Búsqueda Imágenes Maps Play YouTube Noticias Gmail Drive Más »
Iniciar sesión
Usuarios de lectores de pantalla: deben hacer clic en este enlace para utilizar el modo de accesibilidad. Este modo tiene las mismas funciones esenciales pero funciona mejor con el lector.

Patentes

  1. Búsqueda avanzada de patentes
Número de publicaciónCN104003446 A
Tipo de publicaciónSolicitud
Número de solicitudCN 201410234166
Fecha de publicación27 Ago 2014
Fecha de presentación29 May 2014
Fecha de prioridad29 May 2014
También publicado comoCN104003446B
Número de publicación201410234166.X, CN 104003446 A, CN 104003446A, CN 201410234166, CN-A-104003446, CN104003446 A, CN104003446A, CN201410234166, CN201410234166.X
Inventores宋盼淑, 王军, 任同祥, 周涛
Solicitante中国计量科学研究院
Exportar citaBiBTeX, EndNote, RefMan
Enlaces externos:  SIPO, Espacenet
Preparation method of high-purity molybdenum trioxide
CN 104003446 A
Resumen
The invention discloses a preparation method of high-purity molybdenum trioxide. High-purity molybdenum trioxide is obtained by oxidizing and purifying molybdenum powder. The method comprises the following steps: firstly, performing oxidation reaction on molybdenum in the presence of air to obtain molybdenum trioxide, wherein a heating process comprises the following steps: (1) heating to 100-200 DEG C and keeping the constant temperature, and (2) further heating to 550-650 DEG C and performing oxidation reaction; secondly, purifying, wherein the purifying process comprises the following steps: (1) putting molybdenum trioxide into a closed container and arranging a collecting pipe in the container; (2) heating the region in which molybdenum trioxide is arranged, to 100-150 DEG C; vacuumizing the container to be 10Pa-100Pa and keeping the constant temperature and the constant pressure; (3) stopping vacuumizing, heating the region in which molybdenum trioxide is arranged, to 600-720 DEG C and keeping the constant temperature; (4) further vacuumizing the container to be 10Pa-100Pa and keeping the constant pressure for 120-150 minutes. The process for preparing molybdenum trioxide is simple, the requirement on purification or preparation of a micro molybdenum reagent in a lab can be met, and the purity of the prepared molybdenum reagent reaches up to 99.99%.
Reclamaciones(6)  traducido del chino
1.一种高纯三氧化钥的制备方法,包括如下步骤: 在空气存在的条件下,钥金属单质粉末经氧化反应得到三氧化钥; 所述氧化反应的升温过程如下: 1)将温度升至100°C~20(TC,并保持恒温; 2)继续升温至550°C~650°C,进行所述氧化反应。 A method for preparing a high-purity oxide keys, comprising the steps of: in the presence of air, the key elemental metal powder obtained by the oxidation reaction trioxide key; during heating the oxidation reaction are as follows: 1) the temperature rise to 100 ° C ~ 20 (TC, and maintain a constant temperature; 2) continue to heat up to 550 ° C ~ 650 ° C, carry out the oxidation reaction.
2.根据权利要求1所述的制备方法,其特征在于:所述方法还包括对所述三氧化钥进行纯化的步骤: 1)将所述三氧化钥置于一封闭的容器中,并在所述容器中设置收集管; 2)加热所述三氧化钥所在区域,使温度升至100~150°C ;对所述容器进行抽真空至10~lOOPa,并保持恒温恒压; 3)停止抽真空,并使所述三氧化钥所在区域的温度升至600°C~720°C,且保持恒温; 4)继续对所述容器进行抽真空至10~lOOPa,并保持恒压120~150min,即在所述收集管中收集得到升华提纯后的三氧化钥。 The production method according to claim 1, characterized in that: said method further comprises the step of purification of the key trioxide were: 1) the key trioxide was placed in a closed container, and collection tube disposed in said container; 2) heating the trioxide key location, and the temperature was raised to 100 ~ 150 ° C; on the vessel evacuated to 10 ~ lOOPa, and maintain constant temperature and pressure; 3) Stop vacuum, and the temperature in your area trioxide key rose 600 ° C ~ 720 ° C, and maintain a constant temperature; and 4) continue to be evacuated from the vessel 10 ~ lOOPa, and maintain constant pressure 120 ~ 150min that collected in the collection tube to give trioxide key after sublimation purification.
3.根据权利要求1或2所述的制备方法,其特征在于:所述氧化反应的升温过程中,步骤I)中,在20~40min 内所述恒温的时间为30~60min。 3. The production method according to claim 1 or claim 2, wherein: heating the oxidation reaction process, step I), the time at the constant temperature of 20 ~ 40min to 30 ~ 60min.
4.根据权利要求1-3中任一项所述的制备方法,其特征在于:所述氧化反应的升温过程中,步骤2)中,在60~90min内将温度升至550°C~650°C ; 所述氧化反应的时间为480~960min。 4. The process according to any one of claims 1-3, characterized in that: the heating process in the oxidation reaction, step 2), the inside temperature was raised to 60 ~ 90min 550 ° C ~ 650 ° C; the reaction time of the oxidation is 480 ~ 960min.
5.根据权利要求2-4中任一项所述的制备方法,其特征在于:所述纯化的步骤中,步骤2)中,在20~40min内将温度升至100°C~150°C ; 所述恒温恒压的保持时间为30~60min。 5. The process according to any one of claims 2-4, characterized in that: the purification step, step 2), when the temperature was raised to 20 ~ 40min 100 ° C ~ 150 ° C ; the constant temperature and pressure holding time of 30 ~ 60min.
6.根据权利要求2-5中任一项所述的制备方法,其特征在于:所述纯化的步骤中,步骤3)中,在60~90min内将温度升至600°C~720°C ; 所述恒温的保持时间为120~150min。 6. The process according to any one of claims 2-5, characterized in that: the purification step, step 3), the inner temperature was raised to 60 ~ 90min 600 ° C ~ 720 ° C ; the constant temperature holding time is 120 ~ 150min.
Descripción  traducido del chino

