CN104310323B - The preparation method of a kind of low nitrogen tantalum oxide and the low nitrogen tantalum oxide of preparation thereof - Google Patents
The preparation method of a kind of low nitrogen tantalum oxide and the low nitrogen tantalum oxide of preparation thereof Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of low nitrogen tantalum oxide, in addition to including neutralization precipitation, adjusting eccysis fluorine, drying and calcining step, adjusting between eccysis ammonia step and baking step, also including adjusting eccysis ammonia.Concrete operations are: the tantalum hydroxide after toning eccysis fluorine is adjusted with 75 ~ 85 DEG C of pure water and is washed till nitrogen content≤0.10g/L.Described preparation method is being adjusted between eccysis ammonia step and baking step, also includes distillation: is placed in distillation container through the tantalum hydroxide of toning eccysis ammonia, is passed through steam, distills 3 ~ 6 hours under pressure 0.1 ~ 0.5MPa.Additionally, drying and calcining step are also optimized and improve by the present invention.The present invention also provides for a kind of low nitrogen tantalum oxide, described low nitrogen tantalum oxide nitrogen content≤60ppm, is prepared by above-mentioned preparation method.
Description
Technical field
This law is bright belongs to metallochemistry field of smelting, is specifically related to the preparation method of a kind of low nitrogen tantalum oxide, and the low nitrogen tantalum oxide that the method prepares.
Background technology
Tantalum oxide is applied to the industrial circles such as electronics, iron and steel, machinery, aviation widely.Owing to tantalum-oxide film layer has high index of refraction, high-k, so it is also the important materials manufacturing thin film capacitor.The film layers such as anti-reflection film that tantalum oxide and silica composition are coated with, reflectance coating, interferometric filter are firm, and chemical stability is good, and resisting laser damage ability is strong.It addition, tantalum oxide has high transmitance and reflectance in visible and near infrared region, it is applied on the components and parts such as laser instrument, solaode.
The preparation of tantalum oxide, general method includes: add Fluohydric acid. in the raw material containing tantalum and sulphuric acid obtains fluorotantalic acid solution, sec-octyl alcohol is utilized to be extracted by tantalum, remove other metal impurities such as ferrum, manganese, then after adding the precipitate that ammonia obtains tantalum hydroxide, carry out adjusting eccysis fluorine to tantalum hydroxide with the pure water containing ammonia, finally it be dried and calcine.
Owing to employing ammonia in preparation process, final products tantalum oxide can inevitably there is nitrogen to remain.And nitrogen content is too high, tantalum oxide plated film material and sputtering target material can be caused to become fragile, easy shattered crack.Along with hitech materials performance requirement is improved day by day, it is desirable in tantalum oxide, the content of nitrogen is more and more lower.But in industry standard YS/T547-2007 of existing high purity tantalum oxide, it is not specified by nitrogen content.In practice, in current tantalum oxide main market players product, nitrogen content is general all at about 2000ppm.And about the report of tantalum oxide preparation method in prior art, be concentrated mainly on Oil repellent in reduction product, improve product stability, the most still without reference to effective solution reducing nitrogen content.Such as 28 days October 2009 publication number CN101565207A(publication date) Chinese invention patent application " preparation method of the high-purity tantalum pentoxide of low fluorine ", essentially disclose the process conditions of calcining step last in high purity tantalum oxide preparation process, i.e. calcine according to following program segmenting: 180-230 DEG C is incubated 2-3 hour, 480-530 DEG C is incubated 4-6 hour, 620-680 DEG C is incubated 2-3 hour, 790-840 DEG C is incubated 3-5 hour, comes out of the stove after then cooling to 180-230 DEG C.The method mainly solves the tradition homogeneity of product that once intensification calcining causes, lack of homogeneity, and Oil repellent is high, and the problem of burner hearth easy-sintering.April 28 2004 publication number CN1492838A(publication date) application for a patent for invention " tantalum oxide or niobium oxide powder and preparation method thereof ", also the improvement to calcination process is only disclosed, by fully providing oxygen to roasting product when calcining, improve tantalum oxide or the stability of niobium oxide.
Therefore, it is necessary to the preparation method of tantalum oxide is improved, thus reduce the content of wherein nitrogen.
