CN1156404C - Solid state production process - Google Patents
Solid state production process Download PDFInfo
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- CN1156404C CN1156404C CNB011273011A CN01127301A CN1156404C CN 1156404 C CN1156404 C CN 1156404C CN B011273011 A CNB011273011 A CN B011273011A CN 01127301 A CN01127301 A CN 01127301A CN 1156404 C CN1156404 C CN 1156404C
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- carbonate
- acid salt
- strong acid
- alkali
- ammonium
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Abstract
The present invention provides a production technology for directly producing zirconium basic carbonate by zirconic strong acid salt and the carbonate of alkali or alkaline earth metal (including ammonium). The present invention particularly comprises: solid materials of zirconic strong acid salt and the carbonate of alkali or alkaline earth metal (including ammonium) are directly mixed according to a certain proportion; the mixture of the solid materials of zirconic strong acid salt and the carbonate of alkali or alkaline earth metal reacts completely through sufficiently stirring and grinding; then, zirconium basic carbonate is produced through washing and dewatering. The method that the solid materials of the zirconic strong acid salt and the carbonate of the alkali or the alkaline earth metal (including ammonium) are directly mixed according to the certain proportion for reacting is used by the technology of the present invention, which has the characteristics of simple equipment, short technological process, high yield and no discharge of three kinds of waste.
Description
Technical field
The invention provides with the strong acid salt solid material of zirconium and the carbonate of alkali-metal carbonate or ammonium is the production technique of raw material direct production zirconyl carbonate, belongs to technical field of inorganic chemical industry.
Background technology
The production technique of traditional zirconyl carbonate, be raw material normally with zirconium oxychloride, be made into certain density solution, add a certain amount of sulfuric acid or vitriol then, the controlled temperature hydrolysis generates zirconium basic sulphate, carbonate solution carbonization with alkali such as bicarbonate of ammonia or yellow soda ash and alkaline-earth metal or ammonium generates zirconyl carbonate again, obtains finished product through washing, centrifuge dehydration.This technical process is complicated, and energy consumption is big, needs through twice washing, 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 cost-effective production zirconyl carbonate, but shortened process cut down the consumption of energy, and reduce 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 with the carbonate of alkali-metal carbonate or ammonium; 2. mixture is stirred, grinds, make it abundant reaction, generate the strong acid salt reaction product of zirconyl carbonate and alkali-metal strong acid salt or ammonium; 3. reaction product is added entry by washing all over cover; 4. first pass washing lotion condensing crystal is produced the strong acid salt of alkali-metal strong acid salt of byproduct or ammonium; 5. will clean the reaction product centrifuge dehydration of the strong acid salt of alkali-metal strong acid salt or ammonium and produce zirconyl carbonate.
The strong acid salt of described zirconium is: the strong acid salt of zirconium comprises subsalt, acid salt, normal salt, double salt and other are as salts such as zirconium oxychlorides.The carbonate of alkaline carbonate or ammonium comprises normal salt, acid salt etc.The alkali-metal strong acid salt that reaction generates or the strong acid salt of ammonium should be soluble in water.
A kind of solid state reaction of the present invention is produced in the technology of zirconyl carbonate, the strong acid salt of zirconium is pressed product requirement with the blending ratio of the carbonate of alkali-metal carbonate or ammonium can be different, and step optimum proportion 1. is the carbonate generation equivalent replacement(metathesis)reaction of the strong acid salt, basic metal or the ammonium that make zirconium.
A kind of solid state reaction of the present invention is produced in the technology of zirconyl carbonate, the ratio that adds water when reaction product is washed is looked the basic metal of generation or the character of ammonium strong acid salt determines that step optimum proportion 3. should be convenient to the production of byproduct basic metal or ammonium strong acid salt and make washing times minimum.
A kind of solid state reaction of the present invention is produced in the technology of zirconyl carbonate, step can be carried out secondary filter earlier in 4. before condensing crystal, with the secondary filter of first pass washing lotion, remove impurity in the washing lotion, can improve the quality of byproduct basic metal or ammonium strong acid salt and improve the yield of zirconyl carbonate, the method for secondary filter is natural filtration, press filtration, centrifugation filtration etc.
