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 B
Tipo de publicaciónConcesión
Número de solicitudCN 201410234166
Fecha de publicación17 Jun 2015
Fecha de presentación29 May 2014
Fecha de prioridad29 May 2014
También publicado comoCN104003446A
Número de publicación201410234166.X, CN 104003446 B, CN 104003446B, CN 201410234166, CN-B-104003446, CN104003446 B, CN104003446B, 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 B
Resumen  traducido del chino
本发明公开了一种高纯三氧化钼的制备方法。 The present invention discloses a method for preparing high purity molybdenum trioxide. 以金属钼单质粉末为原料,经氧化和纯化后得到。 Elemental molybdenum metal powder as raw material, obtained after oxidation and purification. 首先,在空气存在的条件下,钼单质经氧化反应得到三氧化钼,其中升温过程包括:1)将温度升至100℃~200℃,并保持恒温;2)继续升温至550℃~650℃,进行氧化反应;其次,纯化步骤包括:1)将所述三氧化钼置于一封闭容器中,并在所述容器中设置收集管;2)加热三氧化钼所在区域,使温度升至100~150℃;对容器抽真空至10Pa~100Pa,并保持恒温恒压;3)停止抽真空,并使三氧化钼所在区域的温度升至600℃~720℃,保持恒温;4)继续对所述容器抽真空至10Pa~100Pa,并保持恒压120~150min。 First, in the presence of air, elemental molybdenum trioxide by oxidation reaction, wherein the heating process comprising: 1) the temperature was raised to 100 ℃ ~ 200 ℃, and maintained a constant temperature; 2) continue to heat up to 550 ℃ ~ 650 ℃ , oxidation reaction; secondly, the purification step comprises: a) the molybdenum trioxide was placed in a closed vessel and collection tube disposed in said container; 2) Area molybdenum trioxide is heated, and the temperature was raised to 100 ~ 150 ℃; the container is evacuated to 10Pa ~ 100Pa, and maintain constant temperature and pressure; and 3) to stop vacuum, and the temperature was raised to molybdenum trioxide Area 600 ℃ ~ 720 ℃, constant temperature; 4) to continue to the said container is evacuated to 10Pa ~ 100Pa, and to maintain constant pressure 120 ~ 150min. 本发明制备高纯三氧化钼的操作过程简单,能够满足实验室纯化或制备微量钼试剂的需求,所制得钼试剂纯度高达99.99%。 Procedure for preparing high purity molybdenum trioxide of the present invention is simple, purified or prepared to meet the needs of laboratory reagents trace amounts of molybdenum, molybdenum prepared reagent purity as high as 99.99%.
Reclamaciones(5)  traducido del chino
1. 一种高纯三氧化钼的制备方法,其特征在于,包括如下步骤: 在空气存在的条件下,钼金属单质粉末经氧化反应得到三氧化钼; 所述氧化反应的升温过程如下: 1) 将温度升至100°c~200°C,并保持恒温; 2) 继续升温至550°C~650°C,进行所述氧化反应; 所述方法还包括对所述三氧化钼进行纯化的步骤: 1) 将所述三氧化钼置于一封闭的容器中,并在所述容器中设置收集管; 2) 加热所述三氧化钼所在区域,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,并使所述三氧化钼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钼。 1. A method for preparing high-purity molybdenum trioxide, which is characterized by comprising the steps of: in the presence of air, elemental molybdenum metal powder obtained by the oxidation reaction of molybdenum trioxide; during heating the oxidation reaction are as follows: 1 ) The temperature was raised to 100 ° c ~ 200 ° C, and maintained a constant temperature; 2) continue to heat up to 550 ° C ~ 650 ° C, performing the oxidation reaction; said method further comprises purifying said molybdenum trioxide Step: 1) the molybdenum trioxide was placed in a closed container, and the collection tube disposed in said container; 2) heating said molybdenum trioxide Area, and the temperature was raised to 100 ~ 150 ° C; for The vessel was evacuated to 10 ~ lOOPa, and maintain constant temperature and pressure; and 3) stop the vacuum, and temperature of the molybdenum trioxide Area rose to 600 ° C ~ 720 ° C, and maintain a constant temperature; 4) Continue to the container evacuated to 10 ~ lOOPa, and maintain constant pressure 120 ~ 150min, namely in the collection tube collected trioxide after sublimation purification.
2. 根据权利要求1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1) 中,在20~40min内将温度升至100°C~200°C ; 所述恒温的时间为30~60min。 The production method according to claim 1, characterized in that: the heating process of the oxidation reaction, step 1), in a 20 ~ 40min and the temperature was raised to 100 ° C ~ 200 ° C; the thermostat The time is 30 ~ 60min.
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。 3. The production method according to claim 1 or claim 2, wherein: heating of said oxidation reaction process, step 2), in a 60 ~ 90min and the temperature was raised to 550 ° C ~ 650 ° C; the said oxidation reaction time was 480 ~ 960min.
4. 根据权利要求1或2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。 4. The production method according to claim 1 or claim 2, wherein: said purification step, step 2), in a 20 ~ 40min and the temperature was raised to 100 ° C ~ 150 ° C; the thermostat constant retention time of 30 ~ 60min.
5. 根据权利要求1或2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。 5. The production method according to claim 1 or claim 2, wherein: said purification step, step 3), the inner temperature was raised to 60 ~ 90min 600 ° C ~ 720 ° C; the thermostat The retention 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钼的制备方法,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 molybdenum trioxide, it belongs to the technical field of the preparation of high purity metal oxides. 背景技术 Background technique

