CN107892327A - A kind of zirconium oxide production technology - Google Patents
A kind of zirconium oxide production technology Download PDFInfo
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- CN107892327A CN107892327A CN201711213792.0A CN201711213792A CN107892327A CN 107892327 A CN107892327 A CN 107892327A CN 201711213792 A CN201711213792 A CN 201711213792A CN 107892327 A CN107892327 A CN 107892327A
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
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Abstract
The invention discloses a kind of zirconium oxide production technology, comprise the following steps：Zircon is placed in smelting furnace, and caustic soda is added into smelting furnace, it need to be mixed in real time, pass through hot water leaching melt liquid, first mixed liquor is placed in agitator, then sodium zirconate is added thereto, and it is stirred in real time, add acid solution thereto again, obtain the second mixed liquor, the second mixed liquor after cleaning will be completed again to be placed in vessel, and mixed under conditions of 60 80 degrees Celsius, while stirring, precipitating reagent is added thereto, by the zirconium hydroxide after processing, it is again placed in smelting furnace, and second melting is carried out under conditions of 500 600 degrees Celsius, then catalyst is added into solution, produce zirconium oxide.The present invention can not only effectively improve the quality of zirconium oxide, additionally it is possible to improve the fusing point of zirconium oxide, so as to adapt it in different environment, meet the demand developed now.
Description
Technical field
The present invention relates to zirconium oxide preparing technical field, more particularly to a kind of zirconium oxide production technology.
Background technology
Zirconium oxide (ZrO2) nature zirconium oxide raw mineral materials, mainly have baddeleyite and zircon.Zircon system fire into
Rock deep layer mineral, color have yellowish, pale brown, yellowish green etc., proportion 4.6-4.7, hardness 7.5, have strong metallic luster, can
For ceramic glaze raw material.As present zirconium oxide suffers from more or less utilization in all trades and professions, to the quality of zirconium oxide
Increasingly pay attention to, in the prior art, all simply just directly make use of after baddeleyite either zircon progress preliminary treatment,
So that the quality deficiency of zirconium oxide.Therefore, we have proposed a kind of zirconium oxide production technology.
The content of the invention
The present invention proposes a kind of zirconium oxide production technology, to solve the problems mentioned in the above background technology.
The present invention proposes a kind of zirconium oxide production technology, comprises the following steps：
S1：Selection zircon is raw material, and zircon is carried out into repeated ultrasonic ripple cleaning, to remove the miscellaneous of zircon surface
Matter, then it is dried for standby；
S2：Zircon after being handled in S1 is placed in smelting furnace, and caustic soda is added into smelting furnace, is taken the photograph in 600-700
Melted, in fusion process, it need to be mixed in real time, to ensure that zircon mixes with caustic soda under conditions of family name's degree
Close uniformly, after the completion for the treatment of melting, by hot water leaching melt liquid, form the first mixed liquor, it is standby；
S3：First mixed liquor of above-mentioned formation is placed in agitator, and its temperature is reduced to 300-450 degrees Celsius,
Then sodium zirconate is added thereto, and is stirred in real time, so as to be separated to the first mixed liquor, after the completion of separation, then to
Acid solution is wherein added, obtains the second mixed liquor, and the second mixed liquor is placed in filter mechanism and removed the gred, it is standby after the completion of removal of impurities
With；
S4：The second mixed liquor after cleaning will be completed again to be placed in vessel, and is carried out under conditions of 60-80 degrees Celsius
Mix, while stirring, add precipitating reagent thereto, precipitation obtains zirconium hydroxide, standby；
S5：The zirconium hydroxide after being handled in S4 is again placed in smelting furnace, and under conditions of 500-600 degrees Celsius
Second melting is carried out, catalyst is then added into solution, and is mixed evenly, is then filtered solution, after filtering,
Concentration, crystallisation by cooling, crushing, roasting are evaporated again, produce zirconium oxide.
Preferably, the acid solution in S3 is nitric acid and one kind in sulfuric acid.
Preferably, the precipitating reagent in S4 is the mixture of oxalic acid, ammonium hydrogen carbonate, ammoniacal liquor and sodium hydroxide, and oxalic acid,
The weight ratio of ammonium hydrogen carbonate, ammoniacal liquor and sodium hydroxide is 1：0.5：1：0.5.
