CN101565207B - Producing method of low-fluorine high-purity tantalic oxide - Google Patents
Producing method of low-fluorine high-purity tantalic oxide Download PDFInfo
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- CN101565207B CN101565207B CN2009100398747A CN200910039874A CN101565207B CN 101565207 B CN101565207 B CN 101565207B CN 2009100398747 A CN2009100398747 A CN 2009100398747A CN 200910039874 A CN200910039874 A CN 200910039874A CN 101565207 B CN101565207 B CN 101565207B
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Abstract
The invention provides a preparation method of low-fluorine high-purity tantalic oxide, which comprises the following steps: preparing high-purity tantalic liquid from impure tantalic liquid materialsby adopting a liquid-liquid extraction method; neutralizing the high-purity tantalic liquid by purified ammonia to obtain high-purity tantalum hydroxide which is then washed, filtered, dried; section ally calcining the high-purity tantalum hydroxide according to the following steps: heating to 180-230 DEG C, and carrying out heat preservation for 2-3 hours; heating to 480-530 DEG C, and carrying out heat preservation for 4-6 hours; heating to 620-680 DEG C, and carrying out heat preservation for 2-3 hours; heating to 790-840 DEG C, and carrying out heat preservation for 3-5 hours; reducing temperature to 180-230 DEG C, and then discharging the high-purity tantalum hydroxide from a furnace and screening to obtain the high-purity tantalic oxide. The invention has the advantages that the prepared high-purity tantalic oxide product has good consistency and evenness, low fluorine content, less ignition loss and protection function to a furnace hearth, and the service life of a roasting hearth can be prolonged.
Description
Technical field
The present invention relates to a kind of preparation method of tantalum metal oxide, specifically, relate to the preparation method of high-purity tantalum pentoxide.
Background technology
At present, traditional high-purity tantalum pentoxide is to produce with the tantalum liquid in the liquid-liquid extraction isolating tantalum niobium process, earlier tantalum liquid is squeezed into the neutralization precipitation groove, under agitation feeds NH
3Gas makes pH value of solution=8-9, generates Ta (OH)
5Precipitation is passed through pressure filter or vacuum filtration with it then.Then tantalum hydroxide is reentered in the decomposer, adds hydrofluoric acid and sulfuric acid dissolution, carry out reextraction with organism and obtain High-purity Tantalum liquid, High-purity Tantalum liquid is with obtaining the High Purity Hydrogen tantalum oxide through the ammoniacal liquor neutralization that purifies.The High Purity Hydrogen tantalum oxide is calcined in retort furnace, cools off, is sieved, and obtains high-purity tantalum pentoxide product.Generating high-purity tantalum pentoxide with the method for calcinating that once heats up, promptly is that the tantalum hydroxide after the oven dry is packed in the calcining furnace, is warmed up to 800 ℃ of insulations after 8 hours, and cooling is come out of the stove, and is high-purity tantalum pentoxide.
Tradition calcination method shortcoming: 1, because heat-up rate is too fast, cause non-uniform temperature in the stove, the homogeneity of product of producing is not so good; 2, fluorine content is too high; 3, because local temperature is too high, the stove silk easily blows, the burner hearth easy-sintering.
Summary of the invention
The objective of the invention is at above-mentioned prior art problems, propose a kind of new process that uses the branch section calcining to produce the low high-purity tantalum pentoxide of fluorine, prepare the existing drawback of high-purity tantalum pentoxide so that overcome the calcination method that once heats up.
Technical scheme of the present invention is as follows:
From impure tantalum liquid material, make High-purity Tantalum liquid with liquid-liquid extraction method, again High-purity Tantalum liquid is obtained the High Purity Hydrogen tantalum oxide with neutralizing through the ammoniacal liquor that purifies, again with the washing of High Purity Hydrogen tantalum oxide, filtration, oven dry, it is characterized in that the High Purity Hydrogen tantalum oxide after the oven dry is packed in the stoving oven, carry out the branch section calcining as follows:
(1) is warmed up to 180-230 ℃ earlier, is incubated 2-3 hour;
(2) be warmed up to 480-530 ℃ again, be incubated 4-6 hour;
(3) be warmed up to 620680 ℃ again, be incubated 2-3 hour;
(4) be warmed up to 790-840 ℃ again, be incubated 3-5 hour;
(5) come out of the stove to sieve after cooling to 180-230 ℃ and promptly get high-purity tantalum pentoxide.
The preferred processing method of the present invention is as follows:
High Purity Hydrogen tantalum oxide after the oven dry is carried out the branch section calcining as follows:
(1) is warmed up to 200 ℃ earlier, is incubated 2 hours;
(2) be warmed up to 500 ℃ again, be incubated 5 hours;
(3) be warmed up to 650 ℃ again, be incubated 2 hours;
(4) be warmed up to 800 ℃ again, be incubated 4 hours;
(5) come out of the stove to sieve after cooling to 200 ℃ and promptly get high-purity tantalum pentoxide.
