CN1281498C - Method of preparing nanometer magnesium oxide using uniform precipitation-supercritical carbon dioxide drying method - Google Patents
Method of preparing nanometer magnesium oxide using uniform precipitation-supercritical carbon dioxide drying method Download PDFInfo
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 33
- 238000002210 supercritical carbon dioxide drying Methods 0.000 title claims abstract description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000001556 precipitation Methods 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 11
- -1 enamel Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- 159000000003 magnesium salts Chemical class 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 8
- 229960004756 ethanol Drugs 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000000352 supercritical drying Methods 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 3
- 238000006073 displacement reaction Methods 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 2
- 235000011285 magnesium acetate Nutrition 0.000 claims description 2
- 239000011654 magnesium acetate Substances 0.000 claims description 2
- 229940069446 magnesium acetate Drugs 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 2
- 230000003252 repetitive effect Effects 0.000 claims description 2
- 238000005201 scrubbing Methods 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 239000012456 homogeneous solution Substances 0.000 claims 8
- 238000012423 maintenance Methods 0.000 claims 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000002244 precipitate Substances 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 abstract description 2
- 210000003298 dental enamel Anatomy 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 abstract 2
- 239000000347 magnesium hydroxide Substances 0.000 abstract 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 abstract 2
- 239000002537 cosmetic Substances 0.000 abstract 1
- 238000004377 microelectronic Methods 0.000 abstract 1
- 239000000123 paper Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 7
- 239000007791 liquid phase Substances 0.000 description 5
- 239000012808 vapor phase Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 235000011147 magnesium chloride Nutrition 0.000 description 1
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical class O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 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
- 239000012071 phase Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a method for preparing nanometer magnesium oxide by a supercritical carbon dioxide drying method through homogeneous precipitation, which belongs to the technical field of the preparation of nanometer materials. The method mainly comprises the steps that magnesium hydroxide precipitates are prepared by a homogeneous precipitation method in a water solution; water in the precipitates is replaced by ethanol, and ethanol in the precipitates are removed by a supercritical CO2 drying method; the ethanol is separated by a separator and recovered, and CO2 can be used in the circulation mode; dried magnesium hydroxide is calcined at a high temperature to obtain nanometer MgO powders. The method solves the agglomeration problem existing during drying for the preparation of nanometer powders and has the advantages of simple operation technology and easy industrialization realization. Nanometer magnesium oxide has a wide application prospect in the fields of ceramic, enamel, medicine, cosmetics, paint, paper, aviation, military affairs, quantum devices, microelectronics, etc.
Description
Technical field
The invention belongs to the nano material preparation technical field, particularly the novel process of nano-MgO powder preparing.
Background technology
Nano magnesia is a kind of novel inorganic functional material, has a wide range of applications at aspects such as pottery, enamel, medical science, makeup, paint, paper and aviations.Nano magnesia and superpolymer or other materials are compounded with good microwave absorbing function.Adopt nano magnesia, do not need sintering aid just can realize low-temperature sintering and make fine and close thin brilliant pottery, this pottery is expected to develop into the tip materials of using under high temperature, high etching condition.Nano magnesia can be used as the sintering aid and the stablizer of the high-quality nanophase zirconia ceramics of preparation, alumina-ceramic, ferric oxide pottery simultaneously.Nano magnesia also can be used as fat-splitting agent and pharmaceuticals polish.The nano magnesia thin-film material can be used as PbTiO
3The monocrystal chip material of ferroelectric membranc and YBCO superconducting film and high-temperature superconductor dielectric insulation material have important application prospects in fields such as military affairs, quantum device, microtronics.
According to the state of reaction mass, preparation method for nanometer magnesium oxide can be divided into vapor phase process, solid phase method and liquid phase method.Vapor phase process can be divided into two kinds of physical vapor deposition PVD and chemical vapour deposition CVD.More than nano oxidized magnesium particle purity height, narrow particle size distribution, the good dispersitys of two kinds of vapor phase processs preparation.But vapor phase process is to the equipment requirements height, and preparation temperature requires high, so energy consumption is big, and chemical Vapor deposition process also can produce obnoxious flavour.And product collection difficulty, also have a lot of problems to need to solve so want to realize large-scale industrial production.Solid phase method is difficult to prepare the magnesia particle of particle diameter less than 100nm, needs to adopt to strengthen the means of pulverizing, and introduces impurity easily, and particle morphology also is difficult to control.Liquid phase method is the main means of present nano magnesia powder synthetic, can be divided into direct precipitation method, sluggish precipitation, reverse precipitation method etc. according to the different liquid phase methods of technological process.Agglomeration traits is a great problem of nano powder preparation always, is accompanied by in liquid phase production, drying, storage and the application process of nano-powder because reunite, and the existence of coacervate can have a strong impact on the performance of nano material, as moulding, dispersion and sintering etc.When liquid phase method prepares nano magnesia, add the agglomeration traits that suitable dispersion agent can solve liquid reaction phase, it is still very serious to reunite when still adopting common desiccating method that powder is carried out drying.
