CN104261448A - Nano calcium oxide and preparation method thereof - Google Patents
Nano calcium oxide and preparation method thereof Download PDFInfo
- Publication number
- CN104261448A CN104261448A CN201410547580.6A CN201410547580A CN104261448A CN 104261448 A CN104261448 A CN 104261448A CN 201410547580 A CN201410547580 A CN 201410547580A CN 104261448 A CN104261448 A CN 104261448A
- Authority
- CN
- China
- Prior art keywords
- calcium oxide
- nano
- preparation
- nano calcium
- steel vessel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 239000000292 calcium oxide Substances 0.000 title claims abstract description 43
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 title claims abstract description 43
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 36
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000010791 quenching Methods 0.000 claims abstract description 13
- 230000000171 quenching effect Effects 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000012467 final product Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract 3
- 229910000831 Steel Inorganic materials 0.000 abstract 2
- 239000010959 steel Substances 0.000 abstract 2
- 238000004321 preservation Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 9
- 238000000354 decomposition reaction Methods 0.000 description 8
- 235000010216 calcium carbonate Nutrition 0.000 description 7
- 239000002994 raw material Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000005036 potential barrier Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 239000002772 conduction electron Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/02—Oxides or hydroxides
- C01F11/04—Oxides or hydroxides by thermal decomposition
- C01F11/06—Oxides or hydroxides by thermal decomposition of carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to nano calcium oxide and a preparation method thereof. According to the technical scheme, a steel vessel filled with nano calcium carbonate is placed into a vacuum heating furnace; the vacuum heating furnace is vacuumized to 10 Pa or lower than 10 Pa; the vacuumized vacuum heating furnace is heated to the temperature of 300 DEG C-500 DEG C and subjected to heat preservation for 1-1,800 seconds; and finally, the steel vessel is cooled with a quenching method or a rapid cooling method, and nano calcium oxide is taken out. The nano calcium oxide and the preparation method have the characteristics of simple process, low preparation cost and high production efficiency, and the prepared nano calcium oxide is uniform in microstructure, small in granularity and wide in use range.
Description
Technical field
The invention belongs to materialogy technical field.Particularly relate to a kind of nano calcium oxide and preparation method thereof.
Background technology
In a broad sense, nano material refers to the material having at least one dimension to be in nanoscale scope (0.1nm ~ 100nm) or to be made up of as elementary cell them in three dimensions.The characteristic that nano material has comprises:
(1) surface and interface effect, this refers to that the ratio of nanocrystal grain surface atom number and total atom number diminishes with particle diameter and sharply increases rear caused qualitative change; (2) small-size effect, when nanoparticle size and optical wavelength, the physical features sizes such as the de broglie wavelength of conduction electron and the coherence length of superconducting state, transmission depth quite or less time, its periodic boundary is destroyed, thus makes the performances such as its sound, optical, electrical, magnetic and thermodynamics present the phenomenon of " novelty "; (3) quantum size effect, when the size of particle reaches nanometer scale, there will be the quantum effect of nano material, thus makes its magnetic, light, sound, heat, electricity, superconduction performance variation.Such as, have kind of metal nanoparticle to absorb light ability very strong, as long as put into this particle of thousandth in 1.1365 kg water, water will become completely opaque; (4) macro quanta tunnel effect, microcosmic particle has the ability running through potential barrier and is called tunnel effect.The specific magnetising moment of nanoparticle etc. also have tunnel effect, and they can change through the potential barrier of macrosystem, this macro quanta tunnel effect being called as nanoparticle.By means of the various special propertys of nano material, scientific workers achieve breakthrough progress in each research field, also promote more and more extensively changing of Application of micron, as having a wide range of applications in the multiple field of catalysis, biomedicine, fine chemistry industry, science and techniques of defence, seawater cleaning, aerospace, environmental energy and microtronics simultaneously.
Though nano calcium oxide can be widely used in above-mentioned field, preparation technology's more complicated.If any people at preparation CaO base CO
2during reactive adsorption agent, with Nano-meter CaCO3
3, Alumina gel, nickel salt (Nickelous nitrate hexahydrate) be raw material, prepared composite catalyst Cata, composite catalyst is with Al
2o
3for carrier, to Nano-meter CaCO3
3dispersion play a good role, and Nano-meter CaCO3
3surface is by Al
2o
3after coated, its apparent activation energy reduces, and makes CaCO
3more easily decompose, it decomposes minimum temperature is 550 DEG C.There is report by Nano-meter CaCO3
3add NaSiO
3be made into suspension in solution, then pass into CO
2, finally obtain Nano-meter SiO_2
2/ CaCO
3particle (is equivalent at CaCO
3the coated one deck SiO of particle surface
2).Contrast by experiment, obtain the decomposition temperature of composite particles than non-coated Si O
2nano-meter CaCO3
3decomposition temperature low 9 ~ 42 DEG C, but temperature is also more than 600 DEG C.Similar method adds Al in addition
2o
3, MgO, ZrO
2, B
2o
3deng.
Summary of the invention
The present invention is intended to overcome prior art defect, and object is to provide the preparation method of the nano calcium oxide that a kind of technique is simple, cost is low and production efficiency is high; The nano calcium oxide uniform microstructure prepared by the method, granularity is little and use range is wide.
For achieving the above object, the technical solution used in the present invention is: the concrete steps of described preparation method are:
Step one, nano-calcium carbonate is loaded Steel Vessel, more described Steel Vessel is put into vacuum furnace;
Step 2, described vacuum furnace is evacuated to 10pa or below 10Pa;
Step 3, the vacuum furnace after described vacuumizing is heated to 300 DEG C ~ 500 DEG C, is incubated 1 ~ 1800 second;
Step 4, employing quenching method or quick cooling method cool described Steel Vessel, are taken out by nano calcium oxide and get final product.
CaCO in described nano-calcium carbonate
3content>=97wt%; The particle diameter of nano-calcium carbonate is 0.1 ~ 100nm.
Described quenching method refers to the method adopting quenching in liquid nitrogen quenching or water.
Described quick cooling method refers to the method adopting high pressure air-cooled.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect:
Preparation process temperature of the present invention is low, at 300 ~ 500 DEG C; Soaking time is within 30 minutes, and preparation time is short, therefore can enhance productivity and reduce preparation cost.
First the present invention is reduction of the decomposition temperature of calcium carbonate, next be that of avoiding nano-calcium carbonate decompose after the problem of nano calcium oxide of obtaining at high temperature grain growth.Under vacuum condition, the decomposition temperature of nano-calcium carbonate reduces greatly, and the nano calcium oxide obtained after low-temperature decomposition just can avoid the abnormal growth of its crystal grain by the method for cooling fast, thus keeps nanometer uniform microstructure.The average grain size of obtained nano calcium oxide be 34nm(wherein, the grain-size of the nano-calcium carbonate raw material used is 57nm).
Nano calcium oxide prepared by the present invention can be used as the uses such as carbon dioxide absorber, Metal Melting calcium oxide raw material and agglutinant, and use range is wide.
Therefore, the present invention has the advantages that technique is simple, preparation cost is low and production efficiency is high, and prepared nano calcium oxide uniform microstructure, granularity is little and use range is wide.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, the restriction not to its protection domain.
Nano-calcium carbonate Unify legislation in this embodiment is as follows, repeats no more in embodiment:
CaCO in described nano-calcium carbonate
3content>=97wt%; The particle diameter of nano-calcium carbonate is 0.1 ~ 100nm.
embodiment 1
A kind of nano calcium oxide and preparation method thereof.Described in the present embodiment, the concrete steps of preparation method are:
Step one, nano-calcium carbonate is loaded Steel Vessel, more described Steel Vessel is put into vacuum furnace;
Step 2, described vacuum furnace is evacuated to 5 ~ 10pa;
Step 3, the vacuum furnace after described vacuumizing is heated to 480 ~ 500 DEG C, is incubated 1 ~ 60 second;
The method of step 4, employing liquid nitrogen quenching cools described Steel Vessel, is taken out by nano calcium oxide and get final product.
