CN1125195A - Producing zirconium series products using non-crystallization purification method - Google Patents
Producing zirconium series products using non-crystallization purification method Download PDFInfo
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- CN1125195A CN1125195A CN 94118617 CN94118617A CN1125195A CN 1125195 A CN1125195 A CN 1125195A CN 94118617 CN94118617 CN 94118617 CN 94118617 A CN94118617 A CN 94118617A CN 1125195 A CN1125195 A CN 1125195A
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- zirconium
- crystallization
- purification method
- technical characterictic
- series products
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Abstract
The production method of zirconium series product instead of purification by crystallization is characterized by reducing Fe3+ to Fe2+; controlling appropriate pH value; heating and boiling zirconium solution to make the zirconium solution hydrolyze and sedimentate to separate out Fe, Ti and Si etc.; removing aluminium by using alkali liquor so as to easily obtain pure zirconium solution.
Description
This invention belongs to chemical technology field (comprising inorganic chemical industry, fine chemistry industry, technical analysis)
The prior art of producing serial zirconium products has carbonization monochlor(in)ate method, lime (or limestone powder) sintering process, soda ash sintering process or caustic soda scorification with regard to regard to the method difference of decomposing zircon sand.When the zirconium liquid of above-mentioned these methods after grog is carried out acidifying is purified, no matter be diacid two alkali technologies, or a sour alkali primary crystallization or a sour alkali secondary crystallization process etc., that uses all carries out crystallization and purification by concentrating, the present invention is then completely different with prior art, and have incomparable advantage of prior art or positively effect, in the middle of the process of this invention of research, I am with reference to following four parts of materials:
1, " inorganic chemistry " is write group and is compiled inorganic chemistry, People's Education Publishing House, 1978.
2, rare metal knowledge is write group and is compiled zirconium and hafnium, metallurgical industry press, 1974.
3, one piece of paper writing such as Li Baolan, teachers college, Guangxi journal (natural science edition), 19881.
4, Lou Shucong writes, chemical reagent preparation handbook, Jiangsu science tech publishing house, 1993.
The technical scheme of this invention is:
Substantially, decompose completely the zircon sand grog with the acid dissolving after, ferric iron is reduced to ferrous iron, the ebuillition of heated silica removal with suitable reductive agent, under suitable pH value condition,, remove aluminium with alkali lye by impurity such as hydrolytic precipitation separating ferrum, titaniums, afterwards, can obtain purified zirconium liquid easily.
The comparison of this invention and prior art:
1, the production cycle: no matter existing crystallization and purification technology is to adopt spontaneous nucleation or stirring crystallisation by cooling, and in a single day the production cycle is all very long, but adopts the present invention, then significantly shortened the production cycle.
2, the utilization of zirconium: during crystallization and purification, acid will recycle, and will cause iron, titanium, sodium or calcium etc. poly-more many more like this, the discharging regularly of having to, this not only will cause the waste (also will cause the energy to heighten even reclaim) of acid, and the loss of zirconium is also relatively more serious, still, in case adopt method of the present invention, zirconium has then almost absolutely obtained utilization, also can find out from this point, material consumption, the energy consumption of 1 ton of product of every production, crystallization purification method is high than the method for this invention.
3, energy consumption.If adopting, crystallization stirs crystallisation by cooling, then long owing to the production cycle, thus cause energy consumption higher, especially must concentrate before the crystallization, the energy consumption that causes like this is just more, if still adopted after the method for the present invention, energy consumption just can be significantly reduced.
4, acid consumption.Crystallization purification method is produced zirconium dioxide, if dissolution of crystals and be neutralized to alkalescence, and then not only many consumption neutral alkali, and will waste nearly 2 tons of the hydrochloric acid of folding 30% more, even crystal is directly sent to roasting, more product per ton also will be wasted and roll over nearly 2 tons of 30% hydrochloric acid.
5, environmental protection.Crystallization purification method, what generally adopt is concentrated hydrochloric acid, especially lime sinter process like this, must cause the operating environment severe contamination, have a strong impact on the healthy of operator, but,, just can make that operating environment significantly improves as long as adopted production method of the present invention, certainly also just make production operation, the production management facility many.
