WO2012055323A1 - Method for preparing na-β"-al2o3 powder - Google Patents
Method for preparing na-β"-al2o3 powder Download PDFInfo
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- WO2012055323A1 WO2012055323A1 PCT/CN2011/080784 CN2011080784W WO2012055323A1 WO 2012055323 A1 WO2012055323 A1 WO 2012055323A1 CN 2011080784 W CN2011080784 W CN 2011080784W WO 2012055323 A1 WO2012055323 A1 WO 2012055323A1
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- 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
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/028—Beta-aluminas
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- 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
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- the specific preparation method of the present invention is as follows:
- the obtained Na-P-Al 2 O 3 powder after calcination for 12 hours, the X-ray diffraction spectrum of the comparative product is shown in Fig. 1.
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Abstract
A method for preparing Na-β"-Al2O3 powder. The method is characterized by reacting of high purity aluminum with aqueous solutions of sodium hydroxide and lithium hydroxide at a certain temperature to obtain aluminum hydroxide precipitate, then removing water from the resultant solid-liquid mixture by decompression evaporation to obtain a powder mixture containing aluminum hydroxide, sodium hydroxide and lithium hydroxide and high temperature calcining the mixture to obtain the Na-β"-Al2O3 powder. The method in this invention has advantages of low requirements for processing condition, environmental friendness, low cost and good repeatability, and is especially suitable for large scale production.
Description
—种 Ν3-β"-ΑΙ203粉体的制备方法 技术领域 -Preparation method of Ν3-β"-ΑΙ 2 0 3 powder
本发明涉及一种 Na-P-Al203粉体的制备方法， 属于无机非金 属材料粉体制备领域。 技术背景 The invention relates to a preparation method of a Na-P-Al 2 O 3 powder, belonging to the field of preparation of inorganic non-metallic material powder. technical background
Na-P-Al203粉体由于具有较高的 Na 离子导电率， 可以作为 一种固体电解质应用于钠硫电池及多种电化学装置中， 是一种新 能源材料。 Na-P-Al203粉体性能的好坏直接影响着钠硫电池核心 部件固体电解质陶瓷管的质量。 制备 Na-P-Al203粉体的传统方法 是固相反应法， 即以氧化铝或氢氧化铝与钠化合物混合、 烧结制 备， 该方法工艺简单、 设备投资小， 但物料混合不均匀、 反应温 度高、 时间长、 合成产品纯度低、 粒径大且分布不均匀。 为了避 免固相法的缺点， 人们开发了金属醇盐溶胶-凝胶法、 无机盐溶胶 -凝胶法。 金属醇盐溶胶 -凝胶法虽然可以使反应物组分在溶液中 以分子级水平均勾混合，增大组分接触反应面积，加速反应进程， 降低了焙烧温度， 但金属醇盐价格较贵， 且反应介质需要有机溶 剂， 导致成本较高以及规模制备时的安全隐患问题。 采用无机金 属盐溶胶-凝胶法， 如中国发明专利 200910264429.0 采用铝、 钠 的硝酸盐为原料， 虽然降低了成本，但一般需要加入有机添加剂， 并且在干燥及焙烧过程中会释放出有害气体如 N02, NO等， 造 成环境问题， 同时溶胶-凝胶法制备周期长、 过程较为繁瑣。 为了 避免现有制备方法的诸多弊端， 本发明以金属铝、 氢氧化钠为原 料、 水为介质可以制得高质量的 Na-P-Al203粉体。
发明内容 Na-P-Al 2 0 3 powder is a new energy material because it has high conductivity of Na ion and can be used as a solid electrolyte in sodium-sulfur batteries and various electrochemical devices. The performance of the Na-P-Al 2 0 3 powder directly affects the quality of the solid electrolyte ceramic tube of the core component of the sodium-sulfur battery. The conventional method for preparing the Na-P-Al 2 0 3 powder is a solid phase reaction method, which is prepared by mixing and sintering aluminum oxide or aluminum hydroxide with a sodium compound. The method is simple in process, small in equipment investment, but uneven in material mixing. The reaction temperature is high, the time is long, the purity of the synthetic product is low, the particle size is large, and the distribution is uneven. In order to avoid the