Summary of the invention
For above-mentioned technical problem, the present invention provides the preparation method of a kind of low nitrogen tantalum oxide.The method is by improving technique, and the tantalum oxide prepared, nitrogen content is minimum can be controlled at below 60ppm, and relatively prior art have dropped more than 30 times.
In order to realize foregoing invention purpose, present invention employs following technical scheme:
The preparation method of a kind of low nitrogen tantalum oxide, including neutralization precipitation, tune eccysis fluorine, dries and calcines.
Preferably, the preparation method of a kind of low nitrogen tantalum oxide, adjusting between eccysis ammonia step and baking step, also including adjusting eccysis ammonia；Wherein, the concrete operations of described tune eccysis ammonia step are: the tantalum hydroxide after toning eccysis fluorine is adjusted with 75 ~ 85 DEG C of pure water and is washed till nitrogen content≤0.10g/L.
Preferably, the preparation method of above-mentioned low nitrogen tantalum oxide, adjusting between eccysis ammonia step and baking step, also including distillation；The concrete operations of described distilation steps are: in the tantalum hydroxide of toning eccysis ammonia is placed in distillation container, be passed through steam, distill 3 ~ 6 hours under pressure 0.1 ~ 0.5MPa.
In above-mentioned preparation method, the concrete operations of described baking step are: the tantalum hydroxide distilled is placed in microwave drying oven, add water abundant moistening tantalum hydroxide, dry to being gently twisted powder with hands, cross 30 mesh sieves for 60 ~ 85 DEG C.
As one preferred embodiment, the present invention provides the preparation method of a kind of low nitrogen tantalum oxide, including neutralization precipitation, tune eccysis fluorine, tune eccysis ammonia, distills, dries and calcines；Wherein, after neutralization precipitation and tune eccysis fluorine, tantalum hydroxide is adjusted with 75 ~ 85 DEG C of pure water and is washed till nitrogen content≤0.10g/L, is subsequently placed in distillation container, is passed through steam, distills 3 ~ 6 hours under pressure 0.1 ~ 0.5MPa.
As a preferred embodiment, the present invention provides the preparation method of a kind of low nitrogen tantalum oxide, including neutralization precipitation, tune eccysis fluorine, tune eccysis ammonia, distills, dries and calcines；Wherein, after neutralization precipitation and tune eccysis fluorine, tantalum hydroxide is adjusted with 75 ~ 85 DEG C of pure water and is washed till nitrogen content≤0.10g/L, it is subsequently placed in distillation container, is passed through steam, distill 3 ~ 6 hours under pressure 0.1 ~ 0.5MPa, the tantalum hydroxide distilled is placed in microwave drying oven, add water abundant moistening tantalum hydroxide, dry to being gently twisted powder with hands, cross 30 mesh sieves for 60 ~ 85 DEG C.
In above-mentioned preparation method, it is preferred that described neutralization precipitation step is carried out in neutralization chamber, puts into tantalum liquid, makes every 1m3Neutralization chamber inner oxide total amount is with Ta2O5It is calculated as 70 ~ 100Kg, acidity 0.2～1.0N, then is neutralized with liquefied ammonia and is precipitated to pH9.0 ~ 10.0.
In above-mentioned preparation method, it is also preferred that in described tune eccysis fluorine step, tantalum hydroxide with 65 ~ 75 DEG C, concentration be that the ammonia spirit of 3 ~ 4M is adjusted and is washed till Oil repellent≤0.15g/L.
In above-mentioned preparation method, it is also preferred that in described calcining step, calcining heat is 1000 ~ 1200 DEG C, calcination time is 8 ~ 10 hours.
