CN108584984A - A kind of metal organic framework powder and preparation method thereof with big negative expansion coefficient - Google Patents
A kind of metal organic framework powder and preparation method thereof with big negative expansion coefficient Download PDFInfo
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- CN108584984A CN108584984A CN201810342653.6A CN201810342653A CN108584984A CN 108584984 A CN108584984 A CN 108584984A CN 201810342653 A CN201810342653 A CN 201810342653A CN 108584984 A CN108584984 A CN 108584984A
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- organic framework
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- negative expansion
- expansion coefficient
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/08—Simple or complex cyanides of metals
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Abstract
The present invention relates to a kind of metal organic framework powder and preparation method thereof with big negative expansion coefficient, the mechanism of chemical reaction and physical reactions mutually occurs using the aqueous solution of two kinds of raw materials to prepare to study, the molecular formula of the metal organic framework powder is Ag3[Co(CN)6], preparation method includes：The aqueous solution of two kinds of raw materials is slowly merged at room temperature, and is stirred 1 hour at the boiling point, then is slowly cooled to room temperature filtering once, residue is washed at least three times with the cold deionized waters of 100 ml, while being filtered three times, finally 24 hours dry at 60 DEG C.Production cost of the present invention is low, and equipment is simple, and manufacturing cycle is shorter, and manufactured product purity is high, suitable for mass production.This metal organic framework powders A g with big negative expansion coefficient3[Co(CN)6], there is stable negative expansion performance within the scope of 20 ~ 500K of temperature range, and without other phase transformations, there is potential engineering application value.
Description
Technical field
The present invention relates to a kind of metal organic framework powder preparation methods with big negative expansion coefficient, pass through the party
Metal organic framework powder made by method has big negative expansion performance.
Background technology
Almost all of material all has the performance expanded with heat and contract with cold in the Nature.Phenomenon is thermally expanded in metal, ceramics, height
All generally existing, the influence of coefficient of thermal expansion can directly result in generation of expanding with heat and contract with cold in the engineering material such as molecule, composite material
Thermal stress or thermal shock make fatigue of materials performance decline, or even fracture.In view of the importance of coefficient of thermal expansion, heat is solved
Expansion issues, researchers, which explore the metal-organic framework materials with negative expansion performance, can preferably solve modern section
Learn these problems in investigative technique.Numerous studies show that the material with negative thermal expansion is rarely found in the world, and negative heat is swollen
The material that swollen temperature range is wider, negative expansion performance is stablized is even more fewer and fewer.
So far, the material with good negative expansion performance academicly reported is that Sleight research groups exist
《Science》The ZrW of upper report2O8Negative expansion is all shown in the entire temperature range of 0.3K to decomposition temperature 1050K
Can, ZrW2O8Linear expansion coefficient be -9.8x10-6K-1, performance is unstable and negative expansion coefficient is smaller.These performances limit
Its performance and application.Find so far and the material category with huge negative expansion performance that can find out very
Few, the document report about the metal-organic framework materials with huge negative expansion performance is less.
It can be seen that exploitation has, negative expansion section is wider, negative expansion performance is stable, negative expansion coefficient is larger,
Widely used metal-organic framework materials are the common urgent problems to be solved of numerous researchers, and require preparation process simple
It is single, it is suitble to large-scale production, cost more low.
Invention content
In order to efficiently, accurately and fast prepare the metal organic framework powder with big negative expansion performance, this hair
It is bright to have selected a kind of reaction process simple, and the preparation method of the high product of purity stable and reliable for performance is produced, while
Good guarantee is provided for later stage performance characterization and application study.
The molecular formula of the negative expansion powder of the present invention is Ag3[Co(CN)6], the linear expansion system measured with thermal dilatometer
Number is -120x10-6K-1, technical solution is used by solving its technical problem：A kind of gold with big negative expansion coefficient
Belong to the preparation method of organic backbone powder, it is characterised in that carry out according to the following steps：
One, heat collecting type constant-temperature heating magnetic stirring apparatus temperature setting is 100 DEG C, and ultrasonic oscillator temperature setting is 25
DEG C, drying box temperature setting is 60 DEG C；
Two, the beaker for preparing two 100ml, pours into the pure water of 30ml respectively；
Three, the K for being 332 with electronic balance weighing 3.8154g molecular weight3[Co(CN)6] raw material and 5.0889g AgNO3It is former
Material；
Four, by load weighted K3[Co(CN)6] raw material and AgNO3Raw material is poured into respectively in two beakers described in step 2,
Be put into the ultrasonic oscillator set, at the same with glass stirring rod stir 10min, until raw material be all uniformly dissolved for
Only；
Five, the solution of two beakers is slowly all blended in a beaker with 5ml rubber heads dropper at room temperature；
Six, magnetic stirring apparatus is opened, stirrer is added in the beaker equipped with mixed solution, and be put into the magnetic force set and stir
It mixes and stirs 1h in device；
Seven, beaker is taken out from magnetic stirring apparatus, closes beaker mouth with preservative film, is placed in air and is slowly cooled to room temperature；
Eight, it is filtered with 1000ml glass sand core filter devices primary；
Nine, the cold 100ml pure waters of residue are filtered, and in triplicate；
Ten, gained powder is put into and is set as in 60 DEG C of drying box dry left and right for 24 hours.