disadvantages of the solid phase method, a metal alkoxide sol-gel method and an inorganic salt sol-gel method have been developed. The metal alkoxide sol-gel method can make the reactant components in the solution to be mixed at the molecular level, increase the contact reaction area of the components, accelerate the reaction process, and lower the calcination temperature, but the metal alkoxide is more expensive. And the reaction medium requires an organic solvent, resulting in high cost and safety hazard problems in scale preparation. The inorganic metal salt sol-gel method, such as the Chinese invention patent 200910264429.0, uses aluminum and sodium nitrate as raw materials. Although the cost is lowered, it is generally required to add an organic additive, and a harmful gas is released during drying and roasting. N0 2 , NO, etc., cause environmental problems, and the preparation period of the sol-gel method is long and the process is cumbersome. In order to avoid many disadvantages of the prior preparation methods, the present invention can produce high quality Na-P-Al 2 O 3 powder by using aluminum metal, sodium hydroxide as a raw material and water as a medium. Summary of the invention
本发明的目的是提供一种 Na- β -A 1203粉体制备方法，其特征在于 采用金属铝与氢氧化钠、 氢氧化锂水溶液反应制得氢氧化铝沉淀， 反 应液经减压浓缩、 干燥、 煅烧、 粉碎后得到 Na- P-A1203粉体。 The object of the present invention is to provide a method for preparing a powder of Na-β-A 1 2 3 3 , which is characterized in that aluminum hydroxide is precipitated by reacting aluminum metal with sodium hydroxide or lithium hydroxide aqueous solution, and the reaction solution is decompressed. After concentration, drying, calcination, and pulverization, a Na-P-A1 2 3 powder was obtained.
本发明制备氢氧化铝的原理是： The principle of the preparation of aluminum hydroxide of the present invention is:
NaOH/LiOH NaOH/LiOH
3H20 ► Al (OH) 3H 2 0 ► Al (OH)
本发明的具体制备方法如下： The specific preparation method of the present invention is as follows:
( 1)将金属铝加入到氢氧化钠和氢氧化锂的混合水溶液中， 金属铝质量与混合水溶液体积的比例为 5克 /100毫升- 12克 /100毫 升， 控制温度在 60- 80C 搅拌反应 5- 15小时， 得到固液混合物； 其 中氢氧化钠的浓度为 0.35-0.60 mol/L,氢氧化锂的浓度为 0.05-0.12 mol/L,使其对应生成的 A1203、 Na20与 Li20的质量比例为 A1203: Na20: Li20 =(89.0-91.5): (8.0-10.0): (0.3-0.75)， 从而确保其产物是 P 相； (1) Adding aluminum metal to a mixed aqueous solution of sodium hydroxide and lithium hydroxide, the ratio of the mass of the metal aluminum to the volume of the mixed aqueous solution is 5 g / 100 ml - 12 g / 100 ml, and the temperature is controlled at 60-80 C. 5-15 hours, a solid-liquid mixture is obtained; wherein the concentration of sodium hydroxide is 0.35-0.60 mol/L, and the concentration of lithium hydroxide is 0.05-0.12 mol/L, which corresponds to the generated A1 2 0 3 , Na 2 0 The mass ratio to Li 2 0 is A1 2 0 3 : Na 2 0: Li 2 0 = (89.0-91.5): (8.0-10.0): (0.3-0.75), thereby ensuring that the product is phase P;
( 2) 所得固液混合物在 80-100"C下、 压力 -0. IMPa 下匀速搅拌 去除水分得到氢氧化铝、 氢氧化钠和氢氧化锂的粉体混合物； (2) The obtained solid-liquid mixture is stirred at a constant pressure of 80-100"C under a pressure of -0. IMPa to remove water to obtain a powder mixture of aluminum hydroxide, sodium hydroxide and lithium hydroxide;
( 3)将步驟（2)所得粉体混合物在 1100- ΠΟΟΌ煅烧 2-10小时 后， 得到氧化铝粉体； (3) Step (2) After the resultant powder mixture 1100- ΠΟΟΌ calcined for 2 to 10 hours, to obtain an alumina powder;
( 4)将步骤（3)所得氧化铝粉体置于气流磨中粉碎、 过筛得到 Na-β -Α1203粉体。 (4) The alumina powder obtained in the step (3) is pulverized in a jet mill and sieved to obtain a Na-β-Α1 2 3 powder.