[0002] 在自然界中,钼有7种稳定同位素,分别为92Mo、94Mo、95Mo、 96Mo、97Mo、98Mo和1(l°Mo。 当地质和海洋环境的氧化-还原状态发生变化时,可导致钼同位素的质量分馏。同时,钼元素是植物、动物和人体内多种酶的重要组成部分。因此,建立钼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宄具有重要意义。通常采用质量百分比多99. 99%的钼金属单质或钼化合物,制备钼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。由于目前市售的高纯钼试剂种类少,价格昂贵,且货期较长,建立钼元素纯化方法,制备纯度多99. 99%的钼试剂具有重要的应用价值。另一方面,高纯三氧化钼是一种重要的化工原料,主要用于生产高纯钼金属单质和钼的化合物,以及在石油工业中用作催化剂。 [0002] In nature, there are seven kinds of stable isotopes of molybdenum, respectively 92Mo, 94Mo, 95Mo, 96Mo, 97Mo, 98Mo and 1 (l ° Mo when the oxidation geology and marine environment - when you restore the status change can lead to quality molybdenum isotope fractionation. Meanwhile, molybdenum is an important part of plant, animal and human body a variety of enzymes. Therefore, the establishment of molybdenum content and isotope ratio measurements of geochemistry, geology and biology and other fields a Subsidiary of great significance. usually more than 99.99% by mass percentage of elemental molybdenum or molybdenum compounds, molybdenum component preparation or isotopic reference materials, thereby improving the reliability of the measurement results and accuracy. Because of high purity molybdenum currently marketed reagent type less expensive and longer delivery time, the establishment of molybdenum purification methods, preparation purity of more than 99.99% molybdenum reagent has important application value. On the other hand, high purity molybdenum trioxide is an important chemical raw materials, mainly used for the production of high-purity molybdenum metal compound and elemental molybdenum, and 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、血清中的钼元素进行分离和富集。 [0003] The literature mainly 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 molybdenum. 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 requirements 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 produce sample contamination.

[0004] 在专利申请"一种钼粉的纯化方法"(公开号为"CN101347839A")中公开了一种以普通钼粉为原料,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钼粉的方法。 [0004] In the patent application "method of purifying a molybdenum powder" (published as "CN101347839A") discloses an ordinary molybdenum powder as raw material, after washing or acid cleaning, drying, high temperature hydrogen protection except hybrid or high-temperature vacuum cleaning, vacuum sieving process to obtain purified molybdenum powder method. 采用该方法纯化后的钼粉中钼的质量百分比为99. 94%~99. 95%。 The percentage of quality using this method purified molybdenum powder molybdenum was 99.94% ~ 99.95%.

