CN114890430B - Preparation method of tetragonal petalite powder - Google Patents
Preparation method of tetragonal petalite powder Download PDFInfo
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- CN114890430B CN114890430B CN202210521486.8A CN202210521486A CN114890430B CN 114890430 B CN114890430 B CN 114890430B CN 202210521486 A CN202210521486 A CN 202210521486A CN 114890430 B CN114890430 B CN 114890430B
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- 239000000843 powder Substances 0.000 title claims abstract description 80
- 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 52
- 229910052670 petalite Inorganic materials 0.000 title claims abstract description 52
- 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 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 3
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 239000013078 crystal Substances 0.000 abstract description 14
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 229910018068 Li 2 O Inorganic materials 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 239000003832 thermite Substances 0.000 abstract description 4
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000005496 eutectics Effects 0.000 abstract description 2
- 239000012467 final product Substances 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
- 239000000047 product Substances 0.000 description 21
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 238000004458 analytical method Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 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
- 238000007133 aluminothermic reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 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
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000007780 powder milling Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Classifications
-
- 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 preparation method of tetragonal petalite powder, wherein SiO is added into Al powder 2 And Li (lithium) 2 CO 3 In the mixture of (2) will initiate a thermite reaction which releases a significant amount of heat to effect the decomposition reaction Li 2 CO 3 ＝Li 2 O+CO 2 Generates more Li 2 O, simultaneous with the synthesis reaction Li 2 O+8SiO 2 +Al 2 O 3 ＝2LiAlSi 4 O 10 The target reactant of petalite is produced. Since the thermite reaction is a spontaneous exothermic reaction, a large amount of heat is spontaneously released by the lower reaction temperature in the present invention to help the formation of petalite. Meanwhile, the content of Al powder is controlled to be 1-3wt%, the thermit reaction time is controlled, and the Li2O is ensured not to be excessively volatilized to reduce the purity of a final product. The invention does not need petalite as seed crystal initiator, has few process steps, is simple and convenient to operate, and is convenient for large-scale industrialization. The calcining temperature is low, so that the energy consumption can be greatly reduced on the one hand; on the other hand, long-time high-temperature conditions are not needed, so that the component loss caused by volatilization of eutectic matters formed by 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
The petalite with a special crystal structure 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 ores. Such minerals are unevenly present around the world, especially in rare amounts in our country, and therefore are costly to use and present a supply risk. For this reason, many researchers have proposed artificial synthesis of petalite having a negative expansion coefficient.
LiO is generally adopted in the prior art for artificially synthesizing petalite 2 、SiO 2 And Al 2 O 3 Calcining at 1800 ℃ to generate LiAlSi 4 O 10 Petalite material. The reaction conditions are that materials are generated by adopting higher reaction temperature, and obviously, the energy consumption is high and the yield is low.
A technical scheme with tetragonal petalite is disclosed in the name of CN112358286A and the preparation method thereof. In the scheme, tetragonal petalite is an isomer of monoclinic natural petalite and has the same thermal negative expansion performance as natural petalite. The specific scheme is that 1-3wt% of natural petalite powder is introduced as seed crystal, and the growth and purification of tetragonal petalite are initiated by calcining (higher than 1300 ℃). The technical scheme is a typical artificial petalite scheme with thermal expansion performance. However, in this scheme, the natural petalite powder is still required to be used as seed crystals for synthesizing the target material.
Accordingly, the applicant further studied to develop a technical scheme capable of artificially synthesizing tetragonal petalite without using natural petalite powder as seed crystal and at a lower calcination temperature.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of tetragonal petalite powder, which aims to artificially synthesize tetragonal petalite without introducing natural petalite seed crystal.
A preparation method of tetragonal petalite powder,
step one: preparing a mixture comprising 76 to 78wt% of SiO 2 9 to 10wt% of Li 2 CO 3 9 to 11wt% of Al 2 O 3 1 to 3wt% of Al powder;
step two: ball milling is carried out to prepare mixture powder, and ball milling treatment is carried out to the mixture obtained in the step two to obtain mixture powder;
step three: and (3) calcining the mixture powder in the step two to obtain high-purity tetragonal petalite powder.
Preferably, the rotational speed of the ball milling treatment in the step II is 350-500 rpm.
And further, heating to the calcination temperature of 600-800 ℃ at 5 ℃/min under the condition of normal temperature, and preserving heat for 1-2 h.
Preferably, the Al powder particle size in the mixture in the second step is 70-100 nm.