Know-why of the present invention has: 1, divide section calcining energy balance furnace body temperature, temperature of charge integral body is consistent, and can avoids the body of heater local temperature too high, play the effect of protection body of heater; 2,500-550 ℃ of insulation 4-6 hour, purpose is to guarantee Ta (OH)
5The NH of absorption
4F vapors away substantially, avoids Ta when high temperature (OH)
5Change into Ta
2O
5Parcel NH
4The phenomenon of F, thus fluorine content in the product reduced greatly; 3, when high temperature 800-850 ℃ of insulation, can make Ta (OH)
5Substantially change into Ta
2O
5, do not have part Ta (OH)
5The phenomenon that is wrapped.
The tantalum pentoxide product that the preparation method that uses segmentation incinerating of the present invention to hang down the high-purity tantalum pentoxide of fluorine is produced, the tantalum pentoxide product of producing with the disposable intensification calcining of utilization, detect through product quality supervision and inspection center, China Non-Ferrous Metals Industry south China, the index measured result of its foreign matter content as shown in Table 1:
Table one
| Sequence number | Test item (foreign matter content ppm) | National standard " high-purity tantalum pentoxide " is technical indicator (GB10577-89) | Disposable intensification calcination product test result | Segmentation calcination method product measured result of the present invention |
| 1 | Nb | ＜30 | ＜10 | ＜10 |
| 2 | Ti | ＜3 | ＜3 | ＜3 |
| 3 | W | ＜5 | ＜5 | ＜5 |
| 4 | Mo | ＜5 | ＜5 | ＜5 |
| 5 | Cr | ＜3 | ＜3 | ＜3 |
| 6 | Mn | ＜3 | ＜3 | ＜3 |
| 7 | Fe | ＜5 | ＜5 | ＜5 |
| 8 | Ni | ＜3 | ＜3 | ＜3 |
| 9 | Cu | ＜5 | ＜5 | ＜5 |
| 10 | A1 | ＜5 | ＜5 | ＜5 |
| 11 | Si | ＜13 | ＜13 | ＜13 |
| 12 | B | / | ＜5 | ＜5 |
| 13 | Sn | ＜3 | ＜3 | ＜3 |
| 14 | Pb | / | ＜5 | ＜5 |
| 15 | Sb | / | ＜5 | ＜5 |
| 16 | F | ＜70 | 60 | ＜40 |
| 17 | Loss on ignition | / | 0.25 | 0.1 |
Repeatedly experiment showed, repeatedly that through the contriver the present invention truly has following beneficial technical effects:
1, high-purity tantalum pentoxide fluorine content of the inventive method production is lower than the product with traditional mode of production; 2, tantalum pentoxide high conformity, the good uniformity produced; 3, loss on ignition is few; 4, the inventive method has provide protection to burner hearth, has improved the work-ing life of burner hearth.
Embodiment
The invention will be further described for the following examples, but should be as the restriction to protection scope of the present invention.
Embodiment one
1, from impure tantalum liquid material, makes High-purity Tantalum liquid with liquid-liquid extraction method, earlier tantalum liquid is squeezed into the neutralization precipitation groove, under agitation feed NH
3Gas makes pH value of solution=8-9, generates Ta (OH)
5Precipitation is passed through pressure filter or vacuum filtration with it then.Then tantalum hydroxide is reentered in the decomposer, adds hydrofluoric acid and sulfuric acid dissolution, carry out reextraction with organism and obtain High-purity Tantalum liquid;
2, the logical ammonia of High-purity Tantalum liquid is neutralized to pH＞9, generates tantalum hydroxide;
3, then with Ta (OH)
5Change in the vacuum filtration washing bath, wash, filter, be washed till filtrate and contain F＜0.02g/L, wash to change in the drying baker after qualified and dry with pure water;
4, the High Purity Hydrogen tantalum oxide after will drying carries out the branch section calcining as follows:
(1) is warmed up to 200 ℃ earlier, is incubated 2 hours;
(2) be warmed up to 500 ℃ again, be incubated 5 hours;
(3) be warmed up to 650 ℃ again, be incubated 2 hours;
(4) be warmed up to 800 ℃ again, be incubated 4 hours;
(5) come out of the stove to sieve after cooling to 200 ℃ and promptly get high-purity tantalum pentoxide.
Embodiment two
1, from impure tantalum liquid material, makes High-purity Tantalum liquid with liquid-liquid extraction method, earlier tantalum liquid is squeezed into the neutralization precipitation groove, under agitation feed NH
3Gas makes pH value of solution=8-9, generates Ta (OH)
5Precipitation is passed through pressure filter or vacuum filtration with it then.Then tantalum hydroxide is reentered in the decomposer, adds hydrofluoric acid and sulfuric acid dissolution, carry out reextraction with organism and obtain High-purity Tantalum liquid;
2, the logical ammonia of High-purity Tantalum liquid is neutralized to pH＞9, generates tantalum hydroxide;
3, then with Ta (OH)
5Change in the vacuum filtration washing bath, wash, filter, be washed till filtrate and contain F＜0.02g/L, wash to change in the drying baker after qualified and dry with pure water;
4, the High Purity Hydrogen tantalum oxide after will drying carries out the branch section calcining as follows:
(1) is warmed up to 230 ℃ earlier, is incubated 2 hours;
(2) be warmed up to 530 ℃ again, be incubated 4 hours;
(3) be warmed up to 620 ℃ again, be incubated 3 hours;
(4) be warmed up to 840 ℃ again, be incubated 3 hours;
(5) come out of the stove to sieve after cooling to 230 ℃ and promptly get high-purity tantalum pentoxide.