[0005]工业上主要采用两种工艺路线对三氧化钼粉末(又称钼焙砂)进行纯化,制备高纯三氧化钼。 [0005] The industry mainly uses two process routes for molybdenum trioxide powder (also known as Mo calcine) was purified preparation of high purity molybdenum trioxide. 一种称为湿法:即由钼焙砂经氨浸,湿法提纯净化,生产成仲钼酸铵,仲钼酸铵经加热分解,去除氨气,从而获得高纯三氧化钼;另一种称为火法,由钼焙砂直接加热,钼焙砂中杂质残留在焙烧渣中,而大部分三氧化钼经升华再结晶,生成高纯三氧化钼。 Called wet: that by ammonia leaching, purification of wet purification of molybdenum calcine, the production cost of ammonium paramolybdate, ammonium paramolybdate decomposed by heating to remove ammonia, thereby obtaining high purity molybdenum trioxide; another species called Fire, directly heated by molybdenum calcine, molybdenum calcine impurities remain in the firing residue, and most of the molybdenum trioxide by sublimation recrystallization, generate high-purity molybdenum trioxide. 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钼的纯度一般不高于99. 95%。 Since the reaction temperature greater impact on the effect of purification, use purified wet or pyrometallurgical purity molybdenum trioxide obtained in industrial production is generally not more than 99.95%.

发明内容 SUMMARY OF THE INVENTION

[0006] 本发明的目的是提供一种高纯三氧化钼的制备方法,利用本方法制备的三氧化钼纯度多99. 99%。 [0006] The object of the present invention is to provide a high-purity molybdenum trioxide production method, using the present method of preparing molybdenum trioxide more than 99.99% purity. 基于钼单质的化学性质和三氧化钼易升华的性质,本发明采取两步法对普通纯度的钼试剂进行纯化。 Based on the chemical properties of elemental molybdenum and molybdenum trioxide easy sublimation of nature, the present invention is a two-step method for ordinary purity molybdenum reagent for purification.

[0007]本发明提供的一种高纯三氧化钼的制备方法,包括如下步骤: [0007] A method for preparing high-purity molybdenum trioxide of the present invention provides, comprising the steps of:

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

[0009] 所述氧化反应的升温过程如下: [0009] The temperature during the oxidation reaction are as follows:

[0010] 1)将温度升至100 °C~200 °C,并保持恒温; [0010] 1) The temperature was raised to 100 ° C ~ 200 ° C, and maintain 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,对所述三氧化钼进行纯化: [0012] The second step of the molybdenum trioxide purified:

[0013] 1)将所述三氧化钼置于一封闭的容器中,并在所述容器中设置收集管; [0013] 1) the molybdenum trioxide was placed in a closed container, and the collection tube disposed in said container;

[0014] 2)加热所述三氧化钼所在区域,使温度升至100~150°C;对所述容器进行抽真空至10Pa~lOOPa,并保持恒温恒压; [0014] 2) heating said molybdenum trioxide Area, and the temperature was raised to 100 ~ 150 ° C; of the container is evacuated to 10Pa ~ lOOPa, and to maintain constant temperature and pressure;

[0015] 3)停止抽真空,并使所述三氧化钼所在区域的温度升至600°CC~720°C,保持恒温; [0015] 3) stop the vacuum, and temperature of the molybdenum trioxide Area rose to 600 ° CC ~ 720 ° C, to maintain a constant temperature;

[0016] 4)继续对所述容器进行抽真空至10Pa~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钼。 [0016] 4) continue to be the vessel was evacuated to 10Pa ~ lOOPa, and maintain constant pressure 120 ~ 150min, namely in the collection tube collected trioxide 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1)中,在20~40min 内将温度升至l〇〇°C~200°C,具体可在30min内升温至150°C ; [0017] The production method described above, the first step of the oxidation reaction of the heating process, step 1), the inner temperature was raised to 20 ~ 40min l〇〇 ° C ~ 200 ° C, in particular within 30min was heated to 150 ° C;

[0018] 所述恒温的保持时间为30~60min,具体可为30min。 Thermostat [0018] The holding time is 30 ~ 60min, specifically 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 oxidation reaction of the heating process, the step 2), in a 60 ~ 90min and the temperature was raised to 550 ° C ~ 650 ° C, allowed to warm to specifically within 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720min〇 [0020] The oxidation reaction time was 480 ~ 960min, specifically for 480min ~ 720min, 480min ~ 540min, 540min ~ 720min, 480min, 540min or 720min〇

[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°〇、350°〇、370°〇或400°〇。 [0021] The production method described above, the first step after the end of the oxidation reaction cooled to 300 ° C ~ 400 ° C, it can be reduced particularly 350 ° C ~ 400 ° square, 350 ° square, 370 ° or 400 ° square billion.