Further, the power that the step 4 adjusts ultrasonic oscillator is 90W.
Further, take when solution should slowly and average rate is to ensure that two kinds of solution are slow for step 5 rubber head dropper drop
Uniformly mixing.
Further, beaker is placed in heat collecting type constant temperature magnetic force heating stirrer, the stirring of this blender by the step 6
It is 0~2600r/min that range, which can be arranged, in speed, and the speed of blender is set as 1500~2000r/min.
Further, when the step 8 filter device is connect with vacuum pump, one layer of Φ 7cm filter should be put into filter device
Paper so that product stays in just subsequent step progress above filter paper.
Further, it is stirred using glassed agitator average rate so that solution is uniform when the step 9 pure water.
Further, powder obtained by the step 10 is put into beaker, it should be closed rim of a cup with preservative film, be placed into drying
In case, prevent other samples or reagent from influencing.
The present invention operation principle be：During preparing this metal organic framework powder, according to the change of two kinds of solution
It learns the next entire reaction condition of modification and the preparation process of constantly progressing greatly of reaction mechanism and designs one kind in the case where a large amount of experiment is accumulated
Simpler and suitable preparation method.It is mutual to control two kinds of material solutions by controlling whipping temp and mixing time
Reaction speed and yield efficiency, and regulation and control cooling velocity and cooling condition product purity is improved, pass through washing and mistake
It filters to exclude other impurity, last control drying condition makes sample be able to convenient function research and application verification at dry state.
Advantages of the present invention：(1) the glass sand core Suction filtration device that uses of the present invention is more than simple filter paper filter type
It is quick and easy, efficient.(2) it entirely tests required temperature condition and appointed condition requirement is relatively low, cost is small, manufacturing cycle
Short, preparation method is simple, nonpollution environment.(3) preparation flow of this metal organic framework powder has been advanced optimized.
Description of the drawings
Fig. 1 is the flow sheet of the present invention.
Fig. 2 is the field emission scanning electron microscope figure of present invention gained metal organic framework powder.
Specific implementation mode
It provides the embodiment of the present invention and the embodiment provided is combined to be illustrated the present invention, but given embodiment
The present invention is not limited in any way：
Specific implementation mode one：It is 100 DEG C by heat collecting type constant-temperature heating magnetic stirring apparatus temperature setting, ultrasonic oscillator
Temperature setting is 25 DEG C, and drying box temperature setting is 60 DEG C, then measures 30ml pure water twice with 50ml graduated cylinders and pour into 100ml respectively
In beaker, the K that the molecular weight of 3.8154g is 332 is weighed3[Co(CN)6] raw material and 5.0889g AgNO3Raw material will weigh
K3[Co(CN)6] raw material and AgNO3Raw material is poured into respectively in the beaker described in step 2, is put into the supersonic oscillations set
In device, while using 5ml rubber heads dropper by two at room temperature until raw material all dissolving with glass stirring rod stirring 10min
The solution of a beaker is slowly all blended in a beaker, opens magnetic stirring apparatus, and the beaker equipped with mixed solution is added
Stirrer, and be put into the magnetic stirring apparatus set and stir 1h, beaker is taken out from magnetic stirring apparatus, beaker is closed with preservative film
Mouthful, be put in outside and be slowly cooled to room temperature, filtered with 1000ml glass sand core filter devices it is primary, by residue with cold
100ml pure waters are primary, and filtering is primary, in triplicate, gained powder are put into and is set as drying for 24 hours in 60 DEG C of drying box
Left and right.
Specific implementation mode two：It is 120 DEG C by heat collecting type constant-temperature heating magnetic stirring apparatus temperature setting, ultrasonic oscillator
Temperature setting is 25 DEG C, and drying box temperature setting is 80 DEG C, then measures 30ml pure water twice with 50ml graduated cylinders and pour into 100ml respectively
In beaker, the K that the molecular weight of 3.8154g is 332 is weighed3[Co(CN)6] raw material and 5.0889g AgNO3Raw material will weigh
K3[Co(CN)6] raw material and AgNO3Raw material is poured into respectively in the beaker described in step 2, is put into the supersonic oscillations set
In device, while 5ml graduated cylinders are used to burn two at room temperature until raw material all dissolving with glass stirring rod stirring 10min
The solution of cup is slowly all blended in a beaker, opens magnetic stirring apparatus, and stirring is added in the beaker equipped with mixed solution
Son, and be put into the magnetic stirring apparatus set and stir 1h, beaker is taken out from magnetic stirring apparatus, beaker mouth is closed with preservative film,
It is put in outside to be slowly cooled to room temperature, be filtered once with 1000ml glass sand core filter devices, residue is pure with cold 100ml
Water washing is primary, and filtering is primary, in triplicate, gained powder is put into and is set as in 80 DEG C of drying box dry left and right for 24 hours, institute
It is white powder Ag to obtain product3[Co(CN)6]。
Claims (7)
1. a kind of preparation method of the metal organic framework powder with big negative expansion coefficient, it is characterised in that press following step
It is rapid to carry out：
One, heat collecting type constant-temperature heating magnetic stirring apparatus temperature setting is 100 DEG C, and ultrasonic oscillator temperature setting is 25 DEG C, is done
Dry box temperature degree is set as 60 DEG C；
Two, the beaker for preparing two 100 ml, pours into the pure water of 30 ml respectively；
Three, the K for being 332 with 3.8154 g molecular weight of electronic balance weighing3[Co(CN)6] raw material and 5.0889 g AgNO3It is former
Material;
Four, by load weighted K3[Co(CN)6] raw material and AgNO3Raw material is poured into respectively in two beakers described in step 2, is put into
In the ultrasonic oscillator set, while 10 min are stirred with glass stirring rod, until raw material is all uniformly dissolved；
Five, the solution of two beakers is slowly all blended in a beaker with 5 ml rubber heads droppers at room temperature；
Six, magnetic stirring apparatus is opened, stirrer is added in the beaker equipped with mixed solution, and be put into the magnetic stirring apparatus set
Middle stirring 1h;
Seven, beaker is taken out from magnetic stirring apparatus, closes beaker mouth with preservative film, is placed in air and is slowly cooled to room temperature；
Eight, it is filtered with 1000 ml glass sand core filter devices primary；
Nine, 100 cold ml pure waters of residue are filtered, and in triplicate；
Ten, gained powder is put into and is set as in 60 DEG C of drying box dry 24 h or so.
2. a kind of preparation side of metal organic framework powder with big negative expansion coefficient according to claim 1
Method, it is characterised in that：The power that the step 4 adjusts ultrasonic oscillator is 90 W.
3. a kind of preparation side of metal organic framework powder with big negative expansion coefficient according to claim 1
Method, it is characterised in that：Step 5 rubber head dropper drop should slowly and at the uniform velocity, to ensure that two kinds of solution slowly mix when taking solution
It closes uniform.
4. a kind of preparation side of metal organic framework powder with big negative expansion coefficient according to claim 1
Method, it is characterised in that：Beaker is placed in heat collecting type constant temperature magnetic force heating stirrer by the step 6, and the speed of blender is set as
1500~2000 r/min。
5. a kind of preparation side of metal organic framework powder with big negative expansion coefficient according to claim 1
Method, it is characterised in that：When the step 8 filter device is connect with vacuum pump, the filter of one layer of 7 cm of Φ should be put into filter device
Paper so that product stays in just subsequent step progress above filter paper.
6. a kind of preparation side of metal organic framework powder with big negative expansion coefficient according to claim 1
Method, it is characterised in that：It is at the uniform velocity stirred using glassed agitator when step 9 pure water, so that solution is uniformly mixed.
7. a kind of preparation side of metal organic framework powder with big negative expansion coefficient according to claim 1
Method, it is characterised in that：Powder is put into beaker obtained by the step 10, it should be closed rim of a cup with preservative film, be placed into drying box
In, prevent other samples or reagent from influencing.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624409A (en) * | 2009-07-31 | 2010-01-13 | 江苏科技大学 | PtS cyano-bridged coordination polymer and preparation method thereof |
| CN103578991A (en) * | 2012-07-24 | 2014-02-12 | 中国科学院微电子研究所 | Semiconductor device manufacturing method |
| CN106549016A (en) * | 2015-09-21 | 2017-03-29 | 中国科学院微电子研究所 | Semiconductor device and preparation method thereof |
-
2018
- 2018-04-17 CN CN201810342653.6A patent/CN108584984A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624409A (en) * | 2009-07-31 | 2010-01-13 | 江苏科技大学 | PtS cyano-bridged coordination polymer and preparation method thereof |
| CN103578991A (en) * | 2012-07-24 | 2014-02-12 | 中国科学院微电子研究所 | Semiconductor device manufacturing method |
| CN106549016A (en) * | 2015-09-21 | 2017-03-29 | 中国科学院微电子研究所 | Semiconductor device and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| ANDREW L. GOODWIN等: "Colossal Positive and Negative Thermal Expansion in the Framework Material Ag3[Co(CN)6]", 《SCIENCE》 * |
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Application publication date: 20180928 |