为了保证所获 Na- β -Α1203产品的晶相纯度需要控制金属铝、氢氧 化钠、 氢氧化锂的比例使其对应的质量比 A1203: Na20: Li20 = (89.0-91.5): (8.0-10.0): (0.3-0.75)。 In order to ensure the purity of the crystal phase of the obtained Na-β-Α1 2 0 3 product, it is necessary to control the ratio of metal aluminum, sodium hydroxide and lithium hydroxide to make the corresponding mass ratio A1 2 0 3 : Na 2 0: Li 2 0 = (89.0-91.5): (8.0-10.0): (0.3-0.75).
替换页 （细则第 26条)
上述金属铝根据 Na-P-Al203产品纯度的要求选择， 为铝片、 铝箔、 铝粉中 的一种或多种混合物， 其纯度范围为 99%-99·9999%。 Replacement page (Article 26) The above metal aluminum is selected according to the purity requirement of the Na-P-Al 2 0 3 product, and is a mixture of one or more of aluminum flakes, aluminum foil and aluminum powder, and the purity thereof ranges from 99% to 99.9999%.
为了保证所获产品的纯度， 所采用的氢氧化钠、 氢氧化锂的 纯度级别为分析纯。 In order to ensure the purity of the obtained product, the purity grade of sodium hydroxide and lithium hydroxide used is analytically pure.
为了使反应平稳进行， 氢氧化钠水溶液的浓度优选范围为 0.35-0.50 mol/L。 氢氧化锂的浓度优选范围为 0.055-0.1mol/L。 In order to allow the reaction to proceed smoothly, the concentration of the aqueous sodium hydroxide solution preferably ranges from 0.35 to 0.50 mol/L. The concentration of lithium hydroxide is preferably in the range of 0.055 to 0.1 mol/L.
减压干燥后粉体混合物在 1100-1200eC煅烧的优选时间范围 为 4-6小时， 就可以得到氧化铝粉体， 进而可以将氧化铝粉体气 流磨中粉碎、 过筛， 得到不同粒径的 Na-P-Al203产物。 After drying under reduced pressure, the preferred time range of calcination of the powder mixture at 1100-1200 e C is 4-6 hours, and alumina powder can be obtained, and then the alumina powder can be pulverized and sieved to obtain different particles. The Na-P-Al 2 0 3 product of the diameter.
以 Al(OH)3、 NaOH、 LiOH为原料固相球磨混合 10小时， 1250Ό焙烧 12小时后，所得产品作为比较例，具体为：称取 41.87 克 Al(OH)3、 3.09 克 NaOH、 0.63 克 LiOH H20 , 对应的 Al2O3:Na2O:Li2O=91.26:8:0.74, 进行球磨混合 10 小时， 然后在 1250。C焙烧 12小时后所得 Na-P-Al203粉体， 比较例产品的 X射 线衍射谱图见图 1， 比较例中产品的晶相纯度大约为 80%, 晶相 纯度不高；而本发明制备的 Na-P-Al203粉体的 X射线衍射谱图见 图 2, 可知本发明所得产品的晶相纯度高于 98%。 The solid phase ball milling with Al(OH) 3 , NaOH and LiOH was carried out for 10 hours, and after 12 hours of calcination for 12 hours, the obtained product was used as a comparative example. Specifically, 41.87 g of Al(OH) 3 , 3.09 g of NaOH and 0.63 g were weighed. LiOH H 2 0 , corresponding Al 2 O 3 :Na 2 O:Li 2 O=91.26:8:0.74, was ball milled for 10 hours, then at 1250. The obtained Na-P-Al 2 O 3 powder after calcination for 12 hours, the X-ray diffraction spectrum of the comparative product is shown in Fig. 1. In the comparative example, the crystal phase purity of the product is about 80%, and the purity of the crystal phase is not high; The X-ray diffraction spectrum of the Na-P-Al 2 O 3 powder prepared by the present invention is shown in Fig. 2, and it is understood that the crystal phase purity of the product obtained by the present invention is higher than 98%.