[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), in a 20 ~ 40min and the temperature was raised to 100 ° C ~ 150 ° C, particularly within 30min to be heated to 150 ° 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, specifically 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。 [0024] The production method described above, the purification step of the second step, step 3), the inner temperature was raised to 60 ~ 90min 600 ° C ~ 720 ° C, in particular within the temperature was raised to 60min 600 ° C ~ 675 ° C, 600 ° C, 625 ° C or 675. . ;

[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, specifically 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〇 [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〇

[0027] 本发明方法制备得到的三氧化钼的纯度多99. 99%。 Preparation [0027] The present invention is a method to get more purity molybdenum trioxide 99.99%.

[0028] 本发明制备高纯三氧化钼的操作过程简单,能够满足实验室纯化或制备几十毫克到几百毫克微量钼试剂的需求,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,纯化后可制得纯度彡99. 99%的高纯钼试剂。 [0028] The procedure for preparing high purity molybdenum trioxide of the present invention is simple and can be prepared for laboratory purification or tens of milligrams to several hundred milligrams of trace amounts of molybdenum 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 彡 99.99% purity molybdenum 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 Example [0029] The following examples if no special instructions, all conventional methods.

[0030] 本发明下述实施例中,三氧化钼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 process of recovery of molybdenum trioxide calculated according to the following equation:

Figure CN104003446BD00041

[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钼金属单质粉末以及纯化后制得三氧化钼中杂质的含量。 [0032] The following examples of the present invention uses high resolution inductively coupled plasma mass spectrometry analysis of the content before purification elemental molybdenum metal powder and molybdenum trioxide was obtained after purification of impurities.

[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 the 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宄院。 68 kinds of multi-element metal and non-metallic elements mixed solution of standard substance (BW3197-BW3200) purchased from Chinese Academy of Sciences study based metering.

[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 a mixed solution of the above-described multi-element standard material were diluted to a concentration of 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钼金属单质粉末以及纯化后三氧化钼的纯度。 The standard curve by semi quantitative analysis of the sample 67 kinds of impurities, thus calculated before purification elemental molybdenum metal powder and purified purity molybdenum trioxide.

[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, unless otherwise specified in the examples the materials, reagents, etc., can be obtained from commercial sources.

[0036] 本发明下述实施例中使用的钼金属单质粉末原料颗粒度为100目。 Elemental molybdenum metal powder particle size of the raw material used in the following examples of embodiment [0036] The present invention is a 100 mesh.

[0037] 实施例1、高纯三氧化钼的制备 Preparation of high purity molybdenum trioxide of Example 1 [0037] Example

[0038] 原料为天然丰度钼金属单质,钼的质量百分比为99. 89%。 [0038] raw material for the natural abundance of elemental molybdenum, molybdenum mass percentage was 99.89%. 称取钼粉末原料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。 Molybdenum powder material was weighed into a quartz beaker 605. 64mg, placed in a muffle furnace heated air introduced into the oxidation reaction. 升温过程如下: Heating process is as follows:

[0039] 1)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] 1) 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,以确保钼粉末充分氧化; [0040] 2) 60min and the temperature was elevated from 150 ° C to 600 ° C, the oxidation time was 480min, in order to ensure full oxidation of molybdenum powder;

[0041] 3)停止加热,马弗炉内温度降温至400°C时,打开马弗炉,将装有三氧化钼粉末的烧杯取出,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 the beaker containing molybdenum trioxide powder removed, placed in a vacuum dessicator to cool to room temperature;

[0042] 对上述氧化得到的三氧化钼粉末进行纯化,具体步骤如下: [0042] The above-mentioned oxide powder was purified molybdenum trioxide, concrete steps are as follows:

[0043] 1)称取116. 22mg三氧化钼粉末置于石英舟内; [0043] 1) weighed 116. 22mg 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 may be placed in a tube furnace temperature, quartz tube port connected with 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 and the temperature was elevated from 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,使三氧化钼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 is 120min, so that molybdenum trioxide 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,三氧化钼粉末在样品石英收集管内自然冷却至室温; [0048] 6) the heating was stopped, the vacuum is maintained inside the quartz tube lOOPa, molybdenum 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钼晶体。 [0049] 7) Turn off the mechanical vacuum pump and tube furnace, remove the quartz sample collection tube from the quartz tube, high purity molybdenum trioxide crystals.

