CN104628382B - Reclaim the processing method that feeding injected by zirconia ceramics - Google Patents
Reclaim the processing method that feeding injected by zirconia ceramics Download PDFInfo
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- CN104628382B CN104628382B CN201410550435.3A CN201410550435A CN104628382B CN 104628382 B CN104628382 B CN 104628382B CN 201410550435 A CN201410550435 A CN 201410550435A CN 104628382 B CN104628382 B CN 104628382B
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Abstract
The invention provides a kind of reclaim the processing method that feeding injected by zirconia ceramics, including：Zirconia ceramics injection feeding is carried out low temperature calcination under ozone atmosphere, obtains zirconia ceramics powder；Wherein low temperature is 200～300 DEG C for condition；Zirconia ceramics powder after calcining is carried out ball-milling treatment, obtains dispersed paste；Dispersed paste is carried out iron removal by magnetic separation；Slurry after iron is dried.Using the above-mentioned steps method of the present invention, calcined by odor at low temperature and ball milling and removal of impurities process, it is to avoid the Zirconium powder activity reduction problem that the aging and high-temperature calcination of polymer that feeding Long-Time Service is produced is caused；While realizing removing impurity in rear injection moulding feeding is used for multiple times, zirconic activity and quality is substantially ensure that, improves the utilization rate of resource.
Description
Technical field
The invention belongs to zirconia ceramics technical field, and in particular to the process of feeding injected by a kind of recovery zirconia ceramics
Method.
Background technology
Zirconia ceramics is widely used in various products production, such as fiber stub, watch chain, watch case and each
Plant jewellery etc..In production for wherein shaped piece, zirconium oxide mainly uses injection molding method；Wherein, when
The obtained injection feeding of zirconium oxide powder after a number of uses, can produce polymer aging (mobility reduction), volatilization, iron tramp
Etc. phenomenon, the quality of subsequent product is affected.
And be directed to said circumstances, existing conventional method be by freshly prepd injection feeding with reuse after old material by
After certain ratio mixing, it is continuing with.This method is convenient and simple, can greatly save aging feeding, to a certain degree reduce
The aging impact of polymer volatilization.But for zirconia ceramics, the impurity being mixed in being used for multiple times is inevitable, for
The impact that final products quality reduces cannot be eliminated all the time.
Content of the invention
The above-mentioned deficiency for aiming to overcome that prior art of the embodiment of the present invention, provides one kind by nonexpondable
Injection feeding reclaims white silk again and makes, and the feeding identical in quality with the injection feeding of new mixing is obtained.
In order to realize foregoing invention purpose, the technical scheme of the embodiment of the present invention is as follows：
A kind of processing method for reclaiming zirconia ceramics injection feeding, comprises the steps：
Zirconia ceramics injection feeding is carried out low temperature calcination under ozone atmosphere, obtains zirconia ceramics powder；
The zirconia ceramics powder after calcining is carried out ball-milling treatment, obtains dispersed paste；
The dispersed paste is carried out iron removal by magnetic separation；
Slurry after iron is dried；
During wherein described low temperature calcination, calcining heat controls 200～300 DEG C.
Using the above-mentioned steps method of the present invention, calcined by odor at low temperature and ball milling and removal of impurities process, it is to avoid
The Zirconium powder activity reduction problem that the aging and high-temperature calcination of polymer that feeding Long-Time Service is produced is caused；Realize removing many
Secondary using in rear injection moulding feeding while impurity, substantially ensure that zirconic activity and quality, improve resource
Utilization rate.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only in order to explain the present invention
Limit the present invention.
The embodiment of the present invention provides a kind of processing method for reclaiming zirconia ceramics injection feeding, comprises the steps：
S10, zirconia ceramics injection feeding is carried out low temperature calcination under ozone atmosphere, obtains zirconia ceramics powder；
S20, the zirconia ceramics powder after calcining is carried out ball-milling treatment, obtains dispersed paste；
S30, the slurry after ball milling is passed through iron removal by magnetic separation；
S40, the slurry after iron is dried.
Injection feeding after the above-mentioned steps of the present invention are integrally to be used for multiple times is reclaimed again, and is carried out activating, removed
Miscellaneous grade is processed, and is finally given and the injection feeding feeding identical in quality for newly kneading.
Wherein, zirconia ceramics injection feeding is carried out low temperature calcination first in above-mentioned steps S10, the step is intended that
The organic matter in feeding is made to resolve into the release such as water and carbon dioxide by calcining；And temperature exists during commonly calcining
800～1000 DEG C, powder reuniting, aging degree can be caused to deepen, activity reduces；Even if subsequently opening group by ball milling again
Poly-, in product sintering, activity can also reduce, and final products sintering is not fine and close, and improving sintering temperature can make crystal grain extremely long
Greatly.