Embodiment
Embodiment 1:
1. be the strong acid salt raw material of zirconium with the zirconium oxychloride, bicarbonate of ammonia is the alkaline carbonate raw material.2. with 1: 2 in molar ratio batching of zirconium oxychloride, bicarbonate of ammonia.3. with zirconium oxychloride, bicarbonate of ammonia thorough mixing, grinding, it is fully reacted.4. with reaction product 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 till being washed till muriate and meeting product standard and require (about 5 times), solids is zirconyl carbonate.
Embodiment 2
1. be the strong acid salt raw material of zirconium with the zirconium oxychloride, yellow soda ash is the alkaline carbonate raw material.2. with 1: 1 in molar ratio batching of zirconium oxychloride, yellow soda ash.3. with zirconium oxychloride, yellow soda ash 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 zirconyl carbonate
Embodiment 3
1. be the strong acid salt raw material of zirconium with the zirconium basic sulphate, bicarbonate of ammonia is the alkaline carbonate raw material.2. with 0.55: 1 in molar ratio batching of zirconium basic sulphate, bicarbonate of ammonia.3. with zirconium basic sulphate, bicarbonate of ammonia 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 till being washed till sulfide and meeting product standard and require (about 5 times), solids is zirconyl carbonate.
Embodiment 4:
1. be the strong acid salt raw material of zirconium with the zirconium sulfate, bicarbonate of ammonia is the alkaline carbonate raw material.2. with 1: 4 in molar ratio batching of zirconium sulfate, bicarbonate of ammonia.3. with zirconium sulfate, bicarbonate of ammonia 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 then, production byproduct of ammonium sulfate.7. solid part continues washing in a manner described, and washing lotion is applied mechanically, and till being washed till sulfide and meeting product standard and require (about 5 times), solids is zirconyl carbonate.
Claims (5)
1, a kind of solid state reaction is produced the technology of zirconyl carbonate, with the strong acid salt of zirconium and the carbonate direct production zirconyl carbonate of alkali-metal carbonate or ammonium, it is characterized in that taking following steps: 1. the strong acid salt solid material with zirconium mixes with the carbonate of alkali-metal carbonate or ammonium; 2. mixture is stirred, grinds, make it abundant reaction, generate the strong acid salt reaction product of zirconyl carbonate and alkali-metal strong acid salt or ammonium; 3. reaction product is added entry by washing all over cover; 4. first pass washing lotion condensing crystal is produced the strong acid salt of alkali-metal strong acid salt of byproduct or ammonium; 5. will clean the reaction product centrifuge dehydration of the strong acid salt of alkali-metal strong acid salt or ammonium and produce zirconyl carbonate.
2, solid state reaction as claimed in claim 1 is produced the technology of zirconyl carbonate, and it is characterized in that: the strong acid salt of described zirconium is: zirconium oxychloride, and the subsalt of zirconium or normal salt, the carbonate of described alkaline carbonate or ammonium comprises normal salt, acid salt.
3, solid state reaction as claimed in claim 1 or 2 is produced the technology of zirconyl carbonate, and it is characterized in that: the mol ratio of the carbonate reaction of the strong acid salt of zirconium and alkali-metal carbonate or ammonium is 1: 1～4.
4, solid state reaction as claimed in claim 1 or 2 is produced the technology of zirconyl carbonate, it is characterized in that: the step 3. part by weight of reaction product and water is 1～2: 1.
5, solid state reaction as claimed in claim 1 or 2 is produced the technology of zirconyl carbonate, it 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 |
|---|---|---|---|
| CNB011273011A CN1156404C (en) | 2001-08-07 | 2001-08-07 | Solid state production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011273011A CN1156404C (en) | 2001-08-07 | 2001-08-07 | Solid state production process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1328963A CN1328963A (en) | 2002-01-02 |
| CN1156404C true CN1156404C (en) | 2004-07-07 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011273011A Expired - Fee Related CN1156404C (en) | 2001-08-07 | 2001-08-07 | Solid state production process |
Country Status (1)
| Country | Link |
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| CN (1) | CN1156404C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840363B (en) * | 2017-12-23 | 2019-08-23 | 淄博广通化工有限责任公司 | The industrial carbonic acid zirconium production method of environmental-friendly low cost |
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2001
- 2001-08-07 CN CNB011273011A patent/CN1156404C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1328963A (en) | 2002-01-02 |
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Granted publication date: 20040707 Termination date: 20100807 |