一种高纯三氧化钼的制备方法 A method for preparing high purity molybdenum trioxide

技术领域 Technical Field

[0001] 本发明涉及一种高纯三氧化钥的制备方法,属于高纯金属氧化物制备技术领域。 [0001] The present invention relates to a method for preparing high purity oxide key belongs to the technical field of the preparation of high purity metal oxides. 背景技术 Background

[0002] 在自然界中,钥有7种稳定同位素,分别为92Mo、94Mo、95Mo、96Mo、97Mo、98Mo和iciqMo。 [0002] In nature, there are seven key stable isotopes, respectively 92Mo, 94Mo, 95Mo, 96Mo, 97Mo, 98Mo and iciqMo. 当地质和海洋环境的氧化-还原状态发生变化时,可导致钥同位素的质量分馏。 When the oxide geology and marine environment - when you restore the state changes can lead to key isotope mass fractionation. 同时,钥元素是植物、动物和人体内多种酶的重要组成部分。 Meanwhile, the key element is an important part of plant, animal and human body a variety of enzymes. 因此,建立钥元素含量和同位素丰度比测量方法对地球化学、地质学和生物学等领域的研究具有重要意义。 Therefore, establishing key element content and isotope ratio measurements in the field of research geochemistry, geology and biology of great significance. 通常采用质量百分比^ 99.99%的钥金属单质或钥化合物,制备钥成分或同位素标准物质,从而提高测量结果的可靠性和准确度。 Usually mass percentage of 99.99% ^ key metal simple substance or compound key, key ingredients or preparation isotope reference material, thereby improving the reliability of the measurement results and accuracy. 由于目前市售的高纯钥试剂种类少,价格昂贵,且货期较长,建立钥元素纯化方法,制备纯度> 99.99%的钥试剂具有重要的应用价值。 Due to the current commercially available high-purity reagents few key species, expensive and long delivery time, establish key elements of the purification process, the preparation of a purity of> 99.99% of the key agents have important applications. 另一方面,高纯三氧化钥是一种重要的化工原料,主要用于生产高纯钥金属单质和钥的化合物,以及在石油工业中用作催化剂。 On the other hand, high-purity oxide key is an important chemical raw materials, mainly for the production of compounds of high purity elemental metal key and key, as well as used as a catalyst in the petroleum industry.

[0003] 文献中主要采用离子交换法,如:阴、阳离子交换树脂法,螯合树脂法和阴离子交换树脂法,对复杂基体样品如土壤、血清中的钥元素进行分离和富集。 [0003] The literature mainly used ion exchange, such as: anion and cation exchange resin, chelating resin and anion exchange resin method, complex matrix samples such as soil, serum separation and enrichment of the key elements. 这类方法操作复杂,通常需要使用两种树脂或重复操作2次才能达到高纯试剂的纯度要求;同时,纯化过程中使用硝酸、盐酸、氢氟酸或氨水等化学试剂,这些化学试剂中的杂质元素容易对样品产生污染。 Such methods complex operation, generally requires the use of two types of resins or repeat twice to reach the purity of high purity reagents; at the same time, the purification process using nitric acid, hydrochloric acid, hydrofluoric acid or ammonia and other chemical agents, these chemical reagents impurity elements likely to contaminate the sample. [0004] 在专利申请“一种钥粉的纯化方法”(公开号为“CN101347839A”)中公开了一种以普通钥粉为原料,经过水洗或酸洗除杂,烘干,高温氢气保护除杂或真空高温除杂,真空筛分等过程制得纯化的钥粉的方法。 [0004] The patent application discloses a "method for purifying a key powder" (published as "CN101347839A") in an ordinary key powder as raw material, after acid washing or cleaning, drying, high temperature protection in addition to hydrogen Key powder as miscellaneous or high-temperature vacuum cleaning, vacuum sieving process to obtain purified. 采用该方法纯化后的钥粉中钥的质量百分比为99.94%~99.95%。 Using this method the mass percentage of key powder purified key is 99.94% to 99.95%.