Preferably, the smelting furnace in S2 inside smelting furnace before use, will need to be cleaned multiple times, after then cleaning
Smelting furnace dried, and preheating 10-20min is carried out under conditions of 120-200 degrees Celsius.
Preferably, the catalyst in S5 is zirconium nitrate solution, the mixed liquor of hexamethylenetetramine solution, and zirconium nitrate is molten
Liquid, hexamethylenetetramine solution molal weight ratio are 2：0.5.
A kind of zirconium oxide production technology proposed by the present invention, beneficial effect are：The zirconium oxide production technology passes through to zirconium
Diamond stone is repeatedly handled, and can not only effectively improve the quality of zirconium oxide, additionally it is possible to the fusing point of zirconium oxide is improved, so as to
Enough adapt it in different environment, meet the demand developed now.
Embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
The present invention proposes a kind of zirconium oxide production technology, comprises the following steps：
S1：Selection zircon is raw material, and zircon is carried out into repeated ultrasonic ripple cleaning, to remove the miscellaneous of zircon surface
Matter, then it is dried for standby；
S2：Zircon after being handled in S1 is placed in smelting furnace, and caustic soda is added into smelting furnace, at 600 degrees Celsius
Under conditions of melted, in fusion process, it need to be mixed in real time, to ensure that zircon mixes with caustic soda
It is even, after the completion for the treatment of melting, by hot water leaching melt liquid, the first mixed liquor is formed, it is standby；
S3：First mixed liquor of above-mentioned formation is placed in agitator, and its temperature is reduced to 300 degrees Celsius, then
Sodium zirconate is added thereto, and is stirred in real time, so as to be separated to the first mixed liquor, after the completion of separation, then thereto
Acid solution is added, obtains the second mixed liquor, and the second mixed liquor is placed in filter mechanism and removed the gred, it is standby after the completion of removal of impurities；
S4：The second mixed liquor after cleaning will be completed again to be placed in vessel, and is mixed under conditions of 60 degrees Celsius
Stirring is closed, while stirring, adds precipitating reagent thereto, precipitation obtains zirconium hydroxide, standby；
S5：By the zirconium hydroxide after being handled in S4, it is again placed in smelting furnace, and carried out under conditions of 500 degrees Celsius
Second melting, catalyst is then added into solution, and be mixed evenly, then filtered solution, after filtering, again
Concentration, crystallisation by cooling, crushing, roasting are evaporated, produces zirconium oxide.
Acid solution in S3 is nitric acid and one kind in sulfuric acid.
Precipitating reagent in S4 is oxalic acid, the mixture of ammonium hydrogen carbonate, ammoniacal liquor and sodium hydroxide, and oxalic acid, bicarbonate
The weight ratio of ammonium, ammoniacal liquor and sodium hydroxide is 1：0.5：1：0.5.
Smelting furnace in S2 inside smelting furnace before use, will need to be cleaned multiple times, then by the melting after cleaning
Stove is dried, and preheating 10min is carried out under conditions of 120 degrees Celsius.
Catalyst in S5 is zirconium nitrate solution, the mixed liquor of hexamethylenetetramine solution, and zirconium nitrate solution, six times
Tetramine solution molal weight ratio is 2：0.5.
Embodiment 2
The present invention proposes a kind of zirconium oxide production technology, comprises the following steps：
S1：Selection zircon is raw material, and zircon is carried out into repeated ultrasonic ripple cleaning, to remove the miscellaneous of zircon surface
Matter, then it is dried for standby；
S2：Zircon after being handled in S1 is placed in smelting furnace, and caustic soda is added into smelting furnace, at 625 degrees Celsius
Under conditions of melted, in fusion process, it need to be mixed in real time, to ensure that zircon mixes with caustic soda
It is even, after the completion for the treatment of melting, by hot water leaching melt liquid, the first mixed liquor is formed, it is standby；
S3：First mixed liquor of above-mentioned formation is placed in agitator, and its temperature is reduced to 330 degrees Celsius, then
Sodium zirconate is added thereto, and is stirred in real time, so as to be separated to the first mixed liquor, after the completion of separation, then thereto
Acid solution is added, obtains the second mixed liquor, and the second mixed liquor is placed in filter mechanism and removed the gred, it is standby after the completion of removal of impurities；
S4：The second mixed liquor after cleaning will be completed again to be placed in vessel, and is mixed under conditions of 65 degrees Celsius
Stirring is closed, while stirring, adds precipitating reagent thereto, precipitation obtains zirconium hydroxide, standby；
S5：By the zirconium hydroxide after being handled in S4, it is again placed in smelting furnace, and carried out under conditions of 525 degrees Celsius
Second melting, catalyst is then added into solution, and be mixed evenly, then filtered solution, after filtering, again
Concentration, crystallisation by cooling, crushing, roasting are evaporated, produces zirconium oxide.