The invention providesThe preparation method of the tetragonal petalite powder has the beneficial effects that the applicant discovers that the addition of the Al powder is realized by the SiO 2 And Li (lithium) 2 CO 3 In the mixture of (2) will initiate a thermite reaction which releases a significant amount of heat to effect the decomposition reaction Li 2 CO 3 ＝Li 2 O+CO 2 Generates more Li 2 O, simultaneous with the synthesis reaction Li 2 O+8SiO 2 +Al 2 O 3 ＝2LiAlSi 4 O 10 The target reactant of petalite is produced. Since the thermite reaction is a spontaneous exothermic reaction, a large amount of heat is spontaneously released by the lower reaction temperature in the present invention to help the formation of petalite. Meanwhile, the content of Al powder is controlled to be 1-3wt% in the invention, the thermit reaction time is controlled, and Li is ensured 2 O does not volatilize excessively to reduce the purity of the final product. The invention does not need petalite as seed crystal initiator, has few process steps, is simple and convenient to operate, and is convenient for large-scale industrialization. The calcining temperature is low, so that the energy consumption can be greatly reduced on the one hand; on the other hand, long-time high-temperature conditions are not needed, so that the component loss caused by volatilization of eutectic matters formed by lithium oxide and other substances is reduced, and the yield is increased. According to the invention, aluminum powder is introduced, on one hand, the calcination temperature is reduced through aluminothermic reaction, and meanwhile, the aluminum powder reacts with impurities (ferric oxide) in other substances to remove the impurities, so that the purity of the synthesized tetragonal petalite is high.
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 biological substance according to an embodiment of the present invention;
FIG. 2 is a diagram of the microscopic morphology of a biological object according to an embodiment of the present invention;
FIG. 3 is an XRD pattern of the second product of example II of the invention;
FIG. 4 is a diagram of the microscopic morphology of the second product of the embodiment of the present invention;
FIG. 5 is an XRD pattern of the third product of the invention;
FIG. 6 is a diagram of the microscopic morphology of the third product of the embodiment of the present invention;
FIG. 7 is an XRD pattern of the fourth product of the invention;
FIG. 8 is a diagram of the microscopic morphology of the fourth product of the present invention;
FIG. 9 is an XRD pattern of the fifth product of the invention;
FIG. 10 is a diagram of the microscopic morphology of the fifth product of the embodiment of the present invention;
FIG. 11 is an XRD pattern of the product of this comparative example;
Detailed Description
The technical solutions 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.
Embodiment one:
23.4g of SiO was weighed out 2 Powder, 3.3g of Al 2 O 3 Powder, 0.3g of Al powder, 3g of Li 2 CO 3 The powder was mixed and then ball-milled for 36 hours using a ball mill at a rotational speed of 350 rpm. And then heating the mixed powder which is uniformly mixed by ball milling to 700 ℃ at a heating rate of 5 ℃/min, and calcining for 1h.
Conclusion: the XRD pattern (measured using a D8 type X-ray diffractometer) analysis of this product is shown in FIG. 1. As can be seen from the figure, the product is 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 (the petalite phase Li in the sample powder is quantitatively calculated by using Diffrac. Eva software matched with a D8X-ray diffractometer 0.6 Al 0.6 Si 2.4 O 6 Content of (d) in the composition). The microscopic morphology of the powder is shown in FIG. 2, and as can be seen from FIG. 2, the particle size of the powder is 5 to 15. Mu.m.
Embodiment two:
23.4g of SiO was weighed out 2 Powder, 3g of Al 2 O 3 Powder, 0.6g of Al powder, 3g of Li 2 CO 3 The powder was mixed and then ball-milled for 36 hours using a ball mill at a rotational speed of 350 rpm. Then ball milling and mixingThe uniform mixed powder is heated to 600 ℃ at a heating rate of 5 ℃/min and calcined for 1h.
Conclusion: the XRD pattern (measured using a D8 type X-ray diffractometer) analysis of this product is shown in FIG. 3. As can be seen from the figure, the product is Li as the main crystal phase 0.6 Al 0.6 Si 2.4 O 6 The purity of the petalite powder is 82.5 percent (the petalite phase Li in the sample powder is quantitatively calculated by using Diffrac. Eva software matched with a D8X-ray diffractometer 0.6 Al 0.6 Si 2.4 O 6 Content of (d) in the composition). The microscopic morphology of the powder is shown in FIG. 4, and the particle size of the powder is 5 to 15. Mu.m.