Summary of the invention
The purpose of this invention is to provide a kind of technology simple, produce that this is cheap, be easy to realize that the magnesian using uniform precipitation-supercritical carbon dioxide desiccating method of industrial amplification production high quality nano prepares the method for nano magnesia.
Technical solution of the present invention is: comprise Preparation by Uniform Precipitation precipitation, solvent exchange, supercritical CO
2Drying and high-temperature calcination process, processing step is:
(1) first is 2 with urea and magnesium salts in molar ratio: 1-6: 1 is mixed with the aqueous solution that magnesium ion is the 1-4 mol, adds the dispersion agent of 1-5% by mass percentage simultaneously, and heating in water bath reacts ageing after 2-6 hour to 348-373K and stirring, suction filtration, washing;
(2) solvent exchange process: the precipitation dehydrated alcohol repetitive scrubbing that filtration washing is intact, every washing is changed a dehydrated alcohol 3-5 time, soaks 8-24 hour then, and filtering and washing, and water is replaced fully;
(3) precipitation behind the solvent exchange is put into the supercritical drying device, from the CO of steel cylinder
2Gas is regulated CO after condenser liquefaction, high-pressure pump pressurization and well heater heat up
2Flow is 1.0-4.0kg/h, is forced into 8-33MPa, is warming up to 305-395K then, keeps the constant temperature and pressure 2-8 of system hour, slowly is cooled to 300-365K, and the ethanol in filter cake is fully by supercritical CO
2After the displacement, the adjusting decompression rate is 0.05-0.2MPa/min, contains alcoholic acid CO
2Enter in the separator, isolated liquid ethanol reclaims uses gas CO
2Recycle, system cools are taken out dry sample to 293-303K;
(4) drying is intact sample was calcined 2-5 hour under 623-923K, obtained the nano magnesia powder.
Magnesium salts is a magnesium chloride.
Magnesium salts is a magnesium nitrate.
Magnesium salts is a magnesium acetate.
Magnesium salts is a sal epsom.
Dispersion agent is a polyoxyethylene glycol-400.
Dispersion agent is a polyoxyethylene glycol-1000.
Dispersion agent is a polyoxyethylene glycol-6000.
Dispersion agent is a sodium lauryl sulphate.
The beneficial effect that the present invention reached is:
1, carry out supercritical drying with conventional solvents such as carbonic acid gas replacement ethanol, service temperature and pressure significantly reduce, and energy consumption is low, and technology is simple, easily control;
2, technology of the present invention is easy to realize industrial amplification production;
3, present method synthetic nano magnesia powder has characteristics such as particle is little, monodispersity good, specific surface area is big, absorption property is good.
4, the present invention adopts supercritical CO
2Desiccating method prepares the generation that the nano magnesia powder has solved drying process powder reuniting body well.
Description of drawings
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is the nano magnesia particulate X-ray diffractogram that the present invention prepares.
Fig. 3 is the nano magnesia particulate transmission electron microscope picture that the present invention prepares.
Embodiment
(1) 101.5 gram Magnesium dichloride hexahydrates, 120.0 gram urea and 250 gram water are put into 1000 milliliters there-necked flask, add 1.0 gram polyoxyethylene glycol-1000 and 0.8 gram polyoxyethylene glycol-400 simultaneously, heating in water bath is to 363K, reacted 4 hours, ageing 5 hours, suction filtration is used deionized water wash, until detecting no chlorion with silver nitrate solution.
(2) precipitate 10 times with absolute ethanol washing, soaked then 24 hours, suction filtration washs 6 times again, to guarantee that water is replaced fully.
(3) product that (2) are obtained is put into the supercritical drying device, from the CO of steel cylinder
2Gas reaches supercritical state after condenser liquefaction, high-pressure pump pressurization and well heater heat up, kept constant temperature and pressure 3 hours at 16MPa and 333K, and the ethanol in filter cake is fully by supercritical CO
2After the displacement, regulating decompression rate is to 0.1MPa/min, contains the CO of small amount of ethanol
2Mixture enters in the separator, and isolated liquid ethanol reclaims uses gas CO
2Recycle is treated system cools to room temperature, takes out dry sample from moisture eliminator.
(4) dry sample was calcined 3 hours under 773K, obtained the magnesium oxide powder that particle diameter is 20nm.
