CN104003446B - Preparation method of high-purity molybdenum trioxide - Google Patents
Preparation method of high-purity molybdenum trioxide Download PDFInfo
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Abstract
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%.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity molybdenum trioxide, belong to high purity metal oxides preparing technical field.
Background technology
At occurring in nature, molybdenum has 7 kinds of stable isotopes, is respectively
92mo,
94mo,
95mo,
96mo,
97mo,
98mo and
100mo.When the oxidation-reduction state of geology and ocean environment changes, the mass fractionation of molybdenum isotope can be caused.Meanwhile, molybdenum element is the important component part of multiple enzyme in plant, animal and human's body.Therefore, the research of setting up molybdenum element content and the isotopic abundance ratio measuring method field such as Geochemistry, geology and biology is over the ground significant.The molybdenum simple substance of usual employing mass percent >=99.99% or molybdenum compound, prepare molybdenum composition or isotopic standard material, thus improve reliability and the accuracy of measuring result.Because High-Purity Molybdenum reagent type commercially available is at present few, expensive, and delivery date is longer, sets up molybdenum element purification process, and the molybdate reagent of preparation purity >=99.99% has important using value.On the other hand, high-purity molybdenum trioxide is a kind of important industrial chemicals, mainly for the production of the compound of High-Purity Molybdenum metal simple-substance and molybdenum, and is used as catalyzer in the oil industry.
Mainly ion exchange method is adopted in document, as: anion and cation exchange resin method, resin method and anion-exchange resin method, to complicated substrate sample as the molybdenum element in soil, serum is separated and enrichment.This class methods complicated operation, needs use two kinds of resins or repetitive operation just can reach the purity requirement of high purity reagent for 2 times usually; Meanwhile, use the chemical reagent such as nitric acid, hydrochloric acid, hydrofluoric acid or ammoniacal liquor in purge process, the impurity element in these chemical reagent easily produces sample and pollutes.
One is disclosed with common molybdenum powder for raw material in patent application " a kind of purification process of molybdenum powder " (publication number is " CN101347839A "); through washing or pickling impurity removal; dry; high-temperature hydrogen protection removal of impurities or vacuum high-temperature removal of impurities, the processes such as vacuum screen separation obtain the method for the molybdenum powder of purifying.The mass percent adopting molybdenum in the molybdenum powder after the method purifying is 99.94% ~ 99.95%.
Industrial main employing two kinds of operational paths carry out purifying to molybdenum trioxide powder (also known as molybdenum calcining), prepare high-purity molybdenum trioxide.One is called wet method: namely soaked through ammonia by molybdenum calcining, and wet purification purifies, and is produced into ammonium paramolybdate, and ammonium paramolybdate, through thermal degradation, removes ammonia, thus obtains high-purity molybdenum trioxide; Another kind is called pyrogenic process, and by molybdenum calcining direct heating, in molybdenum calcining, impurities left is in fired slags, and most of molybdic oxide is through distillation recrystallize, generates high-purity molybdenum trioxide.Because temperature of reaction is comparatively large on the impact of purification effect, the purity of the molybdic oxide obtained after adopting wet method or fire cleaning is in the industrial production general not higher than 99.95%.
Summary of the invention
The object of this invention is to provide a kind of preparation method of high-purity molybdenum trioxide, molybdic oxide purity >=99.99% utilizing present method to prepare.Based on the character that chemical property and the molybdic oxide of molybdenum simple substance easily distil, the present invention takes two-step approach to carry out purifying to the molybdate reagent of ordinary purity.
The preparation method of a kind of high-purity molybdenum trioxide provided by the invention, comprises the steps:
The first step, under air existent condition, molybdenum elemental powders obtains molybdic oxide through oxidizing reaction;
The temperature-rise period of described oxidizing reaction is as follows:
1) temperature is risen to 100 DEG C ~ 200 DEG C, and keep constant temperature;
2) continue to be warming up to 550 DEG C ~ 650 DEG C, carry out described oxidizing reaction.