[0005] 工业上主要采用两种工艺路线对三氧化钥粉末(又称钥焙砂)进行纯化,制备高纯三氧化钥。 [0005] The industry mainly uses two process routes for key trioxide powder (also known as the key calcine) was purified preparation of high purity trioxide key. 一种称为湿法:即由钥焙砂经氨浸,湿法提纯净化,生产成仲钥酸铵,仲钥酸铵经加热分解,去除氨气,从而获得高纯三氧化钥;另一种称为火法,由钥焙砂直接加热,钥焙砂中杂质残留在焙烧渣中,而大部分三氧化钥经升华再结晶,生成高纯三氧化钥。 Called wet: that by ammonia leaching, wet purification purify calcine by the key, secondary key production into ammonium, secondary ammonium key decomposed by heating to remove ammonia to obtain high-purity oxide key; another species called Fire, directly heated by key calcine, key calcine impurities remain in the firing residue, and most trioxide key by sublimation recrystallization, high purity oxide generated key. 由于反应温度对纯化效果的影响较大,在工业生产中采用湿法或火法纯化后得到的三氧化钥的纯度一般不闻于99.95%。 Since the reaction temperature greater impact on the effect of purification, use purified wet or Fire get trioxide key purity in industrial production generally does not smell at 99.95%.

发明内容 DISCLOSURE

[0006] 本发明的目的是提供一种高纯三氧化钥的制备方法,利用本方法制备的三氧化钥纯度> 99.99%。 [0006] The object of the present invention is to provide a high-purity oxide-key preparation methods, with the present method of preparing trioxide key purity> 99.99%. 基于钥单质的化学性质和三氧化钥易升华的性质,本发明采取两步法对普通纯度的钥试剂进行纯化。 Based on the chemical properties of elemental key and key trioxide easy sublimation of nature, the present invention is a two-step method for ordinary purity key reagents for purification.

[0007] 本发明提供的一种高纯三氧化钥的制备方法,包括如下步骤: [0007] A method for preparing high purity oxide of the present invention provides a key, comprising the steps of:

[0008] 第一步,在空气存在的条件下,钥金属单质粉末经氧化反应得到三氧化钥; [0008] The first step, in the presence of air, the key elemental metal powder obtained by the oxidation reaction trioxide key;

[0009] 所述氧化反应的升温过程如下:[0010] I)将温度升至100°C~200°C,并保持恒温; [0009] The oxidation reaction of the heating process is as follows: [0010] I) The temperature was raised to 100 ° C ~ 200 ° C, and maintained a constant temperature;

[0011] 2)继续升温至550°C~650°C,进行所述氧化反应。 [0011] 2) continue to heat up to 550 ° C ~ 650 ° C, carry out the oxidation reaction.

[0012] 第二步,对所述三氧化钥进行纯化: [0012] The second step of the purified trioxide key:

[0013] I)将所述三氧化钥置于一封闭的容器中,并在所述容器中设置收集管; [0013] I) the key trioxide was placed in a closed vessel and collection tube disposed in said container;

[0014] 2)加热所述三氧化钥所在区域,使温度升至100~150°C;对所述容器进行抽真空至IOPa~lOOPa,并保持恒温恒压; [0014] 2) heating said third key location oxide, the temperature was raised to 100 ~ 150 ° C; for the container is evacuated to IOPa ~ lOOPa, and maintain constant temperature and pressure;

[0015] 3)停止抽真空,并使所述三氧化钥所在区域的温度升至600°CC~720°C,保持恒温; [0015] 3) Stop the vacuum, and the temperature in your area trioxide key rose 600 ° CC ~ 720 ° C, to maintain a constant temperature;

[0016] 4)继续对所述容器进行抽真空至IOPa~lOOPa,并保持恒压120~150min,即在所述收集管中收集得到升华提纯后的三氧化钥。 [0016] 4) continue to be evacuated from the vessel IOPa ~ lOOPa, and maintain constant pressure 120 ~ 150min, namely in the collection tube collected trioxide key after sublimation purification.

[0017] 上述的制备方法中,所述第一步氧化反应的升温过程中,步骤I)中,在20~40min内将温度升至100°C~200°C,具体可在30min内升温至150°C ; [0017] The production method described above, the first step of heating the oxidation reaction process, step I), at 20 ~ 40min and the temperature was raised to 100 ° C ~ 200 ° C, allowed to warm to specifically in 30min 150 ° C;

[0018] 所述恒温的保持时间为30~60min,具体可为30min。 Thermostat [0018] The retention time of 30 ~ 60min, particularly for 30min.