Acid solution in S3 is nitric acid and one kind in sulfuric acid.
Precipitating reagent in S4 is oxalic acid, the mixture of ammonium hydrogen carbonate, ammoniacal liquor and sodium hydroxide, and oxalic acid, bicarbonate
The weight ratio of ammonium, ammoniacal liquor and sodium hydroxide is 1：0.5：1：0.5.
Smelting furnace in S2 inside smelting furnace before use, will need to be cleaned multiple times, then by the melting after cleaning
Stove is dried, and preheating 13min is carried out under conditions of 140 degrees Celsius.
Catalyst in S5 is zirconium nitrate solution, the mixed liquor of hexamethylenetetramine solution, and zirconium nitrate solution, six times
Tetramine solution molal weight ratio is 2：0.5.
Embodiment 3
The present invention proposes a kind of zirconium oxide production technology, comprises the following steps：
S1：Selection zircon is raw material, and zircon is carried out into repeated ultrasonic ripple cleaning, to remove the miscellaneous of zircon surface
Matter, then it is dried for standby；
S2：Zircon after being handled in S1 is placed in smelting furnace, and caustic soda is added into smelting furnace, at 650 degrees Celsius
Under conditions of melted, in fusion process, it need to be mixed in real time, to ensure that zircon mixes with caustic soda
It is even, after the completion for the treatment of melting, by hot water leaching melt liquid, the first mixed liquor is formed, it is standby；
S3：First mixed liquor of above-mentioned formation is placed in agitator, and its temperature is reduced to 375 degrees Celsius, then
Sodium zirconate is added thereto, and is stirred in real time, so as to be separated to the first mixed liquor, after the completion of separation, then thereto
Acid solution is added, obtains the second mixed liquor, and the second mixed liquor is placed in filter mechanism and removed the gred, it is standby after the completion of removal of impurities；
S4：The second mixed liquor after cleaning will be completed again to be placed in vessel, and is mixed under conditions of 70 degrees Celsius
Stirring is closed, while stirring, adds precipitating reagent thereto, precipitation obtains zirconium hydroxide, standby；
S5：By the zirconium hydroxide after being handled in S4, it is again placed in smelting furnace, and carried out under conditions of 550 degrees Celsius
Second melting, catalyst is then added into solution, and be mixed evenly, then filtered solution, after filtering, again
Concentration, crystallisation by cooling, crushing, roasting are evaporated, produces zirconium oxide.
Acid solution in S3 is nitric acid and one kind in sulfuric acid.
Precipitating reagent in S4 is oxalic acid, the mixture of ammonium hydrogen carbonate, ammoniacal liquor and sodium hydroxide, and oxalic acid, bicarbonate
The weight ratio of ammonium, ammoniacal liquor and sodium hydroxide is 1：0.5：1：0.5.
Smelting furnace in S2 inside smelting furnace before use, will need to be cleaned multiple times, then by the melting after cleaning
Stove is dried, and preheating 15min is carried out under conditions of 160 degrees Celsius.
Catalyst in S5 is zirconium nitrate solution, the mixed liquor of hexamethylenetetramine solution, and zirconium nitrate solution, six times
Tetramine solution molal weight ratio is 2：0.5.