[0050] 纯化后三氧化钼纯度分析: [0050] After purification of molybdenum trioxide purity analysis:

[0051] 称量收集管中三氧化钼晶体,质量为102. 59mg,计算得到利用上述方法制备的三氧化钼的回收率为88. 27 %。 [0051] Weighing collection tube trioxide crystals, the quality of 102. 59mg, calculated by the above method for preparing the molybdenum trioxide 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钼金属单质粉末以及纯化后制得三氧化钼中杂质的含量。 [0052] content before purification using mass spectrometry analysis of elemental molybdenum metal powder and molybdenum trioxide was obtained after purification of impurities in high resolution inductively coupled plasma. 结果表明,纯化前钼试剂中钼金属单质的质量百分比为99. 89%;纯化后制得三氧化钼样品中三氧化钼的质量百分比为99. 99%。 The results show that the mass percentage of molybdenum in the reagent before purified elemental molybdenum is 99.89 percent; purified samples obtained trioxide mass percent molybdenum trioxide is 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.纯化前钼粉末原料及纯化后三氧化钼中主要杂质元素的质量百分比(% ) [0054] Table 1 mass% before purification and after purification of the raw material powder of molybdenum trioxide main impurity elements (%)

Figure CN104003446BD00061

[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、高纯三氧化钼的制备 Preparation of high purity molybdenum trioxide of Example 2 [0057] Example

[0058] 原料为天然丰度钼金属单质,钼的质量百分比为99. 89%。 [0058] The raw material for the natural abundance of elemental molybdenum, molybdenum mass percentage was 99.89%. 称取钼粉末原料939. 93 mg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。 Weighed 939. 93 mg of molybdenum powder material placed in a quartz beaker, placed in a muffle furnace heated air introduced into the oxidation reaction. 升温过程如下: Heating process is as follows:

[0059] 1)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] 1) 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,以确保钼粉末充分氧化; [0060] 2) 60min and the temperature was elevated from 150 ° C to 600 ° C, the oxidation time was 720min, in order to ensure full oxidation of molybdenum powder;

[0061] 3)停止加热,马弗炉内温度降温至350°C时,打开马弗炉,将装有三氧化钼粉末的烧杯取出,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 the beaker containing molybdenum trioxide powder removed, placed in a vacuum dessicator to cool to room temperature;

[0062] 对上述氧化得到的三氧化钼粉末进行纯化,具体步骤如下: [0062] The above-mentioned oxide powder was purified molybdenum trioxide, concrete steps are as follows:

[0063] 1)称取121. 41mg三氧化钼粉末置于石英舟内; [0063] 1) weighed 121. 41mg 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 may be placed in a tube furnace temperature, quartz tube port connected with 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 and the temperature was elevated from 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,使三氧化钼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 is 135min, so that molybdenum trioxide 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,三氧化钼粉末在样品石英收集管内自然冷却至室温; [0068] 6) the heating was stopped, the vacuum is maintained inside the quartz tube lOOPa, molybdenum 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钼晶体。 [0069] 7) Turn off the mechanical vacuum pump and tube furnace, remove the quartz sample collection tube from the quartz tube, high purity molybdenum trioxide crystals.