[0019] 上述的制备方法中,所述第一步氧化反应的升温过程中,步骤2)中,在60~90min内将温度升至550°C~650°C,具体可在60min内升温至580°C或600°C ; [0019] The production method described above, the first step of the process of heating the oxidation reaction in step 2), when the temperature was raised to 60 ~ 90min 550 ° C ~ 650 ° C, in particular can be raised to 60min 580 ° C or 600 ° C;

[0020] 所述氧化反应的时间为480~960min,具体可为480min~720min、480min~540min、540min ~720min、480min、540min 或720mino [0020] The oxidation reaction time was 480 ~ 960min, specifically for 480min ~ 720min, 480min ~ 540min, 540min ~ 720min, 480min, 540min or 720mino

[0021] 上述的制备方法中,所述第一步氧化反应结束之后降温至300°C~400°C,具体可降至350°C~400°C、350°C、370°C或400°C。 [0021] The production method described above, the first step after the end of the oxidation reaction is cooled to 300 ° C ~ 400 ° C, can be reduced particularly 350 ° C ~ 400 ° C, 350 ° C, 370 ° C or 400 ° C.

[0022] 上述的制备方法中,所述第二步纯化的步骤中,步骤2)中,在20~40min内将温度升至100°C~150°C,具体可在30min内升温至至150°C ; [0022] The production method described above, the second step of the purification step, step 2), when the temperature was raised to 20 ~ 40min 100 ° C ~ 150 ° C, in particular can be heated to 150 to 30min ° C;

[0023] 所述恒温恒压的保持时间为30~60min,具体可为30min。 [0023] The constant temperature and pressure holding time of 30 ~ 60min, particularly for 30min.

[0024] 上述的制备方法中,所述第二步纯化的步骤中,步骤3)中,在60~90min内将温度升至600°C~720°C,具体可在60min内将温度升至600°C~675°C、600°C、625°C或675 °C ; [0024] The production method described above, the purification step of the second step, Step 3), 60 ~ 90min within the temperature was raised to 600 ° C ~ 720 ° C, in particular within the temperature was raised to 60min 600 ° C ~ 675 ° C, 600 ° C, 625 ° C or 675 ° C;

[0025] 所述恒温的保持时间具体为30~60min,具体可为30min。 [0025] The isothermal holding time specifically 30 ~ 60min, particularly for 30min.

[0026] 上述的制备方法中,所述第二步纯化的步骤中,步骤4)中,所述恒压的保持时间具体可为120min ~135min、125min ~135min、120min、125min 或135min。 [0026] The above-mentioned production method, the second step of the purification step, step 4), the holding time constant specific for 120min ~ 135min, 125min ~ 135min, 120min, 125min or 135min.

[0027] 本发明方法制备得到的三氧化钥的纯度≥99.99%。 The method of the invention was prepared trioxide key of [0027] The purity ≥99.99%.

[0028] 本发明制备高纯三氧化钥的操作过程简单,能够满足实验室纯化或制备几十毫克到几百毫克微量钥试剂的需求,同时由于纯化过程中不加入任何化学试剂,能够减少杂质的引入,纯化后可制得纯度> 99.99%的高纯钥试剂。 [0028] The procedure for preparing high-purity oxide of the present invention is simple key to meet the laboratory preparation of purified or tens of milligrams to several hundred milligrams of trace key reagent requirements, and because of the purification process does not add any chemicals, can reduce impurities The introduction of purity can be obtained after purification> 99.99% high purity key reagents.

具体实施方式 DETAILED DESCRIPTION

[0029] 下述实施例中所使用的实验方法如无特殊说明,均为常规方法。 Experimental methods used in the examples [0029] The following examples if no special instructions, all conventional methods.

[0030] 本发明下述实施例中,三氧化钥纯化方法的回收率按照下述公式计算: [0030] The following embodiment of the present invention, the purification method of key recovery trioxide calculated according to the following formula:

[0031] [0031]

Figure CN104003446AD00041

[0032] 本发明下述实施例中采用高分辨电感耦合等离子体质谱仪分析纯化前钥金属单质粉末以及纯化后制得三氧化钥中杂质的含量。 [0032] Examples of the use of high resolution inductively coupled plasma mass spectrometer content before purification key elemental metal powder and purified to obtain trioxide key impurities in the following embodiment of the present invention.

[0033] 具体测试条件如下:在2% (v/v)的硝酸中配置浓度分别为lng/g的铍、铟和铋的混合溶液,对高分辨电感耦合等离子体质谱仪的仪器条件进行最佳化选择。 [0033] Specific test conditions are as follows: Configure concentration in 2% (v / v) nitric acid were mixed solution of lng / g of beryllium, indium and bismuth, for high resolution inductively coupled plasma mass spectrometer instrument conditions most Best Choice. 68种金属、非金属元素的多元素混合溶液标准物质(BW3197-BW3200)购买自中国计量科学研究院。 68 kinds of multi-element metal and non-metallic elements mixed solution reference material (BW3197-BW3200) purchased from China Institute of Metrology.