本发明中反应液经减压浓缩、 干燥、 煅烧、 粉碎后得到 Na-P-Al203粉体， 与以往的制备方法相比， 不需要以价格较高的 醇盐为原料， 降低了成本； 在反应中也不需要加入有机溶剂， 不 会释放有害气体， 避免了环境污染。 附图说明 图 1为比较例的 X射线衍射谱图；
图 2本发明产品的 X射线衍射谱图。 具体实施例 In the present invention, the reaction solution is concentrated under reduced pressure, dried, calcined, and pulverized to obtain a Na-P-Al 2 O 3 powder. Compared with the conventional preparation method, it is not required to use a higher-priced alkoxide as a raw material, and is reduced. Cost; no organic solvent is needed in the reaction, no harmful gas is released, and environmental pollution is avoided. BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is an X-ray diffraction spectrum of a comparative example; Figure 2 is an X-ray diffraction spectrum of the product of the invention. Specific embodiment
实施例 1 Example 1
1. 称取 6.19克 NaOH, 1.26克 LiOH H20溶于 300亳升去 离子水中， 得到氢氧化钠的浓度为 0.5mol/L, 氢氧化锂的浓度为 0.1mol/L的混合溶液， 将混合溶液搅拌加热到 80°C, 在 3小时内 分 5次加入 29克纯度为 99%的金属铝， 加完后， 再继续反应 2 小时， 得到固液混合物， 其中， 金属铝质量与混合水溶液体积的 比例为 9.67克 /100亳升， 对应产物中 A1203、 Na20与 Li20的质 量比例为 Al2O3:Na2O:Li2O=91.26:8:0.74; 1. Weigh 6.19 g of NaOH, 1.26 g of LiOH H 2 0 dissolved in 300 liters of deionized water to obtain a mixed solution of sodium hydroxide concentration of 0.5 mol/L and lithium hydroxide concentration of 0.1 mol/L. The mixed solution was heated to 80 ° C with stirring, and 29 g of metal aluminum having a purity of 99% was added in 5 portions over 3 hours. After the addition, the reaction was further continued for 2 hours to obtain a solid-liquid mixture in which the metal aluminum mass and the mixed aqueous solution were obtained. The volume ratio is 9.67 g / 100 liters, and the mass ratio of A1 2 0 3 , Na 2 0 and Li 2 0 in the corresponding product is Al 2 O 3 : Na 2 O: Li 2 O = 91.26: 8: 0.74;
2. 然后在 80°C， -O.lMpa的条件下减压蒸发去除固液混合 物中的水， 得到白色的 Al(OH)3、 NaOH, LiOH粉体混合物； 2. The water in the solid-liquid mixture is then evaporated under reduced pressure at 80 ° C, -O.lMpa to obtain a white Al(OH) 3 , NaOH, LiOH powder mixture;
3. 将该粉体混合物在 1200°C煅烧 6小时后，得到氧化铝粉 体； 3. After the powder mixture is calcined at 1200 ° C for 6 hours, an alumina powder is obtained;
4. 将所得氧化铝粉体置于气流磨中粉碎、 过筛得到最终的 Na-P-Al203粉体， 其晶相纯度高于 98%。 4. The obtained alumina powder was pulverized in a jet mill and sieved to obtain a final Na-P-Al 2 O 3 powder having a crystal phase purity higher than 98%.