As one preferred embodiment, the present invention provides the preparation method of a kind of low nitrogen tantalum oxide, including neutralization precipitation, tune eccysis fluorine, tune eccysis ammonia, distills, dries and calcines；Concrete operations are:
1) neutralization precipitation:
Tantalum liquid is put in the neutralization precipitation groove of volume 1000L, put into tantalum liquid, make every 1m3Neutralization chamber inner oxide total amount is with Ta2O5Being calculated as 70 ~ 100Kg, acidity 0.2～1.0N, be then sufficiently stirred for 10 minutes, slowly open ammonia valve and add liquefied ammonia, neutralization precipitation, to pH=9.0 ~ 10.0, obtains tantalum hydroxide slip；
2) eccysis fluorine is adjusted
Neutralization precipitation step is obtained tantalum hydroxide slip press-in pressure filter, squeezing dries up, with 65 ~ 75 DEG C, concentration be 3 ~ 4M ammonia spirit tune be washed till Oil repellent≤0.15g/L, squeezing dries up, and obtains tantalum hydroxide；
3) eccysis ammonia is adjusted
Being adjusted with the pure water of 75 ~ 85 DEG C by the described tantalum hydroxide adjusting eccysis fluorine step to obtain and be washed till nitrogen content≤0.10g/L, squeezing dries up, discharging, obtains low ammonia tantalum hydroxide；
4) distillation
The described low ammonia tantalum hydroxide adjusting eccysis ammonia step to obtain is placed in distillation container, is passed through steam, distill 3 ~ 6 hours under pressure 0.1 ~ 0.5MPa, cooling discharging, obtain the tantalum hydroxide distilled；
5) dry
The tantalum hydroxide that the described distillation that upper step obtained is good is contained in drying charging tray, adds water abundant moistening tantalum hydroxide, dries to being gently twisted powder with hands, cross 30 mesh sieves for 60 ~ 85 DEG C；
6) calcining
The tantalum hydroxide that the drying that upper step obtains is sieved being delivered to push away boat stove calcine, temperature controls to calcine 8 ~ 10 hours at 1000～1200 DEG C；60 mesh sieves are crossed after cooling.
A kind of low nitrogen tantalum oxide of offer, described low nitrogen tantalum oxide nitrogen content≤60ppm are provided, are prepared by above-mentioned preparation method.
Tantalum liquid of the present invention, refers to fluorotantalic acid solution, or the fluorotantalic acid solution that purity improves after sec-octyl alcohol extraction-pure water back extraction.
In the preparation method of low nitrogen tantalum oxide of the present invention, the water arrived, all referring to the pure water through purified treatment.Therefore adjust the ammonia spirit in eccysis fluorine step, be i.e. the solution that obtains in pure water of liquid ammonia solution.
The present invention well solves the problem that in tantalum oxide, nitrogen content exceeds standard.In existing tantalum oxide production technology, owing in tantalum hydroxide slip, Oil repellent is higher, and ammonia and the good network of fluorine and property, and the good water solubility of ammonia own, volatility is high, therefore takes containing the hot pure water of ammonia to adjust eccysis fluorine.Theoretically, during adjusting eccysis fluorine, ammonia can separate with tantalum hydroxide easily.But proved is undesirable.Finding through detection, conventionally produced tantalum oxide, even meeting the high purity tantalum oxide of the highest trade mark requirement in industry standard YS/T547-2007, wherein the content of nitrogen is also up to 2000ppm.The present invention uses pure water to adjust eccysis ammonia, is found to effectively reduce the content of nitrogen in product.On the other hand, adjust the tantalum hydroxide steam washed out to distill 3 ~ 6 hours under the pressure of 0.1 ~ 0.5MPa, allow free ammonia fully volatilize.Then add water in drying course, make ammonia be transformed into polar molecule, dry in microwave drying box, further reduce the nitrogen in tantalum hydroxide.Drying sieve after the high-temperature calcination of 1000 ~ 1200 DEG C, contribute to making ammonia volatilize further, thus reduce the content of nitrogen.Through said process, the nitrogen content≤60ppm of last tantalum oxide product, thus fully meet the needs of client.
Detailed description of the invention
Below by specific embodiment, the present invention is elaborated.It will be appreciated by those skilled in the art that these embodiments are merely to illustrate the present invention, it limits the scope of the present invention never in any form.
Experimental technique in following embodiment, if no special instructions, is conventional method.Various fibrous materials used in following embodiment, if no special instructions, are commercially available purchase product.
Embodiment 1 The preparation of low nitrogen tantalum oxide
Concentration known is with Ta2O5Being calculated as the tantalum liquid of 100g/L, acidity is 0.7N；Low nitrogen tantalum oxide is prepared through following steps:
1, neutralization precipitation
The volume of neutralization chamber is 1000L；According to technological requirement, controlling every groove oxide aggregate is 85Kg.Then by calculating, tantalum liquid need to be added and amass as 85000g ÷ 100g/L=850L.Described in 850L, tantalum liquid puts into neutralization chamber.After being sufficiently stirred for 10 minutes, slowly opening ammonia valve and add liquefied ammonia, neutralization precipitation is to pH=9.0 ~ 10.0.