[0070] 纯化后三氧化钼样品纯度分析: [0070] Sample purity after purification trioxide analysis:

[0071] 称量收集管中三氧化钼晶体,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 crystals, the quality of 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钼金属单质粉末以及纯化后制得三氧化钼中杂质的含量。 [0072] content before purification using mass spectrometry analysis of elemental molybdenum metal powder and molybdenum trioxide was obtained after purification of impurities in high resolution inductively coupled plasma. 结果表明,纯化前钼试剂中钼金属单质的质量百分比为99. 89% ;纯化后制得三氧化钼样品中三氧化钼的质量百分比为99. 99%。 The results show that the mass percentage of molybdenum in the reagent before purified elemental molybdenum is 99.89 percent; purified samples obtained trioxide mass percent molybdenum trioxide is 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.纯化前钼粉末原料及纯化后三氧化钼中主要杂质元素的质量百分比(% ) [0074] Table 2. Percentage by mass of molybdenum powder raw material before purification and after purification molybdenum trioxide main impurity elements (%)

Figure CN104003446BD00071

[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、高纯三氧化钼的制备 Preparation of high purity molybdenum trioxide of Example 3 [0078] Example

[0079] 原料为98M〇丰度为98. 15%的浓缩钼同位素(金属单质),钼的质量百分比为99. 89%。 [0079] materials 98M〇 abundance of 98.15% of the isotope molybdenum concentrate (metal element), the mass percentage of molybdenum is 99.89 percent. 称取钼粉末原料380. 8lmg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。 Molybdenum powder material was weighed into a quartz beaker 380. 8lmg, placed in a muffle furnace heated air introduced into the oxidation reaction. 升温过程如下: Heating process is as follows:

[0080] 1)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] 1) 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,以确保钼粉末充分氧化; [0081] 2) 60min and the temperature was elevated from 150 ° C to 580 ° C, the oxidation time was 540min, in order to ensure full oxidation of molybdenum powder;

[0082] 3)停止加热,马弗炉内温度降温至370°C时,打开马弗炉,将装有三氧化钼粉末的烧杯取出,放入真空保干器内冷却至室温; When the [0082] 3) Stop heating muffle furnace temperature was lowered to 370 ° C, open muffle the beaker containing molybdenum trioxide powder removed, placed in a vacuum dessicator to cool to room temperature;

[0083] 对上述氧化得到的三氧化钼粉末进行纯化,具体步骤如下: [0083] The above-mentioned oxide powder was purified molybdenum trioxide, concrete steps are as follows:

[0084] 1)称取139. 04mg三氧化钼粉末置于石英舟内; [0084] 1) weighed 139. 04mg 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 may be placed in a tube furnace temperature, quartz tube port connected with 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lOOPa,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 lOOPa, 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 and the temperature was elevated from 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,使三氧化钼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 is 125min, so that molybdenum trioxide 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,三氧化钼粉末在样品石英收集管内自然冷却至室温; [0089] 6) the heating was stopped, the vacuum is maintained inside the quartz tube lOOPa, molybdenum 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钼晶体。 [0090] 7) Turn off the mechanical vacuum pump and tube furnace, remove the quartz sample collection tube from the quartz tube, high purity molybdenum trioxide crystals.

[0091] 纯化后三氧化钼纯度分析: [0091] After purification of molybdenum trioxide purity analysis:

[0092] 称量收集管中三氧化钼晶体,质量为121. 66mg,计算得到上述方法的回收率为87. 50%〇 [0092] Weighing collection tube trioxide crystals, the quality of 121. 66mg, calculated by the above method of recovery was 87.50% billion

[0093] 采用高分辨电感耦合等离子体质谱仪分析纯化前钼金属单质粉末以及纯化后制得三氧化钼中杂质的含量。 [0093] content before purification using mass spectrometry analysis of elemental molybdenum metal powder and molybdenum trioxide was obtained after purification of impurities in high resolution inductively coupled plasma. 结果表明,纯化前钼试剂中钼金属单质的质量百分比为99. 88% ;纯化后制得三氧化钼样品中三氧化钼的质量百分比为99. 99%。 The results show that the mass percentage of molybdenum in the reagent before purified elemental molybdenum is 99.88 percent; purified samples obtained trioxide mass percent molybdenum trioxide is 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.纯化前钼粉末原料及纯化后三氧化钼中主要杂质元素的质量百分比(% ) [0094] Table 3. Percentage of quality raw material powder before and after purification of molybdenum trioxide purification main impurity elements (%)

Figure CN104003446BD00081

[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
Clasificaciones
Clasificación internacionalC01G39/02
Eventos legales
FechaCódigoEventoDescripción
27 Ago 2014C06Publication
24 Sep 2014C10Request of examination as to substance
17 Jun 2015C14Granted