实施例 2 Example 2
1.称取 8.00克 NaOH, 1.26克 LiOH H20溶于 550亳升去离 子水中， 得到氢氧化钠的浓度为 0.35mol/L, 氢氧化锂的浓度为 0.055mol/L的混合溶液， 将混合溶液搅拌加热到 70°C, 在 6小时 内分 5次加入 28克纯度为 99.9999%的金属铝， 加完后， 再继续 反应 2小时， 得到固液混合物， 其中金属铝质量与混合水溶液体 积的比例为 5克 /100亳升， 对应产物中 A1203、 Na20与 Li20的 质量比例为 Al2O3:Na2O:Li2O=89.26:10:0.74; 1. Weigh 8.00 grams of NaOH, 1.26 grams of LiOH H 2 0 dissolved in 550 liters of deionized water, to obtain a mixed solution of sodium hydroxide concentration of 0.35mol / L, lithium hydroxide concentration of 0.055mol / L, will The mixed solution was heated to 70 ° C with stirring, and 28 g of metal aluminum having a purity of 99.9999% was added in 5 hours in 6 hours. After the addition, the reaction was further continued for 2 hours to obtain a solid-liquid mixture in which the mass of the metal aluminum and the volume of the mixed aqueous solution were obtained. The ratio of the ratio is 5 g / 100 liters, the mass ratio of A1 2 0 3 , Na 2 0 and Li 2 0 in the corresponding product is Al 2 O 3 : Na 2 O: Li 2 O = 89.26: 10: 0.74;
2.然后在 90°C , -O.lMpa的条件下减压蒸发去除固液混合物
中的水， 得到白色的 Al(OH)3、 NaOH、 LiOH粉体混合物； 2. Then remove the solid-liquid mixture by evaporation under reduced pressure at 90 ° C, -O.lMpa Water in water to obtain a white Al(OH) 3 , NaOH, LiOH powder mixture;
3.将该粉体混合物在 1100°C煅烧 10 小时后， 得到氧化铝粉 体； 3. After the powder mixture is calcined at 1100 ° C for 10 hours, an alumina powder is obtained;
4.将所得氧化铝粉体置于气流磨中粉碎、 过筛得到最终的 Na-P-Al203粉体， 其晶相纯度高于 98%。 4. The obtained alumina powder was pulverized in a jet mill and sieved to obtain a final Na-P-Al 2 O 3 powder having a crystal phase purity higher than 98%.
实施例 3 Example 3
1.称取 6.96克 NaOH, 0.84克 LiOH'H20溶于 400亳升去离 子水中， 得到氢氧化钠的浓度为 0.43mol/L, 氢氧化锂的浓度为 0.05mol/L的混合溶液， 将混合溶液搅拌加热到 60°C， 在 12小时 内分 5次加入 28.7克纯度为 99.99%的金属铝， 加完后， 再继续 反应 3小时， 得到固液混合物， 其中金属铝质量与混合水溶液体 积的比例为 7.2克： 100亳升， 对应产物中 A1203、 Na20与 Li20 的质量比例为 Al2O3:Na2O:Li2O=90.5:9:0.5; 1. Weigh 6.96 g of NaOH, 0.84 g of LiOH'H 2 0 dissolved in 400 liters of deionized water to obtain a mixed solution of sodium hydroxide concentration of 0.43 mol/L and lithium hydroxide concentration of 0.05 mol/L. The mixed solution was stirred and heated to 60 ° C, and 28.7 g of metal aluminum having a purity of 99.99% was added in 5 hours over 12 hours. After the addition, the reaction was further continued for 3 hours to obtain a solid-liquid mixture in which the metal aluminum mass and the mixed aqueous solution were obtained. The volume ratio is 7.2 g: 100 liters, the mass ratio of A1 2 0 3 , Na 2 0 and Li 2 0 in the corresponding product is Al 2 O 3 :Na 2 O:Li 2 O=90.5:9:0.5;
2.然后在 95°C , -O.lMpa的条件下减压蒸发去除固液混合物 中的水， 得到白色的 Al(OH)3、 NaOH, LiOH粉体混合物； 2. The water in the solid-liquid mixture is then evaporated under reduced pressure at 95 ° C, -O.lMpa to obtain a white Al(OH) 3 , NaOH, LiOH powder mixture;
3.将该粉体混合物在 1200eC煅烧 4小时后，得到氧化铝粉体；3. After the powder mixture is calcined at 1200 e C for 4 hours, an alumina powder is obtained;
4.将所得氧化铝粉体置于气流磨中粉碎、 过筛得到最终的 Na-P-Al203粉体， 其晶相纯度高于 98%。 4. The obtained alumina powder was pulverized in a jet mill and sieved to obtain a final Na-P-Al 2 O 3 powder having a crystal phase purity higher than 98%.