2) eccysis fluorine is adjusted
Tantalum hydroxide slip press-in pressure filter neutralization precipitation step obtained, squeezing dries up, and adjusts with the ammonia spirit of 65 DEG C, molar concentration 3M and is washed till Oil repellent≤0.15g/L, and squeezing dries up, and obtains tantalum hydroxide；
3) eccysis ammonia is adjusted
Being adjusted with 75 DEG C of pure water by the described tantalum hydroxide adjusting eccysis fluorine step to obtain and be washed till nitrogen content≤0.10g/L, squeezing dries up, discharging, obtains low ammonia tantalum hydroxide；
4) distillation
The described low ammonia tantalum hydroxide adjusting eccysis ammonia step to obtain is placed in distillation container, hermetic container, is passed through steam, distills 3 hours under pressure 0.1 ~ 0.5MPa, cooling discharging, obtain the tantalum hydroxide distilled；
5) dry
The tantalum hydroxide that the described distillation that upper step obtained is good is contained in drying charging tray, adds suitable quantity of water, makes water abundant moistening tantalum hydroxide, loads microwave drying box the most from top to bottom, dries to being gently twisted powder with hands, cross 30 mesh sieves for 60 ~ 70 DEG C；
6) calcining
The tantalum hydroxide that the drying that upper step obtains is sieved being delivered to push away boat stove calcine, temperature controls to calcine 10 hours at 1000 ~ 1100 DEG C；60 mesh sieves are crossed after cooling.
7) after sample analysis is qualified, packaging warehouse-in.
Detecting through oxygen nitrogen hydrogen combined measuring instrument, nitrogen (N) content is 32ppm, tantalum oxide (Ta2O5) content is 99.99%.
Embodiment 2 The preparation of low nitrogen tantalum oxide
Concentration known is with Ta2O5Being calculated as the tantalum liquid of 110g/L, acidity is 0.6N；Low nitrogen tantalum oxide is prepared through following steps:
1, neutralization precipitation
The volume of neutralization chamber is 1000L；According to technological requirement, controlling every groove oxide aggregate is 70Kg.Then by calculating, tantalum liquid need to be added and amass as 70000g ÷ 110g/L ≈ 636L.Described in 636L, tantalum liquid puts into neutralization chamber.After being sufficiently stirred for 10 minutes, slowly opening ammonia valve and add liquefied ammonia, neutralization precipitation is to pH=9.0 ~ 10.0.
2) eccysis fluorine is adjusted
Tantalum hydroxide slip press-in pressure filter neutralization precipitation step obtained, squeezing dries up, and adjusts with the ammonia spirit of 70 DEG C, molar concentration 4M and is washed till Oil repellent≤0.15g/L, and squeezing dries up, and obtains tantalum hydroxide；
3) eccysis ammonia is adjusted
Being adjusted with 85 DEG C of pure water by the described tantalum hydroxide adjusting eccysis fluorine step to obtain and be washed till nitrogen content≤0.10g/L, squeezing dries up, discharging, obtains low ammonia tantalum hydroxide；
4) distillation
The described low ammonia tantalum hydroxide adjusting eccysis ammonia step to obtain is placed in distillation container, hermetic container, is passed through steam, distills 6 hours under pressure 0.1 ~ 0.5MPa, cooling discharging, obtain the tantalum hydroxide distilled；
5) dry
The tantalum hydroxide that the described distillation that upper step obtained is good is contained in drying charging tray, adds suitable quantity of water, makes water abundant moistening tantalum hydroxide, loads microwave drying box the most from top to bottom, dries to being gently twisted powder with hands, cross 30 mesh sieves for 75 ~ 85 DEG C；
6) calcining
The tantalum hydroxide that the drying that upper step obtains is sieved being delivered to push away boat stove calcine, temperature controls to calcine 8 hours at 1100 ~ 1200 DEG C；60 mesh sieves are crossed after cooling
7) after sample analysis is qualified, packaging warehouse-in.
Detecting through oxygen nitrogen hydrogen combined measuring instrument, nitrogen (N) content is 55ppm, tantalum oxide (Ta2O5) content is 99.99%.
