CN1401579A - Solid-state production process - Google Patents
Solid-state production process Download PDFInfo
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- CN1401579A CN1401579A CN 01127352 CN01127352A CN1401579A CN 1401579 A CN1401579 A CN 1401579A CN 01127352 CN01127352 CN 01127352 CN 01127352 A CN01127352 A CN 01127352A CN 1401579 A CN1401579 A CN 1401579A
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- zirconium
- alkaline
- acid salt
- alkali
- strong acid
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Abstract
A solid process for preparing zirconium hydroxide includes mixing the zirconium salt of strong acid with the alkali metal (or alkali-earth metal) hydroxide, stirring, grinding, water washing and dewatering. Its advantages are high yield and no environmental pollution.
Description
Technical field
The oxyhydroxide that the invention provides strong acid salt, alkali or alkaline-earth metal (comprising ammonium) with zirconium is the production technique of raw material direct production zirconium hydroxide, belongs to technical field of inorganic chemical industry.
Background technology
The production technique of traditional zirconium hydroxide is a raw material with zirconium oxychloride normally, is made into certain density solution, adds certain amount of ammonia water then, and neutralization generates zirconium hydroxide, obtains finished product through washing, centrifuge dehydration.This handicraft product zirconium dioxide content is low, and water consumption is big, produces a large amount of waste water and is difficult to handle, directly the exhaust emission environment.
Summary of the invention
The purpose of this invention is to provide a kind of economical and effective and must produce the method for zirconium hydroxide, but shortened process, zirconium dioxide content height in the product reduces water consumption, and waste water is easy to handle, and reclaims byproduct, eliminates environmental pollution.
The object of the present invention is achieved like this:
1. the strong acid salt solid material with zirconium mixes by a certain percentage with the oxyhydroxide of alkali or alkaline-earth metal (comprising ammonium).2. mixture is stirred, grinds, make it abundant reaction, generate the strong acid salt reactant of zirconium hydroxide and alkali or alkaline-earth metal.3. reactant is added a certain proportion of pure water by washing all over cover.4. first pass washing lotion condensing crystal is produced byproduct alkali or alkaline-earth metal strong acid salt.5. the reactant centrifuge dehydration that will clean alkaline or alkaline-earth salts promptly obtains zirconium hydroxide.6. with zirconium hydroxide roasting at high temperature, promptly obtain zirconium dioxide.
The production technique of the oxyhydroxide direct production zirconium hydroxide of described a kind of strong acid salt, alkali or alkaline-earth metal (comprising ammonium) with zirconium, the strong acid salt of zirconium comprises subsalt, acid salt, normal salt, double salt and other as salts such as zirconium oxychlorides, and alkali or alkaline-earth metal strong acid salt that reaction generates should be soluble in water.
The production technique of the oxyhydroxide direct production zirconium hydroxide of a kind of strong acid salt of the present invention, alkali or alkaline-earth metal (comprising ammonium) with zirconium, the strong acid salt of zirconium is pressed product requirement with the blending ratio of the oxyhydroxide of alkali or alkaline-earth metal (comprising ammonium) can be different, and step optimum proportion 1. is the oxyhydroxide generation equivalent replacement(metathesis)reaction of strong acid salt, alkali or the alkaline-earth metal (comprising ammonium) that make zirconium.
The production technique of the oxyhydroxide direct production zirconium hydroxide of a kind of strong acid salt with zirconium of the present invention, alkali or alkaline-earth metal (comprising ammonium), the ratio that adds water when reactant is washed are looked the alkali of generation or the character of alkaline-earth metal strong acid salt is determined step
The production technique of the oxyhydroxide direct production zirconium hydroxide of a kind of strong acid salt of the present invention, alkali or alkaline-earth metal (comprising ammonium) with zirconium, step 4. in before condensing crystal, with the accurate separation of first pass washing lotion, remove impurity in the washing lotion, can improve the quality of byproduct alkali or alkaline-earth metal strong acid salt and improve the yield of zirconium hydroxide.
Embodiment
Embodiment 1:
1. be the strong acid salt raw material of zirconium with the zirconium oxychloride, ammoniacal liquor is the alkali metal hydroxide raw material.2. with 1: 2 in molar ratio batching of zirconium oxychloride, ammoniacal liquor.3. with zirconium oxychloride, ammoniacal liquor thorough mixing, grinding, it is fully reacted.4. with reactant and pure water mixed by 2: 1.5. with the mixed serum solid-liquid separation.6. isolated liquid precise is filtered, remove suspended impurity, condensing crystal is produced byproduct ammonium chloride then.7. solid part continues washing in a manner described, and washing lotion is applied mechanically, and is washed till muriate and meets till the product standard requirement, and solids is zirconium hydroxide.8. about 550 ℃ with zirconium hydroxide roasting 4 hours, obtain zirconium dioxide.
Embodiment 2
1. be the strong acid salt raw material of zirconium with the zirconium oxychloride, sodium hydroxide is the alkali metal hydroxide raw material.2. with 1: 2 in molar ratio batching of zirconium oxychloride, sodium hydroxide.3. with zirconium oxychloride, sodium hydroxide thorough mixing, grinding, it is fully reacted.4. with reactant and pure water mixed by weight 1: 1.5. with the mixed serum solid-liquid separation.6. isolated liquid precise is filtered, remove suspended impurity, condensing crystal is produced byproduct sodium-chlor then.7. solid part continues washing in a manner described, and washing lotion is applied mechanically, and till being washed till muriate and meeting product standard and require (about 5 times), solids is zirconium hydroxide.8. about 550 ℃ with zirconium hydroxide roasting 4 hours, obtain zirconium dioxide.
Embodiment 3
1. be the strong acid salt raw material of zirconium with the zirconium basic sulphate, ammoniacal liquor is the alkali metal hydroxide raw material.2. with 1: 2 in molar ratio batching of zirconium basic sulphate, ammoniacal liquor.3. with zirconium basic sulphate, ammoniacal liquor thorough mixing, grinding, it is fully reacted.4. with reactant and pure water mixed by weight 2: 1.5. with the mixed serum solid-liquid separation.6. isolated liquid precise is filtered, remove suspended impurity, condensing crystal then, production byproduct of ammonium sulfate.7. solid part continues washing in a manner described, and washing lotion is applied mechanically, and is washed till sulfide and meets till the product standard requirement, and solids is zirconium hydroxide.8. about 550 ℃ with zirconium hydroxide roasting 4 hours, obtain zirconium dioxide.
Embodiment 4:
1. be the strong acid salt raw material of zirconium with the zirconium sulfate, sodium hydroxide is the alkali metal hydroxide raw material.2. with 1: 4 in molar ratio batching of zirconium sulfate, sodium hydroxide.3. with zirconium sulfate, sodium hydroxide thorough mixing, grinding, it is fully reacted.4. with reactant and pure water mixed by 5: 3.5. with the mixed serum solid-liquid separation.6. isolated liquid precise is filtered, remove suspended impurity, condensing crystal is produced byproduct sulfite then.7. solid part continues washing in a manner described, and washing lotion is applied mechanically, and is washed till sulfide and meets till the product standard requirement, and solids is zirconium hydroxide.8. about 550 ℃ with zirconium hydroxide roasting 4 hours, obtain zirconium dioxide.
Claims (6)
1, the production technique of the oxyhydroxide direct production zirconium hydroxide of a kind of strong acid salt with zirconium, alkali or alkaline-earth metal (comprising ammonium) is characterized in that taking following steps: 1. the oxyhydroxide of the solid-state material of the strong acid salt of zirconium with alkali or alkaline-earth metal (comprising ammonium) is mixed by a certain percentage.2. mixture is stirred, grinds, make it abundant reaction, generate the strong acid salt reactant of zirconium hydroxide and alkali or alkaline-earth metal.3. reactant is added a certain proportion of pure water by washing all over cover.4. first pass washing lotion condensing crystal is produced byproduct alkali or alkaline-earth metal strong acid salt.5. the reactant centrifuge dehydration that will clean alkaline or alkaline-earth salts promptly obtains zirconium hydroxide.6. with zirconium hydroxide roasting at high temperature, promptly obtain zirconium dioxide.
2, the production technique of the oxyhydroxide direct production zirconium hydroxide of a kind of strong acid salt as claimed in claim 1, alkali or alkaline-earth metal (comprising ammonium) with zirconium, it is characterized in that: the strong acid salt of described zirconium comprises subsalt, acid salt, normal salt, double salt and other as salts such as zirconium oxychlorides, and alkali that reaction generates or alkaline-earth metal strong acid salt must be soluble in water.
3, the production technique of the oxyhydroxide direct production zirconium hydroxide of a kind of strong acid salt as claimed in claim 1, alkali or alkaline-earth metal (comprising ammonium) with zirconium, the strong acid salt of zirconium is pressed product requirement with the blending ratio of the oxyhydroxide of alkali or alkaline-earth metal (comprising ammonium) can be different, it is characterized in that: step optimum proportion 1. is the oxyhydroxide generation equivalent replacement(metathesis)reaction of strong acid salt, alkali or the alkaline-earth metal (comprising ammonium) that make zirconium.
4, the production technique of the oxyhydroxide direct production zirconium hydroxide of a kind of strong acid salt as claimed in claim 1, alkali or alkaline-earth metal (comprising ammonium) with zirconium, the ratio that adds water when reactant is washed is looked the alkali of generation or the character of alkaline-earth metal strong acid salt determines that it is characterized in that: step optimum proportion 3. should be convenient to the production of byproduct alkali or alkaline-earth metal strong acid salt and make washing times minimum.
5, the production technique of the oxyhydroxide direct production zirconium hydroxide of a kind of strong acid salt as claimed in claim 1, alkali or alkaline-earth metal (comprising ammonium) with zirconium, step can be carried out precision in 4. earlier and be separated before condensing crystal, it is characterized in that: with the accurate separation of first pass washing lotion, remove impurity in the washing lotion, can improve the quality of byproduct alkali or alkaline-earth metal strong acid salt and improve the yield of zirconium hydroxide.
6, the production technique of the oxyhydroxide direct production zirconium hydroxide of a kind of strong acid salt as claimed in claim 1, alkali or alkaline-earth metal (comprising ammonium) with zirconium, the maturing temperature difference of zirconium hydroxide, the crystalline form difference of gained zirconium dioxide is characterized in that: the optimum temps of roasting is 500 ℃ to 600 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011273526A CN1160254C (en) | 2001-08-28 | 2001-08-28 | Solid-state production process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011273526A CN1160254C (en) | 2001-08-28 | 2001-08-28 | Solid-state production process |
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| CN1401579A true CN1401579A (en) | 2003-03-12 |
| CN1160254C CN1160254C (en) | 2004-08-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB011273526A Expired - Fee Related CN1160254C (en) | 2001-08-28 | 2001-08-28 | Solid-state production process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101708862B (en) * | 2009-12-10 | 2011-06-15 | 江西晶安高科技股份有限公司 | Zirconium hydroxide solid-phase grinding synthesis method |
| CN105502490A (en) * | 2015-04-21 | 2016-04-20 | 江西晶安高科技股份有限公司 | Coarse-grained sphere-like zirconium hydroxide with large specific surface area and preparation method of zirconium hydroxide |
-
2001
- 2001-08-28 CN CNB011273526A patent/CN1160254C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101708862B (en) * | 2009-12-10 | 2011-06-15 | 江西晶安高科技股份有限公司 | Zirconium hydroxide solid-phase grinding synthesis method |
| CN105502490A (en) * | 2015-04-21 | 2016-04-20 | 江西晶安高科技股份有限公司 | Coarse-grained sphere-like zirconium hydroxide with large specific surface area and preparation method of zirconium hydroxide |
| CN105502490B (en) * | 2015-04-21 | 2017-03-29 | 江西晶安高科技股份有限公司 | A kind of coarseness, spherical zirconium hydroxide of bigger serface and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1160254C (en) | 2004-08-04 |
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