Second step, carries out purifying to described molybdic oxide:
1) described molybdic oxide is placed in a container closed, and collection tube is set in the above-described container;
2) heat described molybdic oxide region, make temperature rise to 100 ~ 150 DEG C; 10Pa ~ 100Pa is evacuated to described container, and keeps constant temperature and pressure;
3) stop vacuumizing, and make the temperature of described molybdic oxide region rise to 600 DEG C of C ~ 720 DEG C, keep constant temperature;
4) continue to be evacuated to 10Pa ~ 100Pa to described container, and keep constant voltage 120 ~ 150min, namely in described collection tube, collect the molybdic oxide after being elevated purification.
In above-mentioned preparation method, in the temperature-rise period of described the first step oxidizing reaction, step 1) in, in 20 ~ 40min, temperature is risen to 100 DEG C ~ 200 DEG C, specifically can be warming up to 150 DEG C in 30min;
The hold-time of described constant temperature is 30 ~ 60min, specifically can be 30min.
In above-mentioned preparation method, in the temperature-rise period of described the first step oxidizing reaction, step 2) in, in 60 ~ 90min, temperature is risen to 550 DEG C ~ 650 DEG C, specifically can be warming up to 580 DEG C or 600 DEG C in 60min;
The time of described oxidizing reaction is 480 ~ 960min, specifically can be 480min ~ 720min, 480min ~ 540min, 540min ~ 720min, 480min, 540min or 720min.
In above-mentioned preparation method, after described the first step oxidizing reaction terminates, be cooled to 300 DEG C ~ 400 DEG C, specifically can be down to 350 DEG C ~ 400 DEG C, 350 DEG C, 370 DEG C or 400 DEG C.
In above-mentioned preparation method, in the step of described second step purifying, step 2) in, in 20 ~ 40min, temperature is risen to 100 DEG C ~ 150 DEG C, specifically can be warming up in 30min to 150 DEG C;
The hold-time of described constant temperature and pressure is 30 ~ 60min, specifically can be 30min.
In above-mentioned preparation method, in the step of described second step purifying, step 3) in, in 60 ~ 90min, temperature is risen to 600 DEG C ~ 720 DEG C, specifically in 60min, temperature can be risen to 600 DEG C ~ 675 DEG C, 600 DEG C, 625 DEG C or 675 DEG C;
The hold-time of described constant temperature is specially 30 ~ 60min, specifically can be 30min.
In above-mentioned preparation method, in the step of described second step purifying, step 4) in, the hold-time of described constant voltage specifically can be 120min ~ 135min, 125min ~ 135min, 120min, 125min or 135min.
Purity >=99.99% of the molybdic oxide that the inventive method prepares.
The operating process that the present invention prepares high-purity molybdenum trioxide is simple, laboratory purifying can be met or prepare tens milligrams of demands to hundreds of milligram Microamounts of Mo reagent, simultaneously owing to not adding any chemical reagent in purge process, the introducing of impurity can be reduced, the High-Purity Molybdenum reagent of purity >=99.99% after purifying, can be obtained.
Embodiment
The experimental technique used in following embodiment if no special instructions, is ordinary method.
In the following embodiment of the present invention, the rate of recovery of molybdic oxide purification process calculates according to the following equation:
High resolution-inductive coupled plasma mass spectrometry instrument is adopted to analyze the content of impurity in obtained molybdic oxide after molybdenum elemental powders before purifying and purifying in the following embodiment of the present invention.
Concrete test condition is as follows: in the nitric acid of 2% (v/v), configuration concentration is respectively the mixing solutions of the beryllium of 1ng/g, indium and bismuth, carries out optimizing selection to the instrument condition of High resolution-inductive coupled plasma mass spectrometry instrument.The mixture of multi-elements solution reference material (BW3197-BW3200) of 68 kinds of metals, non-metallic element is bought from China National Measuring Science Research Inst..