Embodiment 3 The preparation of low nitrogen tantalum oxide
Concentration known is with Ta2O5Being calculated as the tantalum liquid of 100g/L, acidity is 0.7N；Tantalum oxide is prepared through following steps:
1, neutralization precipitation
The volume of neutralization chamber is 1000L；According to technological requirement, controlling every groove oxide aggregate is 100Kg.Then by calculating, tantalum liquid need to be added and amass as 10000g ÷ 100g/L=1000L.Described in 1000L, tantalum liquid puts into neutralization chamber.After being sufficiently stirred for 10 minutes, slowly opening ammonia valve and add liquefied ammonia, neutralization precipitation is to pH=9.0 ~ 10.0.
2) eccysis fluorine is adjusted
Neutralization precipitation step is obtained tantalum hydroxide slip press-in pressure filter, squeezing dries up, with 75 DEG C, molar concentration be 3.5M ammonia spirit tune be washed till Oil repellent≤0.15g/L, squeezing dries up, and obtains tantalum hydroxide；
3) eccysis ammonia is adjusted
Being adjusted with 80 DEG C of pure water by the described tantalum hydroxide adjusting eccysis fluorine step to obtain and be washed till nitrogen content≤0.10g/L, squeezing dries up, discharging, obtains low ammonia tantalum hydroxide；
4) distillation
The described low ammonia tantalum hydroxide adjusting eccysis ammonia step to obtain is placed in distillation container, is passed through steam, distill 4.5 hours under pressure 0.1 ~ 0.5MPa, cooling discharging, obtain the tantalum hydroxide distilled；
5) dry
The tantalum hydroxide that the squeezing that upper step obtains dries up is contained in drying charging tray, adds suitable quantity of water, make water abundant moistening tantalum hydroxide, load microwave drying box the most from top to bottom, dry to being gently twisted powder with hands, cross 30 mesh sieves for 70 ~ 75 DEG C；
6) calcining
The tantalum hydroxide that the drying that upper step obtains is sieved being delivered to push away boat stove calcine, temperature controls to calcine 9 hours at 1150 ~ 1200 DEG C；60 mesh sieves are crossed after cooling.
After testing, nitrogen (N) content is 52ppm, tantalum oxide (Ta2O5) content is 99.99%.
Comparative example The preparation of tantalum oxide
Concentration known is with Ta2O5Being calculated as the tantalum liquid of 100g/L, acidity is 0.7N；Tantalum oxide is prepared through following steps:
1, neutralization precipitation
The volume of neutralization chamber is 1000L；According to technological requirement, controlling every groove oxide aggregate is 85Kg.Then by calculating, tantalum liquid need to be added and amass as 85000g ÷ 100g/L=850L.Described in 1000L, tantalum liquid puts into neutralization chamber.After being sufficiently stirred for 10 minutes, slowly opening ammonia valve and add liquefied ammonia, neutralization precipitation is to pH=9.0 ~ 10.0.
2) eccysis fluorine is adjusted
Neutralization precipitation step is obtained tantalum hydroxide slip press-in pressure filter, squeezing dries up, with 75 DEG C, molar concentration be 3M ammonia spirit tune be washed till Oil repellent≤0.15g/L, squeezing dries up, and obtains tantalum hydroxide；
3) dry
The tantalum hydroxide that the squeezing that upper step obtains dries up is contained in drying charging tray, loads microwave drying box from top to bottom, dry to being gently twisted powder with hands, cross 30 mesh sieves for 60 ~ 70 DEG C；
4) calcining
The tantalum hydroxide that the drying that upper step obtains is sieved being delivered to push away boat stove calcine, temperature controls to calcine 10 hours at 1000 ~ 1100 DEG C；60 mesh sieves are crossed after cooling.
After testing, nitrogen (N) content is 980ppm, tantalum oxide (Ta2O5) content is 99.99%.
Specific description of embodiments of the present invention above is not limiting as the present invention, and those skilled in the art can make various change or deformation according to the present invention, without departing from the spirit of the present invention, all should belong to scope of the following claims of the present invention.
