solution A and
Solution B, wherein the mass ratio of zinc nitrate and 2-methylimidazole is 1:3.3, solution A and solution B is uniformly mixed to obtain molten
Solution C is placed in 100-180 DEG C of autoclave and reacts 1-3h by liquid C, after reaction, cooled to room temperature, by product
It is centrifugated after taking-up, is dried to obtain the flower-shaped Zn-MOF metal organic framework of silk ball.
2. the method for a step solvent structure Zn-Sn-MOF metal organic framework, it is characterised in that specific steps are as follows: will
1.098g zinc nitrate and 3.300g 2-methylimidazole are added separately in 40mL methanol solution and stir molten to being completely dissolved to obtain
Liquid A and solution B, wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, and solution A and solution B are uniformly mixed
To solution C, 1-3h is reacted by Tin tetrachloride pentahydrate solution is added in solution C and is placed in 100-180 DEG C of autoclave,
The mass ratio of middle Tin tetrachloride pentahydrate and zinc nitrate is 3:1, cooled to room temperature after reaction, after product is taken out from
Heart separation is dried to obtain spherical Zn-Sn-MOF metal organic framework.
3. the method for a step solvent structure Zn-Sn-MOF metal organic framework, it is characterised in that specific steps are as follows: will
1.098g zinc nitrate and 3.300g 2-methylimidazole are added separately in 40mL methanol solution and stir molten to being completely dissolved to obtain
Liquid A and solution B, wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, and solution A and solution B are uniformly mixed
To solution C, Tin tetrachloride pentahydrate solution is added and is placed in 100-180 DEG C of autoclave in solution C and reacts 1-3h,
The mass ratio of middle Tin tetrachloride pentahydrate and zinc nitrate is 0.3:1, after reaction cooled to room temperature, after product is taken out
It is centrifugated, is dried to obtain spherical Zn-Sn-MOF metal organic framework.
4. the method for a step solvent structure Zn-Sn-MOF metal organic framework, it is characterised in that specific steps are as follows: will
1.098g zinc nitrate and 3.300g 2-methylimidazole are added separately in 40mL methanol solution and stir molten to being completely dissolved to obtain
Liquid A and solution B, wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, and solution A and solution B are uniformly mixed
To solution C, Tin tetrachloride pentahydrate solution is added and is placed in 100-180 DEG C of autoclave in solution C and reacts 1-3h,
The mass ratio of middle Tin tetrachloride pentahydrate and zinc nitrate is 1:3, cooled to room temperature after reaction, after product is taken out from
Heart separation is dried to obtain polyhedron pattern Zn-Sn-MOF metal organic framework.
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Cited By (3)
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| CN110492069A (en) * | 2019-08-11 | 2019-11-22 | 中山市华舜科技有限责任公司 | Synthetic method of Zn@ metal organic framework composite electrode material |
| CN111072690A (en) * | 2019-12-25 | 2020-04-28 | 中国科学院宁波材料技术与工程研究所 | Flower-shaped metal organic framework composite material, and preparation method and application thereof |
| CN112479246A (en) * | 2020-12-03 | 2021-03-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of Ni-doped stannic oxide formaldehyde sensitive composite material based on ZIF-8 metal organic framework template, product and application |
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| CN111072690A (en) * | 2019-12-25 | 2020-04-28 | 中国科学院宁波材料技术与工程研究所 | Flower-shaped metal organic framework composite material, and preparation method and application thereof |
| CN112479246A (en) * | 2020-12-03 | 2021-03-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of Ni-doped stannic oxide formaldehyde sensitive composite material based on ZIF-8 metal organic framework template, product and application |
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