实施例 4 Example 4
1.称取 6.19克 NaOH, 1.26克 LiOH H20溶于 250亳升去离 子水中， 得到氢氧化钠的浓度为 0.6mol/L , 氢氧化锂的浓度为 0.12mol/L的混合溶液， 将混合溶液搅拌加热到 80°C, 在 8小时 内分 5次加入 29克纯度为 99.99%的金属铝， 加完后， 再继续反 应 2小时， 得到固液混合物， 其中金属铝质量与混合水溶液体积 的比例为 12克： 100毫升， 对应产物中 A1203、 Na20与 Li20的 质量比例为 Al2O3:Na2O:Li2O=90.5:9:0.5;
2.然后在 100°C , -O.lMpa的条件下减压蒸发去除固液混合物 中的水， 得到白色的 Al(OH)3、 NaOH、 LiOH粉体混合物； 1. Weigh 6.19 g of NaOH, 1.26 g of LiOH H 2 0 dissolved in 250 liters of deionized water to obtain a mixed solution of sodium hydroxide concentration of 0.6 mol/L and lithium hydroxide concentration of 0.12 mol/L. The mixed solution was stirred and heated to 80 ° C, and 29 g of metal aluminum having a purity of 99.99% was added in 5 hours in 8 hours. After the addition, the reaction was further continued for 2 hours to obtain a solid-liquid mixture in which the mass of the metal aluminum and the volume of the mixed aqueous solution were obtained. The ratio is 12 g: 100 ml, the mass ratio of A1 2 0 3 , Na 2 0 and Li 2 0 in the corresponding product is Al 2 O 3 :Na 2 O:Li 2 O=90.5:9:0.5; 2. The water in the solid-liquid mixture is then evaporated under reduced pressure at 100 ° C, -O.lMpa to obtain a white Al(OH) 3 , NaOH, LiOH powder mixture;
3.将该粉体混合物在 1200eC煅烧 2小时后，得到氧化铝粉体；3. After the powder mixture is calcined at 1200 e C for 2 hours, an alumina powder is obtained;
4.将所得氧化铝粉体置于气流磨中粉碎、 过筛得到最终的 Na-P-Al203粉体， 其晶相纯度高于 98%。
4. The obtained alumina powder was pulverized in a jet mill and sieved to obtain a final Na-P-Al 2 O 3 powder having a crystal phase purity higher than 98%.
Claims
1、 一种 Na-P-Al203粉体的制备方法， 该方法包括以下步骤：A method for preparing a Na-P-Al 2 0 3 powder, the method comprising the steps of:
( 1 )将金属铝加入到氢氧化钠和氢氧化锂的混合水溶液中，控制 温度在 60-80。C， 搅拌反应 5-15小时， 得到固液混合物； (1) Aluminium metal is added to a mixed aqueous solution of sodium hydroxide and lithium hydroxide at a controlled temperature of 60-80. C, stirring the reaction for 5-15 hours to obtain a solid-liquid mixture;
其中， 氢氧化钠的浓度为 0.35-0.60 mol/L , 氢氧化锂的浓度为 0.05-0.12 mol/L, 金属铝质量与混合水溶液体积的比例为 5克 /100亳 升 -12克 /100亳升， 对应产物中 A1203、 Na20与 Li20的质量比例为 A1203: Na20: Li20 =(89·0-91·5):(8·0-10·0): (0.3-0.75); The concentration of sodium hydroxide is 0.35-0.60 mol/L, the concentration of lithium hydroxide is 0.05-0.12 mol/L, and the ratio of the mass of metal aluminum to the volume of mixed aqueous solution is 5 g/100 liters-12 g/100 亳. l, the mass ratio of A1 2 0 3 , Na 2 0 and Li 2 0 in the corresponding product is A1 2 0 3 : Na 2 0: Li 2 0 = (89·0-91·5): (8·0-10 ·0): (0.3-0.75);
( 2 )所得固液混合物在 80-100。C下、压力 -O.lMPa下匀速搅拌去 除水分得到氢氧化铝、 氢氧化钠、 氢氧化锂的粉体混合物； (2) The obtained solid-liquid mixture is at 80-100. C, under pressure -O.lMPa, stir at a constant speed to remove water to obtain a powder mixture of aluminum hydroxide, sodium hydroxide and lithium hydroxide;
( 3 )将步骤（2 ) 所得粉体混合物在 1100-1200。C煅烧 2-10小时 后， 得到氧化铝粉体； (3) The powder mixture obtained in the step (2) is at 1100-1200. After C calcination for 2-10 hours, an alumina powder is obtained;
( 4 )将步骤（3 ) 所得氧化铝粉体置于气流磨中粉碎、 过筛得到 Na-P-Al203粉体。 (4) The alumina powder obtained in the step (3) is pulverized by a jet mill and sieved to obtain a Na-P-Al 2 0 3 powder.
2、 根据权利要求 1所述的 Na-P-Al203粉体制备方法， 其特征在 于所使用的金属铝的纯度均 99%-99.9999%， 为金属铝片、 铝箔、 铝 粉或其混合物。 2. The method for preparing a Na-P-Al 2 O 3 powder according to claim 1, wherein the metal aluminum used has a purity of 99%-99.999%, and is a metal aluminum sheet, an aluminum foil, an aluminum powder or mixture.
3、 根据权利要求 1所述的 Na-P-Al203粉体制备方法， 其特征在 于所述混合水溶液中氢氧化钠的浓度为 0.35-0.50 mol/L。 3. The method for preparing a Na-P-Al 2 O 3 powder according to claim 1, wherein the concentration of sodium hydroxide in the mixed aqueous solution is from 0.35 to 0.50 mol/L.
4、 根据权利要求 1所述的 Na-P-Al203粉体制备方法， 其特征在 于所述混合水溶液中氢氧化锂的浓度为 0.055-0.1 mol/ L。 4. The method for preparing a Na-P-Al 2 O 3 powder according to claim 1, wherein the concentration of lithium hydroxide in the mixed aqueous solution is 0.055-0.1 mol/L.
5、 根据权利要求 1所述的 Na-P-Al203粉体制备方法， 其特征在 于金属铝质量与混合水溶液体积的比例为 6克 /100亳升 -10克 /100亳 升。 5. The method for preparing a Na-P-Al 2 O 3 powder according to claim 1, wherein the ratio of the mass of the metal aluminum to the volume of the mixed aqueous solution is 6 g / 100 liter - 10 g / 100 liter.
6、 根据权利要求 1所述的 Na-P-Al203粉体制备方法， 其特征在 于步骤（3 ) 中所述煅烧为 4-6小时。 6. The method for preparing a Na-P-Al 2 O 3 powder according to claim 1, wherein the calcination in the step (3) is 4 to 6 hours.
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