Claims (9)
1. precipitation from homogeneous solution-supercritical co desiccating method prepares the method for nano magnesia, it is characterized in that, comprises Preparation by Uniform Precipitation precipitation, solvent exchange, supercritical CO 2 drying and high-temperature calcination process, and processing step is:
(1) first is 2 with urea and magnesium salts in molar ratio: 1-6: 1 is mixed with the aqueous solution that magnesium ion is the 1-4 mol, adds the dispersion agent of 1-5% by mass percentage simultaneously, and heating in water bath reacts ageing after 2-6 hour to 348-373K and stirring, suction filtration, washing;
(2) solvent exchange process: the precipitation dehydrated alcohol repetitive scrubbing that filtration washing is intact, every washing is changed a dehydrated alcohol 3-5 time, soaks 8-24 hour then, and filtering and washing;
(3) precipitation behind the solvent exchange is put into the supercritical drying device, CO2 gas from steel cylinder liquefies through condenser, after high-pressure pump pressurization and well heater heat up, regulating the CO2 flow is 1.0-4.0kg/h, be forced into 8-33MPa, be warming up to 305-395K then, the constant temperature and pressure 2-8 of maintenance system hour, slowly be cooled to 300-365K, after the ethanol in the filter cake was fully by the supercritical CO 2 displacement, the adjusting decompression rate was 0.05-0.2MPa/min, contains alcoholic acid CO2 and enters in the separator, isolated liquid ethanol reclaims to be used, gas CO2 recycle, system cools are taken out dry sample to 293-303K;
(4) drying is intact sample was calcined 2-5 hour under 623-923K, obtained the nano magnesia powder.
2. precipitation from homogeneous solution according to claim 1-supercritical co desiccating method prepares the method for nano magnesia, it is characterized in that, magnesium salts is a magnesium chloride.
3. precipitation from homogeneous solution according to claim 1-supercritical co desiccating method prepares the method for nano magnesia, it is characterized in that, magnesium salts is a magnesium nitrate.
4. precipitation from homogeneous solution according to claim 1-supercritical co desiccating method prepares the method for nano magnesia, it is characterized in that, magnesium salts is a magnesium acetate.
5. precipitation from homogeneous solution according to claim 1-supercritical co desiccating method prepares the method for nano magnesia, it is characterized in that, magnesium salts is a sal epsom.
6. precipitation from homogeneous solution according to claim 1-supercritical co desiccating method prepares the method for nano magnesia, it is characterized in that, dispersion agent is a polyoxyethylene glycol-400.
7. precipitation from homogeneous solution according to claim 1-supercritical co desiccating method prepares the method for nano magnesia, it is characterized in that, dispersion agent is a polyoxyethylene glycol-1000.
8. precipitation from homogeneous solution according to claim 1-supercritical co desiccating method prepares the method for nano magnesia, it is characterized in that, dispersion agent is a polyoxyethylene glycol-6000.
9. precipitation from homogeneous solution according to claim 1-supercritical co desiccating method prepares the method for nano magnesia, it is characterized in that, dispersion agent is a sodium lauryl sulphate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410155314 CN1281498C (en) | 2004-09-27 | 2004-09-27 | Method of preparing nanometer magnesium oxide using uniform precipitation-supercritical carbon dioxide drying method |
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| CN 200410155314 CN1281498C (en) | 2004-09-27 | 2004-09-27 | Method of preparing nanometer magnesium oxide using uniform precipitation-supercritical carbon dioxide drying method |
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| CN1281498C true CN1281498C (en) | 2006-10-25 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102884576B (en) * | 2010-03-31 | 2016-07-06 | 同和电子科技有限公司 | Metallic magnetic powder and manufacture method thereof and magnetic coating and magnetic recording media |
| CN102113699B (en) * | 2010-11-19 | 2012-11-21 | 广东海洋大学 | Device and method for drying food by supercritical carbon dioxide |
| CN105293570B (en) * | 2015-10-16 | 2016-12-07 | 上海纳旭实业有限公司 | Ultrasonic wave added supercritical carbon dioxide process prepares the method for mesoporous tin oxide antimony material |
| CN105271318B (en) * | 2015-11-23 | 2017-03-22 | 中国科学院青海盐湖研究所 | Preparation method of magnesium oxide nanocrystalline |
| CN106430263B (en) * | 2016-09-13 | 2017-09-15 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of magnesium oxide nanoparticle |
| CN106397231B (en) * | 2016-09-14 | 2018-06-29 | 江苏道博化工有限公司 | A kind of synthetic method of solvent red 207 |
| CN106984062B (en) * | 2017-03-28 | 2019-02-01 | 桂林电子科技大学 | A kind of efficient complex compound wet gel solvent method of replacing |
| CN113184883A (en) * | 2021-05-11 | 2021-07-30 | 青海施丹弗化工有限责任公司 | Method for continuously producing nano magnesium oxide |
| CN114180605B (en) * | 2021-12-31 | 2024-02-06 | 青海创信电子材料有限公司 | Preparation method of magnesium oxide particles |
| CN114291832B (en) * | 2021-12-31 | 2024-01-30 | 青海创信电子材料有限公司 | Preparation method of magnesium hydroxide |
| CN114920279B (en) * | 2022-05-09 | 2023-10-24 | 西南石油大学 | Preparation method and application of oxygen carrier for low-temperature oxidation of methane to prepare hydrogen |
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