CN114890430A - Preparation method of tetragonal crystal petalite powder - Google Patents
Preparation method of tetragonal crystal petalite powder Download PDFInfo
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- CN114890430A CN114890430A CN202210521486.8A CN202210521486A CN114890430A CN 114890430 A CN114890430 A CN 114890430A CN 202210521486 A CN202210521486 A CN 202210521486A CN 114890430 A CN114890430 A CN 114890430A
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- 239000000843 powder Substances 0.000 title claims abstract description 82
- HEHRHMRHPUNLIR-UHFFFAOYSA-N aluminum;hydroxy-[hydroxy(oxo)silyl]oxy-oxosilane;lithium Chemical compound [Li].[Al].O[Si](=O)O[Si](O)=O.O[Si](=O)O[Si](O)=O HEHRHMRHPUNLIR-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052670 petalite Inorganic materials 0.000 title claims abstract description 56
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000013078 crystal Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 6
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000003832 thermite Substances 0.000 abstract description 7
- 229910018068 Li 2 O Inorganic materials 0.000 abstract description 6
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000012467 final product Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000003999 initiator Substances 0.000 abstract description 2
- 229910001947 lithium oxide Inorganic materials 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 230000002269 spontaneous effect Effects 0.000 abstract description 2
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 abstract 1
- 230000005496 eutectics Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 24
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000012876 topography Methods 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910010100 LiAlSi Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect 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
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention provides a method for preparing tetragonal petalite powder, wherein SiO is added into Al powder 2 And Li 2 CO 3 In the mixture (A) causes a thermite reaction which releases a large amount of heat to effect a decomposition reaction Li 2 CO 3 ＝Li 2 O+CO 2 Produce more Li 2 O, Simultaneous Synthesis reaction Li 2 O+8SiO 2 +Al 2 O 3 ＝2LiAlSi 4 O 10 And generating a target reactant of petalite. Since the thermite reaction is a spontaneous exothermic reaction, the lower reaction temperature can spontaneously go down to release a large amount of heat to help the formation of petalite. Meanwhile, in the invention, the content of Al powder is controlled to be 1-3 wt%, and the thermite reaction time is controlled, so that the Li2O is prevented from being excessively volatilized to reduce the purity of a final product. The invention does not need petalite as a seed crystal initiator, has less process steps and simple and convenient operation, and is convenient for large-scale industrialization. The calcining temperature is low, on one hand, the energy can be greatly reducedConsumption; on the other hand, long-time high-temperature conditions are not needed, the component loss caused by volatilization of eutectic formed by the lithium oxide and other substances is reduced, and the yield is increased.
Description
Technical Field
The invention relates to the technical field of artificially synthesized inorganic powder materials, in particular to a preparation method of tetragonal crystal petalite powder.
Background
Petalite, a special crystal structure mineral, has the material characteristics of thermal negative expansion and near-zero expansion in the range of room temperature to 600 ℃. Petalite exists in nature as monoclinic silicate ore. The mineral is unbalanced all over the world, and particularly, the mineral is scarce in China, so that the use cost is high and the supply risk exists. For this reason, many researchers have proposed artificially synthesizing petalite having a negative expansion coefficient.
In the prior art, LiO is generally adopted for artificially synthesizing petalite 2 、SiO 2 And Al 2 O 3 Calcining at 1800 deg.C to produce LiAlSi 4 O 10 Petalite material. Under the reaction conditions, materials are generated at higher reaction temperature, obviously, the energy consumption is high, and the yield is low.
The technical scheme of the tetragonal petalite is disclosed in the name of CN112358286A for artificial synthesis of the tetragonal petalite and a manufacturing method thereof. In the scheme, the tetragonal petalite is an isomer of monoclinic natural petalite and has the same thermal negative expansion performance as the natural petalite. The specific scheme is that 1-3 Wt% of natural petalite powder is introduced as a seed crystal, and the tetragonal petalite is initiated to grow and be purified by calcining (more than 1300 ℃) other components. The technical scheme is a typical scheme for artificially synthesizing petalite with thermal expansion performance. But in the scheme, the natural petalite powder is still required to be used as a seed crystal to synthesize the target material.