Claims (4)
1. a preparation method for low nitrogen tantalum oxide, including neutralization precipitation, tune eccysis fluorine, dries and calcines；It is characterized in that,
Described neutralization precipitation step is carried out in neutralization chamber, puts into tantalum liquid, makes every 1m3Neutralization chamber inner oxide total amount is with Ta2O5It is calculated as
70～100Kg, acidity 0.2～1.0N, then be neutralized with liquefied ammonia and be precipitated to pH9.0～10.0；Through neutralization precipitation and tune eccysis fluorine
After, tantalum hydroxide is adjusted with 75～85 DEG C of pure water and is washed till nitrogen content≤0.10g/L, is subsequently placed in distillation container, is passed through steam,
Distilling 3～6 hours under pressure 0.1～0.5MPa, the tantalum hydroxide distilled is placed in microwave drying oven, adds water abundant moistening hydrogen
Tantalum oxide, dries to being gently twisted powder with hands, crosses 30 mesh sieves for 60～85 DEG C；In described calcining step, calcining heat is 1000～1200 DEG C,
Calcination time is 8～10 hours.
Preparation method the most according to claim 1, it is characterised in that: in described tune eccysis fluorine step, tantalum hydroxide is used
65～75 DEG C, concentration be 3～4M ammonia spirit adjust be washed till Oil repellent≤0.15g/L.
3. a preparation method for low nitrogen tantalum oxide, including neutralization precipitation, tune eccysis fluorine, tune eccysis ammonia, distills, dries and forges
Burn；Concrete operations are:
1) neutralization precipitation:
Tantalum liquid is put in the neutralization precipitation groove of volume 1000L, make every 1m3Neutralization chamber inner oxide total amount is with Ta2O5It is calculated as
70～100Kg, acidity 0.2～1.0N, then it is sufficiently stirred for 10 minutes, slowly opens ammonia valve and add liquefied ammonia, neutralization precipitation is extremely
PH=9.0～10.0, obtains tantalum hydroxide slip；
2) eccysis fluorine is adjusted
Neutralization precipitation step is obtained tantalum hydroxide slip press-in pressure filter, squeezing dries up, with 65～75 DEG C, concentration be 3～4M
Ammonia spirit adjust be washed till Oil repellent≤0.15g/L, squeezing dries up, and obtains tantalum hydroxide；
3) eccysis ammonia is adjusted
Being adjusted with the pure water of 75～85 DEG C by the described tantalum hydroxide adjusting eccysis fluorine step to obtain and be washed till nitrogen content≤0.10g/L, squeezing is blown
Dry, discharging, obtain low ammonia tantalum hydroxide；
4) distillation
The described low ammonia tantalum hydroxide adjusting eccysis ammonia step to obtain is placed in distillation container, is passed through steam, at pressure 0.1～0.5MPa
Lower distillation 3～6 hours, cooling discharging, obtain the tantalum hydroxide distilled；
5) dry
The tantalum hydroxide that the described distillation that upper step obtained is good is contained in drying charging tray, adds water abundant moistening tantalum hydroxide, 60～85 DEG C
Dry to being gently twisted powder with hands, cross 30 mesh sieves；
6) calcining
The tantalum hydroxide that the drying that upper step obtains is sieved being delivered to push away boat stove calcine, temperature controls to forge at 1000～1200 DEG C
Burn 8～10 hours；60 mesh sieves are crossed after cooling.
4. a low nitrogen tantalum oxide, it is characterised in that: the nitrogen content≤60ppm of described low nitrogen tantalum oxide, by claim 1
Prepare to the preparation method according to any one of 3.
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| 废钽回收制取高纯高活性氧化钽;李启厚等;《江西有色金属》;19970930;第11卷(第3期);图1 * |
| 溶剂浸取法制备低氟高纯氧化钽研究;蒋柏泉等;《南昌大学学报》;20080630;第30卷(第2期);第120-122页 * |
| 高纯氧化钽的研制;胡益清;《稀有金属与硬质合金》;19940331(第116期);第9-13页 * |
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Effective date of registration: 20181112 Address after: 332014 Research Institute, No. nine Lake Road, lien Xi District, Jiujiang, Jiangxi, 62 Patentee after: Jiujiang Nonferrous Metal Smelting Co., Ltd. Address before: 332014 No. nine Lake Road, Lian Xi District, Jiujiang, Jiangxi. 62 Patentee before: Jiujiang nonferrous metals smelting Limited by Share Ltd |
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