Therefore in this situation, in the present invention using low temperature 200～300 DEG C calcined, and the process that calcines in
Carry out under ozone atmosphere.Zirconia powder itself is all the superfine powder for being close to Nano grade, the process of low temperature calcination can reduce reunion,
Aging degree, while carry out during calcining in ozone atmosphere；In the ozone atmosphere of strong oxidizing property, can promote to have
The oxidation Decomposition of machine thing, it is to avoid the generation of carbon black impurity under high temperature；And the oxygen radical of ozone or active oxygen are additionally aided
Improve zirconic activity.Therefore calcined using the combination of low temperature of the present invention and ozone, the activity of powder and organic
Thing is removed all optimized can be carried out.Make to only exist in its powder sintering a certain degree of soft-agglomerated, final realize adopting ball milling
Can open.And the process time that further preferably calcines controls 1～5 hour, makes process cycle, product efficiency and quality
Energy Efficiency Ratio is maximum.
The mode for calcining in step S10 being obtained zirconia ceramics powder direct kick mill in step S20 further enters one
Step is refined as ultra-fine nanometer grade powder.And in this step, during the ball milling, details controls the condition of ball milling,
Using being 1 according to zirconia ceramics powder and material ball ratio:1～3 carries out pellet mixing, and zirconia ceramics powder with water solid-liquid ratio is
1:0.5～1.5 adds water, and adds PEG, PVA, ammonium polyacrylate in the 0.5～5% of zirconia ceramics powder quality fraction ratio
One or more as Organic Grinding Aid, while adjust pH value 7～14 with ammoniacal liquor, and using addition be amount of water 0.1～
0.5% glycerine is used as the defoamer in mechanical milling process, ball milling 6～72 hours.
By carrying out ball milling in the environment of meta-alkalescence, it is ensured that the oxide morphology of powder and particle activity, and by upper
State the organic polymer grinding aid lifting ball milling effect of PEG, PVA, ammonium polyacrylate.
After ball milling dispersion, step S30 carries out the slurry after ball milling except iron, can be directly using circulation during this
Magnetic separator de-ironing is carried out, and whenabouts can be completed except iron for 2～10 hours.The present invention is become according to material using magnetic separator de-ironing during this
The difference of magnetic in point, irony is removed by the differential separation of magnetic；Carried out using physics mode, it is to avoid chemical subtraction method
Step is complicated, and can destroy the shortcoming of zirconium oxide active.
After iron tramp is removed, the slurry after iron is dried in final step S40, directly permissible during this
Carry out by the way of heat is dried, dry within 2～24 hours at a temperature of 40～100 DEG C of control condition；Obtain after drying
The higher zirconia ceramics reclaimed materials of quality.Different according to the required situation for using, such as can be by obtained zirconia ceramics
Granulation after reclaimed materials directly adds new organic binder bond mixing becomes pelletizing compacting use；Or can directly will be obtained
Zirconia ceramics reclaimed materials air-flow crushing becomes air-flow powder, is subsequently used for production injection feeding.
Using the above-mentioned steps method of the present invention, calcined by odor at low temperature and ball milling and removal of impurities process, it is to avoid
Zirconium powder activity reduces and polymer problem of aging；Realize removing and the same of impurity in rear injection moulding feeding is used for multiple times
When, zirconic activity and quality is substantially ensure that, improves the utilization rate of resource.
It is readily appreciated by one skilled in the art and real for enabling the embodiment of the above-mentioned details of the present invention and the progress of effect to be easier
Apply, the recovery method of the zirconia ceramics injection moulding feeding of the present invention is illustrated below by way of multiple embodiments：
Embodiment 1
In the embodiment 1, taken from ceramic injection machine in prepared by different product by several times and inject not using complete zirconium oxide
Ceramic injection feeding 800g carries out following steps：
S10, by the zirconium oxide injection moulding feeding for obtaining with after saggar splendid attire, inserts in vacuum drying oven；Then in vacuum drying oven
In be passed through ozone until vacuum drying oven in ozone concentration be more than 80%；Then carry out 200 DEG C are heated to, be persistently incubated 5
Hour；After the completion of lower the temperature blow-on, take out obtain zirconia ceramics powder, be weighed as 694g；
S20, the zirconia ceramics powder that step S10 is obtained are placed in ball grinder and carry out ball-milling treatment, add in ball milling
Material is as follows：
The ball milling bead of about 2 times of zirconia ceramics powders is added, 500ml distilled water, PEG, PVA, ammonium polyacrylate are each
10g, forms slurries；Adjusted after slurry pH value 7.5 with ammoniacal liquor, add 2.2g glycerine froth breaking；Then ball milling 12 hours, are divided
Scattered slurry；
S30, by the slurry after ball milling in magnetic separation iron remover circulation deferrization 5 hours；
S40, will except the slurry after iron 40 DEG C in the baking oven at a temperature of dry within 18 hours, that is, obtain zirconia ceramics recovery
Material.
Then by the zirconia ceramics reclaimed materials add again binding agent carry out granulation become pelletizing compacting using prepare
Ceramic product.