Embodiment three
1, from impure tantalum liquid material, makes High-purity Tantalum liquid with liquid-liquid extraction method, earlier tantalum liquid is squeezed into the neutralization precipitation groove, under agitation feed NH
3Gas makes pH value of solution=8-9, generates Ta (OH)
5Precipitation is passed through pressure filter or vacuum filtration with it then.Then tantalum hydroxide is reentered in the decomposer, adds hydrofluoric acid and sulfuric acid dissolution, carry out reextraction with organism and obtain High-purity Tantalum liquid;
2, the logical ammonia of High-purity Tantalum liquid is neutralized to pH＞9, generates tantalum hydroxide;
3, then with Ta (OH)
5Change in the vacuum filtration washing bath, wash, filter, be washed till filtrate and contain F＜0.02g/L, wash to change in the drying baker after qualified and dry with pure water;
4, the High Purity Hydrogen tantalum oxide after will drying carries out the branch section calcining as follows:
(1) is warmed up to 180 ℃ earlier, is incubated 3 hours;
(2) be warmed up to 490 ℃ again, be incubated 6 hours;
(3) be warmed up to 680 ℃ again, be incubated 2 hours;
(4) be warmed up to 790 ℃ again, be incubated 5 hours;
(5) come out of the stove to sieve after cooling to 190 ℃ and promptly get high-purity tantalum pentoxide.
Claims (2)
1. the preparation method of the high-purity tantalum pentoxide of low fluorine, from impure tantalum liquid material, make High-purity Tantalum liquid with liquid-liquid extraction method, again High-purity Tantalum liquid is obtained the High Purity Hydrogen tantalum oxide with neutralizing through the ammoniacal liquor that purifies, again with the washing of High Purity Hydrogen tantalum oxide, filtration, oven dry, it is characterized in that the High Purity Hydrogen tantalum oxide after the oven dry is packed in the stoving oven, carry out the branch section calcining as follows:
(1) is warmed up to 180-230 ℃ earlier, is incubated 2-3 hour;
(2) be warmed up to 480-530 ℃ again, be incubated 4-6 hour;
(3) be warmed up to 620-680 ℃ again, be incubated 2-3 hour;
(4) be warmed up to 790-840 ℃ again, be incubated 3-5 hour;
(5) come out of the stove to sieve after cooling to 180-230 ℃ and promptly get high-purity tantalum pentoxide.
2. the preparation method of the high-purity tantalum pentoxide of low fluorine according to claim 1 is characterized in that the High Purity Hydrogen tantalum oxide after the oven dry is carried out the branch section calcining as follows:
(1) is warmed up to 200 ℃ earlier, is incubated 2 hours;
(2) be warmed up to 500 ℃ again, be incubated 5 hours;
(3) be warmed up to 650 ℃ again, be incubated 2 hours;
(4) be warmed up to 800 ℃ again, be incubated 4 hours;
(5) come out of the stove to sieve after cooling to 200 ℃ and promptly get high-purity tantalum pentoxide.
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| CN102465204B (en) * | 2010-11-16 | 2013-11-06 | 肇庆多罗山蓝宝石稀有金属有限公司 | Method for preparing niobium pentoxide with high apparent density |
| CN102336439B (en) * | 2011-08-30 | 2013-07-31 | 宜春市金洋稀有金属有限公司 | Production method and device for tantalum niobium oxides |
| CN109607614A (en) * | 2018-12-26 | 2019-04-12 | 广东致远新材料有限公司 | A method of removing copper in tantalum niobium oxide process of producing product |
| CN110697774B (en) * | 2019-09-26 | 2021-06-18 | 清远佳致新材料研究院有限公司 | Method for preventing tantalum-niobium material from caking in sintering process |
| CN113213926B (en) * | 2021-04-09 | 2023-03-24 | 宁夏中色新材料有限公司 | Ta 2 O 5 Ceramic target material and preparation method thereof |
| CN114590837B (en) * | 2022-03-15 | 2023-09-01 | 先导薄膜材料（广东）有限公司 | Preparation method and application of high-purity cadmium antimonide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004143009A (en) * | 2002-10-25 | 2004-05-20 | Mitsui Mining & Smelting Co Ltd | Regeneration method of organic solvent in separation purification of tantalum and/or niobium by solvent extraction |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004143009A (en) * | 2002-10-25 | 2004-05-20 | Mitsui Mining & Smelting Co Ltd | Regeneration method of organic solvent in separation purification of tantalum and/or niobium by solvent extraction |
Non-Patent Citations (2)
| Title |
|---|
| 万明远.用N5O3二次萃取法制取高纯氧化钽.《稀有金属与硬质合金》.2002,第30卷(第2期),19-22. * |
| 胡益清.高纯氧化钽的研制.《稀有金属与硬质合金》.1994,(第116期),9-13. * |
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