Embodiment 4
The present invention proposes a kind of zirconium oxide production technology, comprises the following steps：
S1：Selection zircon is raw material, and zircon is carried out into repeated ultrasonic ripple cleaning, to remove the miscellaneous of zircon surface
Matter, then it is dried for standby；
S2：Zircon after being handled in S1 is placed in smelting furnace, and caustic soda is added into smelting furnace, at 675 degrees Celsius
Under conditions of melted, in fusion process, it need to be mixed in real time, to ensure that zircon mixes with caustic soda
It is even, after the completion for the treatment of melting, by hot water leaching melt liquid, the first mixed liquor is formed, it is standby；
S3：First mixed liquor of above-mentioned formation is placed in agitator, and its temperature is reduced to 420 degrees Celsius, then
Sodium zirconate is added thereto, and is stirred in real time, so as to be separated to the first mixed liquor, after the completion of separation, then thereto
Acid solution is added, obtains the second mixed liquor, and the second mixed liquor is placed in filter mechanism and removed the gred, it is standby after the completion of removal of impurities；
S4：The second mixed liquor after cleaning will be completed again to be placed in vessel, and is mixed under conditions of 75 degrees Celsius
Stirring is closed, while stirring, adds precipitating reagent thereto, precipitation obtains zirconium hydroxide, standby；
S5：By the zirconium hydroxide after being handled in S4, it is again placed in smelting furnace, and carried out under conditions of 575 degrees Celsius
Second melting, catalyst is then added into solution, and be mixed evenly, then filtered solution, after filtering, again
Concentration, crystallisation by cooling, crushing, roasting are evaporated, produces zirconium oxide.
Acid solution in S3 is nitric acid and one kind in sulfuric acid.
Precipitating reagent in S4 is oxalic acid, the mixture of ammonium hydrogen carbonate, ammoniacal liquor and sodium hydroxide, and oxalic acid, bicarbonate
The weight ratio of ammonium, ammoniacal liquor and sodium hydroxide is 1：0.5：1：0.5.
Smelting furnace in S2 inside smelting furnace before use, will need to be cleaned multiple times, then by the melting after cleaning
Stove is dried, and preheating 18min is carried out under conditions of 180 degrees Celsius.
Catalyst in S5 is zirconium nitrate solution, the mixed liquor of hexamethylenetetramine solution, and zirconium nitrate solution, six times
Tetramine solution molal weight ratio is 2：0.5.
Embodiment 5
The present invention proposes a kind of zirconium oxide production technology, comprises the following steps：
S1：Selection zircon is raw material, and zircon is carried out into repeated ultrasonic ripple cleaning, to remove the miscellaneous of zircon surface
Matter, then it is dried for standby；
S2：Zircon after being handled in S1 is placed in smelting furnace, and caustic soda is added into smelting furnace, at 700 degrees Celsius
Under conditions of melted, in fusion process, it need to be mixed in real time, to ensure that zircon mixes with caustic soda
It is even, after the completion for the treatment of melting, by hot water leaching melt liquid, the first mixed liquor is formed, it is standby；
S3：First mixed liquor of above-mentioned formation is placed in agitator, and its temperature is reduced to 450 degrees Celsius, then
Sodium zirconate is added thereto, and is stirred in real time, so as to be separated to the first mixed liquor, after the completion of separation, then thereto
Acid solution is added, obtains the second mixed liquor, and the second mixed liquor is placed in filter mechanism and removed the gred, it is standby after the completion of removal of impurities；
S4：The second mixed liquor after cleaning will be completed again to be placed in vessel, and is mixed under conditions of 80 degrees Celsius
Stirring is closed, while stirring, adds precipitating reagent thereto, precipitation obtains zirconium hydroxide, standby；
S5：By the zirconium hydroxide after being handled in S4, it is again placed in smelting furnace, and carried out under conditions of 600 degrees Celsius
Second melting, catalyst is then added into solution, and be mixed evenly, then filtered solution, after filtering, again
Concentration, crystallisation by cooling, crushing, roasting are evaporated, produces zirconium oxide.
Acid solution in S3 is nitric acid and one kind in sulfuric acid.
Precipitating reagent in S4 is oxalic acid, the mixture of ammonium hydrogen carbonate, ammoniacal liquor and sodium hydroxide, and oxalic acid, bicarbonate
The weight ratio of ammonium, ammoniacal liquor and sodium hydroxide is 1：0.5：1：0.5.
Smelting furnace in S2 inside smelting furnace before use, will need to be cleaned multiple times, then by the melting after cleaning
Stove is dried, and preheating 20min is carried out under conditions of 200 degrees Celsius.
Catalyst in S5 is zirconium nitrate solution, the mixed liquor of hexamethylenetetramine solution, and zirconium nitrate solution, six times
Tetramine solution molal weight ratio is 2：0.5.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (5)
1. a kind of zirconium oxide production technology, it is characterised in that comprise the following steps：
S1：Selection zircon is raw material, and zircon is carried out into repeated ultrasonic ripple cleaning, to remove the impurity on zircon surface,
Then it is dried for standby；
S2：Zircon after being handled in S1 is placed in smelting furnace, and caustic soda is added into smelting furnace, at 600-700 degrees Celsius
Under conditions of melted, in fusion process, it need to be mixed in real time, to ensure that zircon mixes with caustic soda
It is even, after the completion for the treatment of melting, by hot water leaching melt liquid, the first mixed liquor is formed, it is standby；
S3：First mixed liquor of above-mentioned formation is placed in agitator, and its temperature is reduced to 300-450 degrees Celsius, then
Sodium zirconate is added thereto, and is stirred in real time, so as to be separated to the first mixed liquor, after the completion of separation, then thereto
Acid solution is added, obtains the second mixed liquor, and the second mixed liquor is placed in filter mechanism and removed the gred, it is standby after the completion of removal of impurities；
S4：The second mixed liquor after cleaning will be completed again to be placed in vessel, and is mixed under conditions of 60-80 degrees Celsius
Stirring, while stirring, precipitating reagent is added thereto, precipitation obtains zirconium hydroxide, standby；
S5：By the zirconium hydroxide after being handled in S4, it is again placed in smelting furnace, and carried out under conditions of 500-600 degrees Celsius
Second melting, catalyst is then added into solution, and be mixed evenly, then filtered solution, after filtering, again
Concentration, crystallisation by cooling, crushing, roasting are evaporated, produces zirconium oxide.
A kind of 2. zirconium oxide production technology according to claim 1, it is characterised in that：Acid solution in S3 for nitric acid with
One kind in sulfuric acid.
A kind of 3. zirconium oxide production technology according to claim 1, it is characterised in that：Precipitating reagent in S4 is oxalic acid,
The mixture of ammonium hydrogen carbonate, ammoniacal liquor and sodium hydroxide, and oxalic acid, ammonium hydrogen carbonate, the weight ratio of ammoniacal liquor and sodium hydroxide are
1：0.5：1：0.5.
A kind of 4. zirconium oxide production technology according to claim 1, it is characterised in that：Smelting furnace in S2 is using
Before, it need to will be cleaned multiple times inside smelting furnace, then be dried the smelting furnace after cleaning, and at 120-200 degrees Celsius
Under conditions of carry out preheating 10-20min.
A kind of 5. zirconium oxide production technology according to claim 1, it is characterised in that：Catalyst in S5 is zirconium nitrate
The mixed liquor of solution, hexamethylenetetramine solution, and zirconium nitrate solution, hexamethylenetetramine solution molal weight ratio are 2：0.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711213792.0A CN107892327A (en) | 2017-11-28 | 2017-11-28 | A kind of zirconium oxide production technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711213792.0A CN107892327A (en) | 2017-11-28 | 2017-11-28 | A kind of zirconium oxide production technology |
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| CN107892327A true CN107892327A (en) | 2018-04-10 |
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ID=61806838
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711213792.0A Pending CN107892327A (en) | 2017-11-28 | 2017-11-28 | A kind of zirconium oxide production technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108636406A (en) * | 2018-04-24 | 2018-10-12 | 方嘉城 | A method of preparing high activity Cu-Zr catalyst using zirconia ball abrasive dust |
-
2017
- 2017-11-28 CN CN201711213792.0A patent/CN107892327A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 刘胜新: "《化验员手册》", 31 March 2014, 机械工业出版社 * |
| 陈肇友: "《相图与耐火材料》", 31 October 2014, 冶金工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108636406A (en) * | 2018-04-24 | 2018-10-12 | 方嘉城 | A method of preparing high activity Cu-Zr catalyst using zirconia ball abrasive dust |
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