Concrete testing method is as follows: in the nitric acid of 2% (v/v), above-mentioned mixture of multi-elements solution reference material is diluted to concentration and is respectively 1ng/g, 5ng/g, 10ng/g are as standardized solution.By the content of 67 kinds of impurity in calibration curve method semi-quantitative analysis sample, thus the purity of molybdic oxide after molybdenum elemental powders and purifying before calculating purifying.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
The molybdenum elemental powders raw material particle size used in the following embodiment of the present invention is 100 orders.
The preparation of embodiment 1, high-purity molybdenum trioxide
Raw material is natural abundance molybdenum simple substance, and the mass percent of molybdenum is 99.89%.Take molybdenum powder raw material 605.64mg and be placed in quartz beaker, put into retort furnace heating, pass into air and carry out oxidizing reaction.Temperature-rise period is as follows:
1) open retort furnace, temperature from ambient is warming up to 150 DEG C by 30min, stablizes 30min to remove the moisture and other possible gaseous impuritieies that wherein adsorb;
2) temperature is warming up to 600 DEG C by 150 DEG C by 60min, and oxidization time is 480min, to guarantee that molybdenum powder is fully oxidized;
3) stop heating, in retort furnace during greenhouse cooling to 400 DEG C, open retort furnace, the beaker that molybdenum trioxide powder is housed is taken out, puts into vacuum desiccator and be cooled to room temperature;
Carry out purifying to the molybdenum trioxide powder that above-mentioned oxidation obtains, concrete steps are as follows:
1) taking 116.22mg molybdenum trioxide powder is placed in quartz boat;
2) quartz boat is slowly put into the silica tube that one end is closed, and be pushed to can the heated center region of temperature-controlled tube stove; Quartz specimen collection tube is put into silica tube, and being pushed to can temperature-controlled tube stove heating region outer end; Afterwards, being put into by silica tube can temperature-controlled tube stove, and the silica tube mouth of pipe is connected with oil-sealed rotary pump;
3) open tube furnace, temperature from ambient is warming up to 150 DEG C by 30min, opens oil-sealed rotary pump, is evacuated to 100Pa, stablizes 30min, to remove the moisture and other possible gaseous impuritieies that wherein adsorb;
4) close vacuum pump, temperature is warming up to 625 DEG C by 150 DEG C by 60min, stablizes 30min;
5) open oil-sealed rotary pump, be evacuated to 100Pa, the evaporation purification time is 120min, makes molybdenum trioxide powder start to distil and is deposited in sample collection tube;
6) stop heating, keep vacuum in silica tube to be 100Pa, molybdenum trioxide powder naturally cools to room temperature in sample quartz selection pipe;
7) close oil-sealed rotary pump and tube furnace, in silica tube, take out quartz specimen collection tube, obtain highly purified molybdic oxide crystal.
Molybdic oxide purity check after purifying:
Weigh molybdic oxide crystal in collection tube, quality is 102.59mg, and the rate of recovery calculating the molybdic oxide utilizing aforesaid method to prepare is 88.27%.
High resolution-inductive coupled plasma mass spectrometry instrument is adopted to analyze the content of impurity in obtained molybdic oxide after molybdenum elemental powders before purifying and purifying.Result shows, before purifying, in molybdate reagent, the mass percent of molybdenum simple substance is 99.89%; After purifying, in obtained molybdic oxide sample, the mass percent of molybdic oxide is 99.99%.