Accordingly, the applicant further researches and develops a technical scheme for artificially synthesizing the tetragonal petalite without using natural petalite powder as a seed crystal and at a lower calcining temperature.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of tetragonal petalite powder, and aims to artificially synthesize the tetragonal petalite without introducing natural petalite seed crystals.
A method for preparing tetragonal petalite powder,
the method comprises the following steps: preparing a mixture comprising 76 to 78 wt% of SiO 2 9 to 10 wt% of Li 2 CO 3 9 to 11 wt% of Al 2 O 3 1-3 wt% of Al powder;
step two: preparing mixture powder by ball milling, and carrying out ball milling treatment on the mixture obtained in the step two to obtain the mixture powder;
step three: and D, calcining the mixture powder obtained in the step two to obtain high-purity tetragonal crystal petalite powder.
Preferably, the rotation speed of the ball milling treatment in the second step is 350-500 rpm.
And further, heating to the calcining temperature of 600-800 ℃ at the normal temperature of 5 ℃/min in the third step, and preserving the heat for 1-2 h.
Preferably, the diameter of the Al powder in the mixture in the second step is 70-100 nm.
The preparation method of the tetragonal petalite powder has the beneficial effect that the applicant finds that SiO is added into the Al powder 2 And Li 2 CO 3 In the mixture (A) causes a thermite reaction which releases a large amount of heat to effect a decomposition reaction Li 2 CO 3 ＝Li 2 O+CO 2 More Li is produced 2 O, Simultaneous Synthesis reaction Li 2 O+8SiO 2 +Al 2 O 3 ＝2LiAlSi 4 O 10 And generating a target reactant of petalite. Since the thermite reaction is a spontaneous exothermic reaction, the lower reaction temperature can spontaneously release a large amount of heat to help produce petalite. Meanwhile, in the invention, the content of Al powder is controlled to be 1-3 wt%, and the thermite reaction time is controlled to ensure Li 2 O does not volatilize excessively to reduce the purity of the final product. The invention does not need petalite as a seed crystal initiator, has less process steps and simple and convenient operation, and is convenient for large-scale industrialization. The calcination temperature is low, so that on one hand, the energy consumption can be greatly reduced; on the other hand, the evaporation of eutectic mixture formed by lithium oxide and other substances is reduced without long-time high-temperature conditionResulting in loss of components and increased yield. According to the invention, aluminum powder is introduced, on one hand, the calcination temperature is reduced through thermite reaction, and simultaneously, the aluminum powder reacts with impurities (iron oxide) in other substances to remove the impurities, so that the synthesized tetragonal crystal petalite has high purity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is an XRD pattern of a product according to an embodiment of the present invention;
FIG. 2 is a microscopic topography of a product according to an embodiment of the present invention;
FIG. 3 is an XRD pattern of a product of example two of the present invention;
FIG. 4 is a microscopic topography of a product of a second embodiment of the present invention;
FIG. 5 is an XRD pattern of a third product of an example of the present invention;
FIG. 6 is a microscopic topography of a third resultant of an embodiment of the present invention;
FIG. 7 is an XRD pattern of the four products of example of the present invention;
FIG. 8 is a microscopic topography of a four-product of an embodiment of the present invention;
FIG. 9 is an XRD pattern of a fifth product of example five of the present invention;
FIG. 10 is a micro-topography of a five-product of an embodiment of the present invention;
FIG. 11 is an XRD pattern of a product of the first comparative example;
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
The first embodiment is as follows:
23.4g of SiO were weighed 2 Powder, 3.3g of Al 2 O 3 Powder, 0.3g of Al powder, 3g of Li 2 CO 3 The powder is mixed and then ball milled for 36h by a ball mill at the rotating speed of 350 rpm. Then ball milling and mixing uniformlyThe mixed powder is heated to 700 ℃ at the heating rate of 5 ℃/min and calcined for 1 h.