[0034] 具体测试方法如下:在2% (v/v)的硝酸中将上述多元素混合溶液标准物质稀释至浓度分别为lng/g, 5ng/g, 10ng/g作为标准溶液。 [0034] The specific test methods are as follows: at 2% (v / v) of nitric acid in the mixed solution of the above-described multi-element standard material were diluted to a concentration lng / g, 5ng / g, 10ng / g as a standard solution. 通过标准曲线法半定量分析样品中67种杂质的含量,从而计算得到纯化前钥金属单质粉末以及纯化后三氧化钥的纯度。 The standard curve by semi quantitative analysis of the sample 67 kinds of impurities, thus calculated before purification key elemental metal oxide powder and purified key purity.

[0035] 下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。 [0035] The following, if no special illustrative embodiment the materials used, reagents, etc., can be obtained from commercial sources.

[0036] 本发明下述实施例中使用的钥金属单质粉末原料颗粒度为100目。 Key elemental metal powder material particles used in the following examples of embodiment of the [0036] The present invention is a 100 mesh.

[0037] 实施例1、高纯三氧化钥的制备 1. Preparation of high-purity oxide key examples of [0037]

[0038] 原料为天然丰度钥金属单质,钥的质量百分比为99.89%。 [0038] the natural abundance of key raw materials for the metal elements, key mass percentage of 99.89%. 称取钥粉末原料605.64mg置于石英烧杯中,放入马弗炉内加热,通入空气进行氧化反应。 Key raw material powder was weighed into a quartz beaker 605.64mg, placed in a muffle furnace heated air through an oxidation reaction. 升温过程如下: Heating process is as follows:

[0039] I)打开马弗炉,30min将温度由室温升温至150°C,稳定30min以除去其中吸附的水分及其他可能的气体杂质; [0039] I) to open the muffle furnace, 30min the temperature was raised from room temperature to 150 ° C, stable 30min to remove the adsorbed water and possibly other gaseous impurities;

[0040] 2)60min将温度由150°C升温至600°C,氧化时间为480min,以确保钥粉末充分氧化; [0040] 2) 60min the temperature was raised by the 150 ° C to 600 ° C, the oxidation time was 480min, to ensure that the key fully oxidized powder;

[0041] 3)停止加热,马弗炉内温度降温至400°C时,打开马弗炉,将装有三氧化钥粉末的烧杯取出,放入真空保干器内冷却至室温; When the [0041] 3) Stop heating muffle furnace temperature was lowered to 400 ° C, open muffle furnace, will be equipped with three key oxide powder beaker removed, placed in a vacuum dessicator to cool to room temperature;

[0042] 对上述氧化得到的三氧化钥粉末进行纯化,具体步骤如下: [0042] The key trioxide powder was subjected to the oxidation purification, follow these steps:

[0043] I)称取116.22mg三氧化钥粉末置于石英舟内; [0043] I) weighed 116.22mg key trioxide powder was placed in a quartz boat;

[0044] 2)将石英舟缓慢放入一端封闭的石英管内,并推动至可温控管式炉的加热中心区域;将石英样品收集管放入石英管内,推动至可温控管式炉加热区域外端;之后,将石英管放入可温控管式炉中,石英管管口与机械真空泵相连; [0044] 2) quartz boat slowly into the quartz tube closed at one end and push to be temperature-controlled tube furnace heated central region; quartz sample collection tube into the quartz tube, pushing to be temperature-controlled tube furnace heating the outer area of the end; after the quartz tube into a tube furnace temperature controlled, quartz tube port to the mechanical vacuum pump;

[0045] 3)打开管式炉,30min将温度由室温升温至150°C,打开机械真空泵,抽真空至lOOPa,稳定30min,以除去其中吸附的水分及其他可能的气体杂质; [0045] 3) Open the tube furnace, 30min the temperature was raised from room temperature to 150 ° C, open the mechanical vacuum pump, vacuum to lOOPa, stable 30min, to remove water and other impurities which may be adsorbed gases;

[0046] 4)关闭真空泵,60min将温度由150°C升温至625°C,稳定30min ; [0046] 4) Close the vacuum pump, 60min the temperature was increased from the 150 ° C to 625 ° C, stable 30min;

[0047] 5)打开机械真空泵,抽真空至lOOPa,蒸发提纯时间为120min,使三氧化钥粉末开始升华并沉积在样品收集管内; [0047] 5) open mechanical vacuum pump, evacuated to lOOPa, evaporation purification time 120min, so that the three key oxide powder starts to sublime and be deposited within the sample collection tube;

[0048] 6)停止加热,保持石英管内真空为lOOPa,三氧化钥粉末在样品石英收集管内自然冷却至室温; [0048] 6) Stop heating, vacuum is maintained within the quartz tube lOOPa, key trioxide powder in a quartz sample collection tube was allowed to cool to room temperature;

[0049]7)关闭机械真空泵和管式炉,从石英管内取出石英样品收集管,获得高纯度的三氧化钥晶体。 [0049] 7) Turn the mechanical vacuum pump and tube furnace, remove the quartz sample collection tube from the quartz tube, high purity crystal key trioxide.