Embodiment III:
23.4g of SiO was weighed out 2 Powder, 2.7g of Al 2 O 3 Powder, 0.9g of Al powder, 3g of Li 2 CO 3 The powder was mixed and then ball-milled for 36 hours using a ball mill at a rotational speed of 350 rpm. And then heating the mixed powder which is uniformly mixed by ball milling to 800 ℃ at a heating rate of 5 ℃/min, and calcining for 1h.
Conclusion: the XRD pattern (measured using a D8 type X-ray diffractometer) analysis of this product is shown in FIG. 5. As can be seen from the figure, the product is 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 (the petalite phase Li in the sample powder is quantitatively calculated by using Diffrac. Eva software matched with a D8X-ray diffractometer 0.6 Al 0.6 Si 2.4 O 6 Content of (d) in the composition). The microscopic morphology of the powder is shown in FIG. 6, and the particle size of the powder is 5 to 15. Mu.m.
From examples one to three, it is known that the purity of the Al powder in the resultant is gradually increased by gradually increasing the percentage amount of the Al powder when the mass percentage of the Al powder in the mixture is in the range of 1 to 3%.
Embodiment four:
all the steps of example 1 were repeated except that the amount of Al powder added was 1.5g.
Conclusion: XRD pattern of the product (usingD8 type X-ray diffractometer test) analysis is shown in fig. 7. As can be seen from the figure, the product is Li as the main crystal phase 0.6 Al 0.6 Si 2.4 O 6 The purity of the petalite powder is 68.5 percent (the petalite phase Li in the sample powder is quantitatively calculated by using Diffrac. Eva software matched with a D8X-ray diffractometer 0.6 Al 0.6 Si 2.4 O 6 Is contained in the composition. The microscopic morphology of the powder is shown in FIG. 8, and the particle size of the powder is 8 to 15. Mu.m.
Fifth embodiment:
all the steps of example 1 were repeated, except that the amount of Al powder added was 3g.
Conclusion: the XRD pattern (measured using a D8 type X-ray diffractometer) analysis of this product is shown in FIG. 9. As can be seen from the figure, the product is Li as the main crystal phase 0.6 Al 0.6 Si 2.4 O 6 The purity of the petalite powder is 50 percent (the Li phase of petalite in the sample powder is quantitatively calculated by using Diffrac.eva software matched with a D8X-ray diffractometer 0.6 Al 0.6 Si 2.4 O 6 Content of (d) in the composition). The microscopic morphology of the powder is shown in FIG. 10, and the particle size of the powder is 8 to 15. Mu.m.
The percentage of the Al powder in the mixture is changed to be higher than 3% in the fourth embodiment and the fifth embodiment, the purity of the petalite powder is obviously 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 is known that the Al powder as an additive increases the final formation content of petalite powder with the increase of the aluminum powder content in the mass percentage content range of 1% -3%. However, when the content of Al powder exceeds 3% by mass, the content of petalite powder finally produced is reduced instead as the content of Al powder is increased.
Comparative example 1
The procedure of example 1 was repeated, except that no Al powder was added.
Conclusion: the XRD pattern analysis of this product is shown in FIG. 11. From the figure, the product is a powder material with aluminum oxide and lithium silicate as main crystal phases, and is not tetragonal petalite powder.
From the comparison of examples one to five with comparative example 1, it is known whether the addition of Al powder is critical to the formation of petalite in the tetragonal phase at 700 ℃.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (3)
1. A preparation method of tetragonal petalite powder is characterized in that,
step one: preparing a mixture comprising 76-78 wt% SiO 2 9 to 10 percent wt percent of Li 2 CO 3 9 to 11wt% of Al 2 O 3 1-3wt% of Al powder;
step two: ball milling to prepare mixture powder: ball milling is carried out on the mixture to obtain mixture powder, wherein the diameter size of Al powder particles in the mixture is 70-100 nm;
and thirdly, heating the mixture powder in the second step to a calcination temperature of 600-800 ℃ at a speed of 5 ℃/min under the normal temperature condition, and preserving heat for 1-2 hours to obtain the high-purity tetragonal petalite powder.
2. The method for preparing the tetragonal petalite powder according to claim 1, wherein the rotation speed of the secondary ball milling treatment is 350-500 rpm.
3. 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 step three, and the temperature is kept for 1h.
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| CN202210521486.8A CN114890430B (en) | 2022-05-13 | 2022-05-13 | Preparation method of tetragonal petalite powder |
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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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