Wherein the content of major impurity element is as shown in table 1:
The mass percent (%) of major impurity element in molybdic oxide after molybdenum powder raw material and purifying before table 1. purifying
a"--" represents that the content of this element under described experiment condition is lower than detectability
The preparation of embodiment 2, high-purity molybdenum trioxide
Raw material is natural abundance molybdenum simple substance, and the mass percent of molybdenum is 99.89%.Take molybdenum powder raw material 939.93 mg and be placed in quartz beaker, put into retort furnace heating, pass into air and carry out oxidizing reaction.Temperature-rise period is as follows:
1) open retort furnace, temperature from ambient is warming up to 150 DEG C by 30min, stablizes 30min to remove the moisture and other possible gaseous impuritieies that wherein adsorb;
2) temperature is warming up to 600 DEG C by 150 DEG C by 60min, and oxidization time is 720min, to guarantee that molybdenum powder is fully oxidized;
3) stop heating, in retort furnace during greenhouse cooling to 350 DEG C, open retort furnace, the beaker that molybdenum trioxide powder is housed is taken out, puts into vacuum desiccator and be cooled to room temperature;
Carry out purifying to the molybdenum trioxide powder that above-mentioned oxidation obtains, concrete steps are as follows:
1) taking 121.41mg molybdenum trioxide powder is placed in quartz boat;
2) quartz boat is slowly put into the silica tube that one end is closed, and be pushed to can the heated center region of temperature-controlled tube stove; Quartz specimen collection tube is put into silica tube, and being pushed to can temperature-controlled tube stove heating region outer end; Afterwards, being put into by silica tube can temperature-controlled tube stove, and the silica tube mouth of pipe is connected with oil-sealed rotary pump;
3) open tube furnace, temperature from ambient is warming up to 150 DEG C by 30min, opens oil-sealed rotary pump, is evacuated to 100Pa, stablizes 30min, to remove the moisture and other possible gaseous impuritieies that wherein adsorb;
4) close vacuum pump, temperature is warming up to 600 DEG C by 150 DEG C by 60min, stablizes 30min;
5) open oil-sealed rotary pump, be evacuated to 100Pa, the evaporation purification time is 135min, makes molybdenum trioxide powder start to distil and is deposited in sample collection tube;
6) stop heating, keep vacuum in silica tube to be 100Pa, molybdenum trioxide powder naturally cools to room temperature in sample quartz selection pipe;
7) close oil-sealed rotary pump and tube furnace, in silica tube, take out quartz specimen collection tube, obtain highly purified molybdic oxide crystal.
After purifying, molybdic oxide sample purity is analyzed:
Weigh molybdic oxide crystal in collection tube, quality is 104.98mg, and the rate of recovery calculating aforesaid method is 86.47%.
High resolution-inductive coupled plasma mass spectrometry instrument is adopted to analyze the content of impurity in obtained molybdic oxide after molybdenum elemental powders before purifying and purifying.Result shows, before purifying, in molybdate reagent, the mass percent of molybdenum simple substance is 99.89%; After purifying, in obtained molybdic oxide sample, the mass percent of molybdic oxide is 99.99%.
Wherein the content of major impurity element is as shown in table 2:
The mass percent (%) of major impurity element in molybdic oxide after molybdenum powder raw material and purifying before table 2. purifying
a"--" represents that the content of this element under described experiment condition is lower than detectability
The preparation of embodiment 3, high-purity molybdenum trioxide
Raw material is
98mo abundance is the concentrated molybdenum isotope (metal simple-substance) of 98.15%, and the mass percent of molybdenum is 99.89%.Take molybdenum powder raw material 380.81mg and be placed in quartz beaker, put into retort furnace heating, pass into air and carry out oxidizing reaction.Temperature-rise period is as follows:
1) open retort furnace, temperature from ambient is warming up to 150 DEG C by 30min, stablizes 30min to remove the moisture and other possible gaseous impuritieies that wherein adsorb;
2) temperature is warming up to 580 DEG C by 150 DEG C by 60min, and oxidization time is 540min, to guarantee that molybdenum powder is fully oxidized;
3) stop heating, in retort furnace during greenhouse cooling to 370 DEG C, open retort furnace, the beaker that molybdenum trioxide powder is housed is taken out, puts into vacuum desiccator and be cooled to room temperature;
Carry out purifying to the molybdenum trioxide powder that above-mentioned oxidation obtains, concrete steps are as follows:
1) taking 139.04mg molybdenum trioxide powder is placed in quartz boat;
2) quartz boat is slowly put into the silica tube that one end is closed, and be pushed to can the heated center region of temperature-controlled tube stove; Quartz specimen collection tube is put into silica tube, and being pushed to can temperature-controlled tube stove heating region outer end; Afterwards, being put into by silica tube can temperature-controlled tube stove, and the silica tube mouth of pipe is connected with oil-sealed rotary pump;
3) open tube furnace, temperature from ambient is warming up to 150 DEG C by 30min, opens oil-sealed rotary pump, is evacuated to 100Pa, stablizes 30min, to remove the moisture and other possible gaseous impuritieies that wherein adsorb;
4) close vacuum pump, temperature is warming up to 675 DEG C by 150 DEG C by 60min, stablizes 30min;
5) open oil-sealed rotary pump, be evacuated to 100Pa, the evaporation purification time is 125min, makes molybdenum trioxide powder start to distil and is deposited in sample collection tube;
6) stop heating, keep vacuum in silica tube to be 100Pa, molybdenum trioxide powder naturally cools to room temperature in sample quartz selection pipe;
7) close oil-sealed rotary pump and tube furnace, in silica tube, take out quartz specimen collection tube, obtain highly purified molybdic oxide crystal.