[0050] 纯化后三氧化钥纯度分析: [0050] After purification trioxide key purity analysis:

[0051] 称量收集管中三氧化钥晶体,质量为102.59mg,计算得到利用上述方法制备的三氧化钥的回收率为88.27%。 [0051] Weighing key collection tube trioxide crystals, the quality of 102.59mg, calculated using the above prepared trioxide key recovery of 88.27%.

[0052] 采用高分辨电感耦合等离子体质谱仪分析纯化前钥金属单质粉末以及纯化后制得三氧化钥中杂质的含量。 [0052] The high resolution inductively coupled plasma mass spectrometer content before purification key elemental metal powder and purified to obtain trioxide key in impurities. 结果表明,纯化前钥试剂中钥金属单质的质量百分比为99.89% ;纯化后制得三氧化钥样品中三氧化钥的质量百分比为99.99%。 The results showed that the quality of reagents before purified key percentages key metal elements of 99.89%; weight percentage obtained after purification trioxide trioxide key key sample was 99.99%. [0053] 其中主要杂质元素的含量如表1所示: [0053] wherein the content of the main impurity element as shown in Table 1:

[0054] 表1.纯化前钥粉末原料及纯化后三氧化钥中主要杂质元素的质量百分比) [0054] Table 1 mass% before purification key raw material powder and purified trioxide key major impurity element)

[0055] [0055]

Figure CN104003446AD00061

[0056] a “一”表示在所述实验条件下该元素的含量低于检测限 [0056] a "one" indicates the experimental conditions under which content element is below the detection limit

[0057] 实施例2、高纯三氧化钥的制备 Preparation of high purity oxide keys of Example 2 [0057] Example

[0058] 原料为天然丰度钥金属单质,钥的质量百分比为99.89%。 [0058] The raw material for the natural abundance of key metals, metal key mass percentage of 99.89%. 称取钥粉末原料939.93mg置于石英烧杯中,放入马弗炉内加热,通入空气进行氧化反应。 Key raw material powder was weighed into a quartz beaker 939.93mg, placed in a muffle furnace heated air through an oxidation reaction. 升温过程如下: Heating process is as follows:

[0059] I)打开马弗炉,30min将温度由室温升温至150°C,稳定30min以除去其中吸附的水分及其他可能的气体杂质; [0059] I) to open the muffle furnace, 30min the temperature was raised from room temperature to 150 ° C, stable 30min to remove the adsorbed water and possibly other gaseous impurities;

[0060] 2)60min将温度由150°C升温至600°C,氧化时间为720min,以确保钥粉末充分氧化; [0060] 2) 60min the temperature was raised by the 150 ° C to 600 ° C, the oxidation time was 720min, to ensure that the key fully oxidized powder;

[0061] 3)停止加热,马弗炉内温度降温至350°C时,打开马弗炉,将装有三氧化钥粉末的烧杯取出,放入真空保干器内冷却至室温; When the [0061] 3) Stop heating muffle furnace temperature was lowered to 350 ° C, open muffle furnace, will be equipped with three key oxide powder beaker removed, placed in a vacuum dessicator to cool to room temperature;

[0062] 对上述氧化得到的三氧化钥粉末进行纯化,具体步骤如下: [0062] The key trioxide powder was subjected to the oxidation purification, follow these steps:

[0063] I)称取121.4Img三氧化钥粉末置于石英舟内; [0063] I) weighed 121.4Img key trioxide powder was placed in a quartz boat;

[0064] 2)将石英舟缓慢放入一端封闭的石英管内,并推动至可温控管式炉的加热中心区域;将石英样品收集管放入石英管内,推动至可温控管式炉加热区域外端;之后,将石英管放入可温控管式炉中,石英管管口与机械真空泵相连; [0064] 2) quartz boat slowly into the quartz tube closed at one end and push to be temperature-controlled tube furnace heated central region; quartz sample collection tube into the quartz tube, pushing to be temperature-controlled tube furnace heating the outer area of the end; after the quartz tube into a tube furnace temperature controlled, quartz tube port to the mechanical vacuum pump;

[0065] 3)打开管式炉,30min将温度由室温升温至150°C,打开机械真空泵,抽真空至lOOPa,稳定30min,以除去其中吸附的水分及其他可能的气体杂质; [0065] 3) Open the tube furnace, 30min the temperature was raised from room temperature to 150 ° C, open the mechanical vacuum pump, vacuum to lOOPa, stable 30min, to remove water and other impurities which may be adsorbed gases;