And (4) conclusion: the XRD pattern of the product (measured with X-ray diffractometer model D8) was analyzed as shown in FIG. 1. As can be seen, the product is a product with Li as the main crystal phase 0.6 Al 0.6 Si 2.4 O 6 The purity of the petalite powder is 82.2 percent (Diffrac. eva software matched with a D8X-ray diffractometer is adopted to quantitatively calculate the phase Li of the petalite in the sample powder 0.6 Al 0.6 Si 2.4 O 6 Content of (d). The microscopic morphology of the powder is shown in FIG. 2. it can be seen from FIG. 2 that the particle size of the powder is 5 to 15 μm.
The second embodiment:
23.4g of SiO were weighed 2 Powder, 3g of Al 2 O 3 Powder, 0.6g of Al powder, 3g of Li 2 CO 3 The powder is mixed and then ball milled for 36h by a ball mill at the rotating speed of 350 rpm. Then heating the mixed powder which is evenly mixed by ball milling to 600 ℃ at the heating rate of 5 ℃/min and calcining for 1 h.
And (4) conclusion: the XRD pattern of this product (measured using X-ray diffractometer model D8) was analyzed as shown in FIG. 3. As can be seen, the product has a main crystal phase of Li 0.6 Al 0.6 Si 2.4 O 6 The purity of the petalite powder is 82.5 percent (Diffrac. eva software matched with a D8X-ray diffractometer is adopted to quantitatively calculate the phase Li of the petalite in the sample powder 0.6 Al 0.6 Si 2.4 O 6 Content of (b). The microscopic morphology of the powder is shown in FIG. 4, which shows that the particle size of the powder is 5-15 μm.
Example three:
23.4g of SiO were weighed 2 Powder, 2.7g of Al 2 O 3 Powder, 0.9g of Al powder, 3g of Li 2 CO 3 The powder is mixed and then ball milled for 36h by a ball mill at the rotating speed of 350 rpm. Then heating the mixed powder which is evenly mixed by ball milling to 800 ℃ at the heating rate of 5 ℃/min and calcining for 1 h.
And (4) conclusion: the XRD pattern of the product (measured by X-ray diffractometer model D8) was analyzedAs shown in fig. 5. As can be seen, the product is a product with Li as the main crystal phase 0.6 Al 0.6 Si 2.4 O 6 The purity of the petalite powder is 82.9 percent (Diffrac. eva software matched with a D8X-ray diffractometer is adopted to quantitatively calculate the phase Li of the petalite in the sample powder 0.6 Al 0.6 Si 2.4 O 6 Content of (b). The microscopic morphology of the powder is shown in FIG. 6, which shows that the particle size of the powder is 5 to 15 μm.
From the first to third examples, it can be seen that the purity of petalite powder in the final product gradually increases by gradually increasing the percentage amount of Al powder when the Al powder accounts for 1-3% by mass of the mixture.
Example four:
all the steps of example 1 were repeated, except that the amount of Al powder added was 1.5 g.
And (4) conclusion: the XRD pattern of this product (measured using an X-ray diffractometer model D8) was analyzed as shown in FIG. 7. As can be seen, the product has a main crystal phase of Li 0.6 Al 0.6 Si 2.4 O 6 The purity of the petalite powder is 68.5 percent (Diffrac. eva software matched with a D8X-ray diffractometer is adopted to quantitatively calculate the phase Li of the petalite in the sample powder 0.6 Al 0.6 Si 2.4 O 6 The content of (a). The microscopic morphology of the powder is shown in FIG. 8, which shows that the particle size of the powder is 8-15 μm.
Example five:
all the steps of example 1 were repeated, except that the amount of Al powder added was 3 g.