Molybdic oxide purity check after purifying:
Weigh molybdic oxide crystal in collection tube, quality is 121.66mg, and the rate of recovery calculating aforesaid method is 87.50%.
High resolution-inductive coupled plasma mass spectrometry instrument is adopted to analyze the content of impurity in obtained molybdic oxide after molybdenum elemental powders before purifying and purifying.Result shows, before purifying, in molybdate reagent, the mass percent of molybdenum simple substance is 99.88%; After purifying, in obtained molybdic oxide sample, the mass percent of molybdic oxide is 99.99%.Wherein the content of major impurity element is as shown in table 3:
The mass percent (%) of major impurity element in molybdic oxide after molybdenum powder raw material and purifying before table 3. purifying
a"--" represents that the content of this element under described experiment condition is lower than detectability.
Claims (5)
1. a preparation method for high-purity molybdenum trioxide, is characterized in that, comprises the steps:
Under air existent condition, molybdenum elemental powders obtains molybdic oxide through oxidizing reaction;
The temperature-rise period of described oxidizing reaction is as follows:
1) temperature is risen to 100 DEG C ~ 200 DEG C, and keep constant temperature;
2) continue to be warming up to 550 DEG C ~ 650 DEG C, carry out described oxidizing reaction;
Described method also comprises the step of described molybdic oxide being carried out to purifying:
1) described molybdic oxide is placed in a container closed, and collection tube is set in the above-described container;
2) heat described molybdic oxide region, make temperature rise to 100 ~ 150 DEG C; 10 ~ 100Pa is evacuated to described container, and keeps constant temperature and pressure;
3) stop vacuumizing, and make the temperature of described molybdic oxide region rise to 600 DEG C ~ 720 DEG C, and keep constant temperature;
4) continue to be evacuated to 10 ~ 100Pa to described container, and keep constant voltage 120 ~ 150min, namely in described collection tube, collect the molybdic oxide after being elevated purification.
2. preparation method according to claim 1, is characterized in that: in the temperature-rise period of described oxidizing reaction, step 1) in, in 20 ~ 40min, temperature is risen to 100 DEG C ~ 200 DEG C;
The time of described constant temperature is 30 ~ 60min.
3. preparation method according to claim 1 and 2, is characterized in that: in the temperature-rise period of described oxidizing reaction, step 2) in, in 60 ~ 90min, temperature is risen to 550 DEG C ~ 650 DEG C;
The time of described oxidizing reaction is 480 ~ 960min.
4. preparation method according to claim 1 and 2, is characterized in that: in the step of described purifying, step 2) in, in 20 ~ 40min, temperature is risen to 100 DEG C ~ 150 DEG C;
The hold-time of described constant temperature and pressure is 30 ~ 60min.
5. preparation method according to claim 1 and 2, is characterized in that: in the step of described purifying, step 3) in, in 60 ~ 90min, temperature is risen to 600 DEG C ~ 720 DEG C;
The hold-time of described constant temperature is 120 ~ 150min.
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