[0066] 4)关闭真空泵,60min将温度由150°C升温至600°C,稳定30min ; [0066] 4) Close the vacuum pump, 60min the temperature was increased from the 150 ° C to 600 ° C, stable 30min;

[0067] 5)打开机械真空泵,抽真空至lOOPa,蒸发提纯时间为135min,使三氧化钥粉末开始升华并沉积在样品收集管内; [0067] 5) open mechanical vacuum pump, evacuated to lOOPa, evaporation purification time 135min, so that the three key oxide powder starts to sublime and be deposited within the sample collection tube;

[0068] 6)停止加热,保持石英管内真空为lOOPa,三氧化钥粉末在样品石英收集管内自然冷却至室温; [0068] 6) Stop heating, vacuum is maintained within the quartz tube lOOPa, key trioxide powder in a quartz sample collection tube was allowed to cool to room temperature;

[0069] 7)关闭机械真空泵和管式炉,从石英管内取出石英样品收集管,获得高纯度的三氧化钥晶体。 [0069] 7) Turn the mechanical vacuum pump and tube furnace, remove the quartz sample collection tube from the quartz tube, high purity crystal key trioxide.

[0070] 纯化后三氧化钥样品纯度分析: [0070] After purification trioxide key sample purity analysis:

[0071] 称量收集管中三氧化钥晶体,质量为104.98mg,计算得到上述方法的回收率为86.47%。 [0071] Weighing collection tube trioxide key crystal quality 104.98mg, calculated by the above method of recovery was 86.47%.

[0072] 采用高分辨电感耦合等离子体质谱仪分析纯化前钥金属单质粉末以及纯化后制得三氧化钥中杂质的含量。 [0072] The high resolution inductively coupled plasma mass spectrometer content before purification key elemental metal powder and purified to obtain trioxide key in impurities. 结果表明,纯化前钥试剂中钥金属单质的质量百分比为99.89% ;纯化后制得三氧化钥样品中三氧化钥的质量百分比为99.99%。 The results showed that the quality of reagents before purified key percentages key metal elements of 99.89%; weight percentage obtained after purification trioxide trioxide key key sample was 99.99%.

[0073] 其中主要杂质元素的含量如表2所示: [0073] wherein the content of the main impurity element as shown in Table 2:

[0074] 表2.纯化前钥粉末原料及纯化后三氧化钥中主要杂质元素的质量百分比) [0074] Table 2 mass% before purification key raw material powder and purified trioxide key major impurity element)

[0075] [0075]

Figure CN104003446AD00071

[0076] [0076]

[0077] a “一”表示在所述实验条件下该元素的含量低于检测限 [0077] a "one" indicates the experimental conditions under which content element is below the detection limit

[0078] 实施例3、高纯三氧化钥的制备 Preparation Example 3, high purity oxide keys of [0078] Example

[0079] 原料为98Mo丰度为98.15%的浓缩钥同位素(金属单质),钥的质量百分比为99.89%。 [0079] materials 98Mo abundance of 98.15% of concentrate key isotopes (metal element), the quality of key percentages of 99.89%. 称取钥粉末原料380.8Img置于石英烧杯中,放入马弗炉内加热,通入空气进行氧化反应。 Key 380.8Img weighed powder raw material into a quartz beaker, placed in a muffle furnace heated air through an oxidation reaction. 升温过程如下: Heating process is as follows:

[0080] I)打开马弗炉,30min将温度由室温升温至150°C,稳定30min以除去其中吸附的水分及其他可能的气体杂质; [0080] I) to open the muffle furnace, 30min the temperature was raised from room temperature to 150 ° C, stable 30min to remove the adsorbed water and possibly other gaseous impurities;

[0081] 2)60min将温度由150°C升温至580°C,氧化时间为540min,以确保钥粉末充分氧化; [0081] 2) 60min the temperature was raised by the 150 ° C to 580 ° C, the oxidation time was 540min, to ensure that the key fully oxidized powder;

[0082] 3)停止加热,马弗炉内温度降温至370°C时,打开马弗炉,将装有三氧化钥粉末的烧杯取出,放入真空保干器内冷却至室温;[0083] 对上述氧化得到的三氧化钥粉末进行纯化,具体步骤如下: When the [0082] 3) Stop heating muffle furnace temperature was lowered to 370 ° C, open muffle furnace, the beaker containing key trioxide powder removed, placed in a vacuum dessicator to cool to room temperature; [0083] for Key oxide powder was subjected to the oxidation purification, follow these steps:

[0084] I)称取139.04mg三氧化钥粉末置于石英舟内; [0084] I) weighed 139.04mg key trioxide powder was placed in a quartz boat;