embodiment 2
A kind of nano calcium oxide and preparation method thereof.Described in the present embodiment, the concrete steps of preparation method are:
Step one, nano-calcium carbonate is loaded Steel Vessel, more described Steel Vessel is put into vacuum furnace;
Step 2, described vacuum furnace is evacuated to 1 ~ 5Pa;
Step 3, the vacuum furnace after described vacuumizing is heated to 450 DEG C ~ 480 DEG C, is incubated 60 ~ 600 seconds;
In step 4, employing water, the method for quenching cools described Steel Vessel, is taken out by nano calcium oxide and get final product.
embodiment 3
A kind of nano calcium oxide and preparation method thereof.Described in the present embodiment, the concrete steps of preparation method are:
Step one, nano-calcium carbonate is loaded Steel Vessel, more described Steel Vessel is put into vacuum furnace;
Step 2, described vacuum furnace is evacuated to 0.1 ~ 1pa;
Step 3, the vacuum furnace after described vacuumizing is heated to 400 ~ 450 DEG C, is incubated 600 ~ 900 seconds;
Step 4, adopt the air-cooled method of high pressure to cool described Steel Vessel, nano calcium oxide is taken out and get final product.
embodiment 4
A kind of nano calcium oxide and preparation method thereof.Described in the present embodiment, the concrete steps of preparation method are:
Step one, nano-calcium carbonate is loaded Steel Vessel, more described Steel Vessel is put into vacuum furnace;
Step 2, described vacuum furnace is evacuated to 0.01 ~ 0.1pa;
Step 3, the vacuum furnace after described vacuumizing is heated to 350 ~ 400 DEG C, is incubated 900 ~ 1200 seconds;
In step 4, employing water, the method for quenching cools described Steel Vessel, is taken out by nano calcium oxide and get final product.
embodiment 5
A kind of nano calcium oxide and preparation method thereof.Described in the present embodiment, the concrete steps of preparation method are:
Step one, nano-calcium carbonate is loaded Steel Vessel, more described Steel Vessel is put into vacuum furnace;
Step 2, described vacuum furnace is evacuated to 0.001 ~ 0.01pa;
Step 3, the vacuum furnace after described vacuumizing is heated to 300 DEG C ~ 350 DEG C, is incubated 1200 ~ 1800 seconds;
Described in the method for step 4, employing liquid nitrogen quenching, Steel Vessel cools, and is taken out by nano calcium oxide and get final product.
This embodiment compared with prior art has following positively effect.
This embodiment preparation process temperature is low, at 300 ~ 500 DEG C; Soaking time is within 30 minutes, and preparation time is short, therefore can enhance productivity and reduce preparation cost.
First this embodiment is reduction of the decomposition temperature of calcium carbonate, next be that of avoiding nano-calcium carbonate decompose after the problem of nano calcium oxide of obtaining at high temperature grain growth.Under vacuum condition, the decomposition temperature of nano-calcium carbonate reduces greatly, and the nano calcium oxide obtained after low-temperature decomposition just can avoid the abnormal growth of its crystal grain by the method for cooling fast, thus keeps nanometer uniform microstructure.The average grain size of obtained nano calcium oxide be 34nm(wherein, the grain-size of nano-calcium carbonate raw material is 57nm).
Nano calcium oxide prepared by this embodiment can be used as the uses such as carbon dioxide absorber, Metal Melting calcium oxide raw material and agglutinant, and use range is wide.
Therefore, this embodiment has the advantages that technique is simple, preparation cost is low and production efficiency is high, and prepared nano calcium oxide uniform microstructure, granularity is little and use range is wide.