Below just the best way that realizes invention is described in detail:
Substantially, decompose zircon sand grog acid (hydrochloric acid or sulfuric acid) dissolving completely, and keep final [H
+About]=0.5M, acid is molten should be carried out in the glassed steel reaction vessels of strap clamp cover, after acid is molten, adds an amount of iron filings (or iron powder) and reduces under stirring heating ebullient condition, by the time Fe
3+All be converted into Fe
2+And some Ti
3+Till the generation, the reductive degree can be learnt by detection.Suction filtration is isolated unnecessary iron filings and part silicon-dioxide, and filtrate is got back in the reactor, with ammoniacal liquor the pH value of feed liquid is transferred near ebuillition of heated under 4 the condition about half an hour, and sampling makes liquid-solid layering, if supernatant liquor has not had ZrO
2+, then boiled water is separated end, and suction filtration is isolated clear liquid, is 4 weak acid scrubbing filter cake with deironing and pH value, until check filtrate iron-free, and till calcium, magnesium disappears.Best testing makes the Fe in the filter cake once
2O
3Amount and ZrO
2Amount ratio less than the ratio of technical indicator, detect again and have or not Ai in the filter cake
3+Exist,, then will unload filter cake and put into enamelled vessel or plastic containers, add the iron-free white liquor, make [the OH of mixed slurry if having
-]=1M is many, stir a quarter, suction filtration is isolated alkali lye then, repeatedly filter cake is soaked again with the many no Fe caustic soda clear liquids of a certain amount of 1M, suction filtration separates, and is till the no Ai, extremely neutral with the pure water washing again in filter cake, add an amount of pure acid (hydrochloric acid or the sulfuric acid etc.) filter cake that heating for dissolving unloads then, add an amount of pure zirconia agent (as NaClO, H
2O
2), make the Ti in the solution all change Ti into
4+, the pH value of transferring solution is between 1～1.5, and ebuillition of heated does not have TiO about half an hour in the clear liquid of sampling filtering
2+, and SiO
2Amount and ZrO
2The ratio of amount less than the corresponding ratio in the technical indicator till, vacuum filtration is isolated the Ti throw out, recycled, the clear liquid of removing behind the Ti transfers pH value near 4 hydrolytic precipitations with pure ammoniacal liquor, the throw out filter dehydration is directly precipitated in also adjustable pH value to 8～9, and use the pure water washes clean, until no Na
+Or there is not a NH
4 +Check Na
2The amount of O and ZrO
2The ratio of amount, be less than the corresponding techniques indicator ratio, the filter cake after qualified can be sent to the direct production serial zirconium products.For example, directly send to the oven dry roasting and promptly get ZrO
2Product is directly with pure hydrochloric acid heating for dissolving and the concentrated a little crystallisation by cooling production zirconium oxychloride product that gets final product.
Attached: 1. above-mentioned deironing and remove these two steps of titanium, order can exchange, and just specific practice is slightly different, for saving space, is omitted herein.
2. above-described vacuum filtration if operational difficulty is arranged, can be used whizzer to carry out centrifuging and separate.
Claims (1)
- The common technical characterictic of noncrystalline purification techniques and existing crystallization and purification technology is, all is to purify with the zirconium liquid after the acidifying.The technical characterictic of this invention is: ferric iron is reduced into ferrous iron; The ebuillition of heated silica removal; Ebuillition of heated hydrolytic precipitation separating ferrum and titanium, alkali lye removes aluminium.The production technology of the serial zirconium products of every technical characterictic that meets foregoing invention all requires to obtain patent protection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94118617 CN1125195A (en) | 1994-12-18 | 1994-12-18 | Producing zirconium series products using non-crystallization purification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94118617 CN1125195A (en) | 1994-12-18 | 1994-12-18 | Producing zirconium series products using non-crystallization purification method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1125195A true CN1125195A (en) | 1996-06-26 |
Family
ID=5038938
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94118617 Pending CN1125195A (en) | 1994-12-18 | 1994-12-18 | Producing zirconium series products using non-crystallization purification method |
Country Status (1)
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|---|---|
| CN (1) | CN1125195A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011278A (en) * | 2013-01-11 | 2013-04-03 | 周涛 | Process for hydrothermally preparing zirconium oxychloride with low alkali consumption |
| CN103253702A (en) * | 2012-02-15 | 2013-08-21 | 淄博市周村磊宝耐火材料有限公司 | Method for purification of waste zirconium brick to prepare high purity zirconia |
| CN106082324A (en) * | 2016-06-03 | 2016-11-09 | 辽宁石化职业技术学院 | A kind of iron-free Zr (SO4)2production method |
-
1994
- 1994-12-18 CN CN 94118617 patent/CN1125195A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253702A (en) * | 2012-02-15 | 2013-08-21 | 淄博市周村磊宝耐火材料有限公司 | Method for purification of waste zirconium brick to prepare high purity zirconia |
| CN103253702B (en) * | 2012-02-15 | 2016-01-27 | 山东磊宝锆业科技股份有限公司 | To purify from zirconium gives up brick the zirconic method of high purity |
| CN103011278A (en) * | 2013-01-11 | 2013-04-03 | 周涛 | Process for hydrothermally preparing zirconium oxychloride with low alkali consumption |
| CN106082324A (en) * | 2016-06-03 | 2016-11-09 | 辽宁石化职业技术学院 | A kind of iron-free Zr (SO4)2production method |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |