CN1160254C - Solid-state production process - Google Patents
Solid-state production process Download PDFInfo
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- CN1160254C CN1160254C CNB011273526A CN01127352A CN1160254C CN 1160254 C CN1160254 C CN 1160254C CN B011273526 A CNB011273526 A CN B011273526A CN 01127352 A CN01127352 A CN 01127352A CN 1160254 C CN1160254 C CN 1160254C
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- zirconium
- acid salt
- hydroxide
- strong acid
- zirconium hydroxide
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Abstract
The present invention relates to a technology for directly producing zirconium hydroxide by zirconic strong acid salt and the hydroxide of alkali or alkaline earth metal (including ammonium). The technology of the present invention particularly comprises: the zirconic strong acid salt and the hydroxide of the alkali or the alkaline earth metal (including ammonium) are directly mixed according to a certain proportion; through sufficiently stirring and grinding, the mixture of the previous raw materials react completely; then, through the processes of washing and dewatering, zirconium hydroxide is produced. The method that solid materials of the zirconic strong acid salt and the hydroxide of the alkali or the alkaline earth metal (including the ammonium) are directly mixed to react according to a certain proportion is used by the technology of the present invention, which has the characteristics of simple equipment, short technological process, high yield and no three-waste discharge.
Description
Technical field
The invention provides a kind of production technique of zirconium hydroxide, being used for the strong acid salt with zirconium, alkali-metal oxyhydroxide or ammoniacal liquor is 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 method that the purpose of this invention is to provide a kind of production zirconium hydroxide of economical and efficient, 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 solid-state material of the strong acid salt of zirconium is mixed with alkali-metal oxyhydroxide or ammoniacal liquor; 2. mixture is stirred, grinds, make it abundant reaction, generate the strong acid salt reaction product of zirconium hydroxide and basic metal or ammonium; 3. this reaction product is added pure water by washing all over cover; 4. first pass washing lotion condensing crystal is produced byproduct basic metal or ammonium strong acid salt; 5. the reaction product centrifuge dehydration that will clean the strong acid salt of basic metal or ammonium obtains zirconium hydroxide.
Above-mentioned zirconium hydroxide at high temperature roasting obtains zirconium dioxide.
The production technique of zirconium hydroxide of the present invention, the strong acid salt of zirconium comprise subsalt, acid salt, normal salt, double salt and other as salts such as zirconium oxychlorides, and basic metal or ammonium strong acid salt that reaction generates are soluble in water.
The production technique of zirconium hydroxide of the present invention, the strong acid salt of zirconium is pressed product requirement with the blending ratio of the oxyhydroxide of alkali or alkaline-earth metal and ammonium can be different, and step optimum proportion 1. is the strong acid salt, alkali or the alkaline-earth metal that make zirconium and the oxyhydroxide generation equivalent replacement(metathesis)reaction of ammonium.
The production technique of zirconium hydroxide of the present invention, the ratio that adds water when reaction product is washed is looked the alkali of generation or the character of alkaline-earth metal strong acid salt determines 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.
The production technique of zirconium hydroxide of the present invention, step 4. in before condensing crystal, should separate the first pass washing lotion is accurate, 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 zirconium oxychloride, ammoniacal liquor 1:2 batching in molar ratio.3. with zirconium oxychloride, ammoniacal liquor thorough mixing, grinding, it is fully reacted.4. reaction product is mixed with the part by weight of pure water 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.Resulting zirconium hydroxide can obtain zirconium dioxide in 4 hours in about 550 ℃ of following roastings.
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 reaction product 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.Resulting zirconium hydroxide can obtain zirconium dioxide in 4 hours in about 500 ℃ of following roastings.
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 reaction product 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.Resulting zirconium hydroxide can obtain zirconium dioxide in 4 hours in about 550 ℃ of following roastings.
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 reaction product 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.Resulting zirconium hydroxide can obtain zirconium dioxide in 4 hours in about 550 ℃ of following roastings.
Claims (5)
1, a kind of production technique of zirconium hydroxide, strong acid salt and alkali-metal oxyhydroxide or ammoniacal liquor direct production zirconium hydroxide with zirconium is characterized in that taking following steps: 1. the solid-state material of the strong acid salt of zirconium is mixed with alkali-metal oxyhydroxide or ammoniacal liquor; 2. mixture is stirred, grinds, make it abundant reaction, generate the strong acid salt reaction product of zirconium hydroxide and basic metal or ammonium; 3. this reaction product is added pure water by washing all over cover; 4. first pass washing lotion condensing crystal is produced byproduct basic metal or ammonium strong acid salt; 5. the reaction product centrifuge dehydration that will clean the strong acid salt of basic metal or ammonium obtains zirconium hydroxide.
2, the production technique of zirconium hydroxide as claimed in claim 1 is characterized in that: the strong acid salt of described zirconium is: zirconium oxychloride, the subsalt of zirconium or following salt.
3, the production technique of zirconium hydroxide as claimed in claim 1 or 2 is characterized in that: the mol ratio of the strong acid salt of zirconium and alkali metal hydroxide or ammoniacal liquor is 1: 1～4.
4, the production technique of zirconium hydroxide as claimed in claim 1 or 2 is characterized in that: the step 3. part by weight of reaction product and water is 1～2: 1.
5, the production technique of zirconium hydroxide as claimed in claim 1 or 2 is characterized in that: step is filtered earlier before condensing crystal in 4., removes impurity in the washing lotion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011273526A CN1160254C (en) | 2001-08-28 | 2001-08-28 | Solid-state production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011273526A CN1160254C (en) | 2001-08-28 | 2001-08-28 | Solid-state production process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1401579A CN1401579A (en) | 2003-03-12 |
| CN1160254C true 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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| CN (1) | CN1160254C (en) |
Families Citing this family (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 |
| 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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2001
- 2001-08-28 CN CNB011273526A patent/CN1160254C/en not_active Expired - Fee Related
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| CN1401579A (en) | 2003-03-12 |
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