Claims (5)
1. a preparation method for nano calcium oxide, is characterized in that the concrete steps of described preparation method are:
Step one, nano-calcium carbonate is loaded Steel Vessel, more described Steel Vessel is put into vacuum furnace;
Step 2, described vacuum furnace is evacuated to 10pa or below 10Pa;
Step 3, the vacuum furnace after described vacuumizing is heated to 300 DEG C ~ 500 DEG C, is incubated 1 ~ 1800 second;
Step 4, employing quenching method or quick cooling method cool described Steel Vessel, are taken out by nano calcium oxide and get final product.
2. the preparation method of nano calcium oxide according to claim 1, is characterized in that CaCO in described nano-calcium carbonate
3content>=97wt%; The particle diameter of nano-calcium carbonate is 0.1 ~ 100nm.
3. the preparation method of nano calcium oxide according to claim 1, is characterized in that described quenching method refers to the method adopting quenching in liquid nitrogen quenching or water.
4. the preparation method of nano calcium oxide according to claim 1, is characterized in that described quick cooling method refers to the method adopting high pressure air-cooled.
5. a nano calcium oxide, is characterized in that described nano calcium oxide is the nano calcium oxide prepared by the preparation method of nano calcium oxide described in claim 1 ~ 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410547580.6A CN104261448B (en) | 2014-10-16 | 2014-10-16 | A kind of nano calcium oxide and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410547580.6A CN104261448B (en) | 2014-10-16 | 2014-10-16 | A kind of nano calcium oxide and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104261448A true CN104261448A (en) | 2015-01-07 |
| CN104261448B CN104261448B (en) | 2016-01-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410547580.6A Expired - Fee Related CN104261448B (en) | 2014-10-16 | 2014-10-16 | A kind of nano calcium oxide and preparation method thereof |
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| Country | Link |
|---|---|
| CN (1) | CN104261448B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105130403A (en) * | 2015-08-14 | 2015-12-09 | 武汉科技大学 | Self-binding calcium oxide material and preparation method thereof |
| CN108557856A (en) * | 2018-05-08 | 2018-09-21 | 武汉科技大学 | A kind of calcium oxide particle and preparation method thereof based on vacuum-sintering |
| CN108686616A (en) * | 2017-04-10 | 2018-10-23 | 北京林业大学 | A kind of carbon dioxide absorbing material and preparation method thereof |
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|---|---|---|---|---|
| CN101311369A (en) * | 2008-04-21 | 2008-11-26 | 上海大学 | Method for preparing pure phase bismuth ferric crystallite |
| CN103184400A (en) * | 2011-12-27 | 2013-07-03 | 上海宝钢设备检修有限公司 | Nano-ceramic composite spraying powder and preparation method for same |
-
2014
- 2014-10-16 CN CN201410547580.6A patent/CN104261448B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311369A (en) * | 2008-04-21 | 2008-11-26 | 上海大学 | Method for preparing pure phase bismuth ferric crystallite |
| CN103184400A (en) * | 2011-12-27 | 2013-07-03 | 上海宝钢设备检修有限公司 | Nano-ceramic composite spraying powder and preparation method for same |
Non-Patent Citations (3)
| Title |
|---|
| 侯德榜等: "《制碱工业工作者手册》", 31 December 1962, 中国工业出版社 * |
| 卢宇飞等: "《炼铁技术》", 31 January 2010, 冶金工业出版社 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105130403A (en) * | 2015-08-14 | 2015-12-09 | 武汉科技大学 | Self-binding calcium oxide material and preparation method thereof |
| CN105130403B (en) * | 2015-08-14 | 2017-04-12 | 武汉科技大学 | Self-binding calcium oxide material and preparation method thereof |
| CN108686616A (en) * | 2017-04-10 | 2018-10-23 | 北京林业大学 | A kind of carbon dioxide absorbing material and preparation method thereof |
| CN108686616B (en) * | 2017-04-10 | 2020-09-11 | 北京林业大学 | Carbon dioxide adsorbing material and preparation method thereof |
| CN108557856A (en) * | 2018-05-08 | 2018-09-21 | 武汉科技大学 | A kind of calcium oxide particle and preparation method thereof based on vacuum-sintering |
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| CN104261448B (en) | 2016-01-13 |
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