[0085] 2)将石英舟缓慢放入一端封闭的石英管内,并推动至可温控管式炉的加热中心区域;将石英样品收集管放入石英管内,推动至可温控管式炉加热区域外端;之后,将石英管放入可温控管式炉中,石英管管口与机械真空泵相连; [0085] 2) quartz boat slowly into the quartz tube closed at one end and push to be temperature-controlled tube furnace heated central region; quartz sample collection tube into the quartz tube, pushing to be temperature-controlled tube furnace heating the outer area of the end; after the quartz tube into a tube furnace temperature controlled, quartz tube port to the mechanical vacuum pump;

[0086] 3)打开管式炉,30min将温度由室温升温至150°C,打开机械真空泵,抽真空至IOOPa,稳定30min,以除去其中吸附的水分及其他可能的气体杂质; [0086] 3) Open the tube furnace, 30min the temperature was raised from room temperature to 150 ° C, open the mechanical vacuum pump, vacuum to IOOPa, stable 30min, to remove water and other impurities which may be adsorbed gases;

[0087] 4)关闭真空泵,60min将温度由150°C升温至675°C,稳定30min ; [0087] 4) Close the vacuum pump, 60min the temperature was increased from the 150 ° C to 675 ° C, stable 30min;

[0088] 5)打开机械真空泵,抽真空至lOOPa,蒸发提纯时间为125min,使三氧化钥粉末开始升华并沉积在样品收集管内; [0088] 5) open mechanical vacuum pump, evacuated to lOOPa, evaporation purification time 125min, so that the three key oxide powder starts to sublime and be deposited within the sample collection tube;

[0089] 6)停止加热,保持石英管内真空为lOOPa,三氧化钥粉末在样品石英收集管内自然冷却至室温; [0089] 6) Stop heating, vacuum is maintained within the quartz tube lOOPa, key trioxide powder in a quartz sample collection tube was allowed to cool to room temperature;

[0090] 7)关闭机械真空泵和管式炉,从石英管内取出石英样品收集管,获得高纯度的三氧化钥晶体。 [0090] 7) Turn the mechanical vacuum pump and tube furnace, remove the quartz sample collection tube from the quartz tube, high purity crystal key trioxide.

[0091] 纯化后三氧化钥纯度分析: [0091] After purification trioxide key purity analysis:

[0092] 称量收集管中三氧化钥晶体,质量为121.66mg,计算得到上述方法的回收率为87.50%。 [0092] Weighing collection tube trioxide key crystal quality 121.66mg, calculated by the above method of recovery was 87.50%.

[0093] 采用高分辨电感耦合等离子体质谱仪分析纯化前钥金属单质粉末以及纯化后制得三氧化钥中杂质的含量。 [0093] The high resolution inductively coupled plasma mass spectrometer content before purification key elemental metal powder and purified to obtain trioxide key in impurities. 结果表明,纯化前钥试剂中钥金属单质的质量百分比为99.88% ;纯化后制得三氧化钥样品中三氧化钥的质量百分比为99.99%。 The results showed that the quality of reagents before purified key percentages key metal elements of 99.88%; weight percentage obtained after purification trioxide trioxide key key sample was 99.99%. 其中主要杂质元素的含量如表3所示: Wherein the content of the main impurity element as shown in Table 3:

[0094] 表3.纯化前钥粉末原料及纯化后三氧化钥中主要杂质元素的质量百分比) [0094] Table 3. Quality Percentage key before purification powder materials and purified trioxide key major impurity element)

[0095] [0095]

Figure CN104003446AD00081

[0096] a “一”表示在所述实验条件下该元素的含量低于检测限。 [0096] a "one" indicates the experimental conditions under which content element is below the detection limit.

Citas de patentes
Patente citada Fecha de presentación Fecha de publicación Solicitante Título
CN101092249A *27 Abr 200726 Dic 2007中山大学Method for preparing Nano structure and thin film of molybdenum trioxide by using infrared sintering furnace
CN101254949A *19 Mar 20083 Sep 2008嵩县开拓者钼业有限公司Method for preparing high-pure molybdenum oxide by vacuum decomposition of molybdenite
CN102351249A *21 Jul 201115 Feb 2012华南理工大学Method for preparing molybdenum trioxide in nanometer structure
CN202988768U *12 Oct 201212 Jun 2013嵩县开拓者钼业有限公司High-purity superfine molybdenum trioxide production device
RU2382736C1 * Título no disponible
US6468497 *9 Nov 200022 Oct 2002Cyprus Amax Minerals CompanyMethod for producing nano-particles of molybdenum oxide
Otras citas
Referencia
1 *向铁根: "《钼冶金》", 31 December 2009, article ""单元系烧结"", pages: 342-344
Citada por
Patente citante Fecha de presentación Fecha de publicación Solicitante Título
CN104241624A *24 Sep 201424 Dic 2014南京大学Method for preparing anode material of molybdenum oxide lithium ion battery by controlling oxidation
Clasificaciones
Clasificación internacionalC01G39/02
Eventos legales
FechaCódigoEventoDescripción
27 Ago 2014C06Publication
24 Sep 2014C10Request of examination as to substance
17 Jun 2015C14Granted