And (4) conclusion: the XRD pattern of this product (measured using X-ray diffractometer model D8) was analyzed as shown in FIG. 9. As can be seen, the product has a main crystal phase of Li 0.6 Al 0.6 Si 2.4 O 6 The purity of the petalite powder is 50% (Diffrac. eva software matched with D8X-ray diffractometer is adopted to quantitatively calculate the Li phase of the petalite in the sample powder 0.6 Al 0.6 Si 2.4 O 6 Content of (d). The micro-morphology of the powder is as followsAs shown in FIG. 10, the particle diameter of the powder was 8 to 15 μm.
The fourth and fifth examples change the percentage of the Al powder in the mixture to be higher than 3%, the purity of the petalite powder is significantly reduced, and the purity of the petalite powder is lower as the mass ratio of the Al powder is higher.
From the first to fifth embodiments, it can be seen that the content of the petalite powder is increased as the content of the aluminum powder is increased within the range of 1 to 3 mass percent of the Al powder as an additive. However, when the content of the Al powder exceeds 3 mass%, the content of the petalite powder finally generated is reduced along with the increase of the content of the Al powder.
Comparative example 1
The procedure of example 1 was repeated, except that no Al powder was added.
And (4) conclusion: the XRD pattern analysis of the product is shown in fig. 11. As can be seen, the product is a powder material with alumina and lithium silicate as main crystal phases, and is non-tetragonal petalite powder.
It can be seen from the comparison between examples one to five and comparative example 1 that whether the addition of Al powder is critical to the formation of tetragonal petalite at 700 ℃.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (5)
1. A method for preparing tetragonal petalite powder, which is characterized in that,
the method comprises the following steps: preparing a mixture comprising 76 to 78 wt% SiO 2 9 to 10 wt% of Li 2 CO 3 9 to 11 wt% of Al 2 O 3 1-3 wt% of Al powder;
step two: preparing mixture powder by ball milling, and carrying out ball milling treatment on the mixture obtained in the step two to obtain the mixture powder;
and step three, calcining the mixture powder obtained in the step two to obtain high-purity tetragonal crystal petalite powder.
2. The method for preparing the tetragonal petalite powder according to claim 1, wherein the rotation speed of the ball milling treatment in the second step is 350-500 rpm.
3. The preparation method of the tetragonal petalite powder according to claim 1, wherein the temperature is raised to 600-800 ℃ at 5 ℃/min under the condition of normal temperature, and the temperature is kept for 1-2 h.
4. The method for preparing the tetragonal petalite powder according to claim 1, wherein the diameter of Al powder particles in the mixture obtained in the second step is 70-100 nm.
5. The method for preparing the tetragonal petalite powder according to claim 1, wherein the temperature is raised to 700 ℃ at 5 ℃/min under the condition of normal temperature in the third step, and the temperature is kept for 1 h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3499787A (en) * | 1965-08-12 | 1970-03-10 | Nippon Toki Kk | Method of manufacturing low thermal-expansion porcelain |
| CN88100211A (en) * | 1988-01-09 | 1988-08-03 | 景德镇陶瓷学院 | Low expansion ceramic and manufacture method thereof |
| CN101113093A (en) * | 2007-06-30 | 2008-01-30 | 景德镇陶瓷学院 | Castorite/cordierite multi-phase low-buckling ceramic and preparation method thereof |
| CN112358286A (en) * | 2020-12-02 | 2021-02-12 | 黄新开 | Artificially synthesized tetragonal petalite and its preparing process |
-
2022
- 2022-05-13 CN CN202210521486.8A patent/CN114890430B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3499787A (en) * | 1965-08-12 | 1970-03-10 | Nippon Toki Kk | Method of manufacturing low thermal-expansion porcelain |
| CN88100211A (en) * | 1988-01-09 | 1988-08-03 | 景德镇陶瓷学院 | Low expansion ceramic and manufacture method thereof |
| CN101113093A (en) * | 2007-06-30 | 2008-01-30 | 景德镇陶瓷学院 | Castorite/cordierite multi-phase low-buckling ceramic and preparation method thereof |
| CN112358286A (en) * | 2020-12-02 | 2021-02-12 | 黄新开 | Artificially synthesized tetragonal petalite and its preparing process |
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