Embodiment 2
In the embodiment 2, taken from ceramic injection machine in prepared by different product by several times and inject not using complete zirconium oxide
Ceramic injection feeding 700g carries out following steps：
S10, by the zirconium oxide injection moulding feeding for obtaining with after saggar splendid attire, inserts in vacuum drying oven；Then in vacuum drying oven
In be passed through ozone until vacuum drying oven in ozone concentration be more than 85%；Then carry out 300 DEG C are heated to, be persistently incubated 1
Hour；After the completion of lower the temperature blow-on, take out obtain zirconia ceramics powder, be weighed as 572g；
S20, the zirconia ceramics powder that step S10 is obtained are placed in ball grinder and carry out ball-milling treatment, add in ball milling
Material is as follows：
Add the ball milling bead of about 2.5 times of zirconia ceramics powders, 450ml distilled water, PEG15g, formation slurries；Use ammonia
After water adjusts slurry pH value 8, add 2g glycerine froth breaking；Then ball milling 48h, obtains dispersed paste；
S30, by the slurry after ball milling in magnetic separation iron remover circulation deferrization 10 hours；
S40, will except the slurry after iron 100 DEG C in the baking oven at a temperature of dry within 5 hours, that is, obtain zirconia ceramics recovery
Material.
Then the zirconia ceramics reclaimed materials airflow milling is ground into air-flow powder, being subsequently used for production injection feeding is carried out
Prepare ceramic product.
Embodiment 3
In the embodiment 3, taken from ceramic injection machine in prepared by different product by several times and inject not using complete zirconium oxide
Ceramic injection feeding 750g carries out following steps：
S10, by the zirconium oxide injection moulding feeding for obtaining with after saggar splendid attire, inserts in vacuum drying oven；Then in vacuum drying oven
In be passed through ozone until vacuum drying oven in ozone concentration be more than 90%；Then carry out 250 DEG C are heated to, be persistently incubated 3
Hour；After the completion of lower the temperature blow-on, take out obtain zirconia ceramics powder, be weighed as 545g；
S20, the zirconia ceramics powder that step S10 is obtained are placed in ball grinder and carry out ball-milling treatment, add in ball milling
Material is as follows：
The ball milling bead of about 2 times of zirconia ceramics powders is added, 350ml distilled water, 5gPEG, 5g PVA form slurries；With
After ammoniacal liquor adjusts slurry pH value 10, add 1g glycerine froth breaking；Then ball milling 20 hours, obtain dispersed paste；
S30, by the slurry after ball milling in magnetic separation iron remover circulation deferrization 5 hours；
S40, will except the slurry after iron 40 DEG C in the baking oven at a temperature of dry within 18 hours, that is, obtain zirconia ceramics recovery
Material.
Then the zirconia ceramics reclaimed materials airflow milling is ground into the air-flow powder of nanoscale fineness, encapsulation is preserved, standby
With.
By above-described embodiment 1-2 with using after being used for multiple times injection feeding mix with virgin material after, according to same product
Preparation process, carries out the contrast of product preparation with the powder that reclaims of embodiment 1-2, and its result is as follows：
Rough Statistics contrast on result product yield from upper table, as the processing mode of powder is different, using this Shen
Please ozone low temperature calcination mode, make the lifting of powder active, the performance and yields for final products has obviously
Lifting and improvement.
Presently preferred embodiments of the present invention is the foregoing is only, not in order to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement that is made within god and principle etc., all should be included within protection scope of the present invention.
Claims (7)
1. the processing method of feeding injected by a kind of recovery zirconia ceramics, it is characterised in that comprise the steps：
Zirconia ceramics injection feeding is carried out low temperature calcination under ozone atmosphere, obtains zirconia ceramics powder；
The zirconia ceramics powder after calcining is carried out ball-milling treatment, obtains dispersed paste；
The dispersed paste is carried out iron removal by magnetic separation；
Slurry after iron is dried；
During wherein described low temperature calcination, calcining heat controls 200～300 DEG C.
2. the processing method of feeding injected by recovery zirconia ceramics as claimed in claim 1, it is characterised in that described by calcining
The zirconia ceramics powder afterwards is carried out in ball-milling treatment step, by the zirconia ceramics powder and pellet, water, has machine aided
Grinding agent, glycerine mixing are simultaneously adjusted after pH to 7～14 with ammoniacal liquor, carry out ball milling.
3. the processing method of feeding injected by recovery zirconia ceramics as claimed in claim 2, it is characterised in that by the oxidation
Zircon ceramic powder is mixed with pellet, water, Organic Grinding Aid, glycerine and is adjusted after pH to 7～14 with ammoniacal liquor, carries out ball milling
In step, it is 1～3 according to the pellet addition and zirconia ceramics powder body weight ratio：1 adds pellet；And according to described
Zirconia ceramics powder is 1 with the weight ratio of water:0.5～1.5 adds water；
The addition of the glycerine is the 0.1～0.5% of the water quality；
The addition of the Organic Grinding Aid is the 0.5～5% of the zirconia ceramics powder quality fraction.
4. the processing method of feeding injected by recovery zirconia ceramics as claimed in claim 2 or claim 3, it is characterised in that described have
Machine aided grinding agent is PEG, PVA, at least one in ammonium polyacrylate.
5. the processing method of feeding injected by the recovery zirconia ceramics as described in any one of claims 1 to 3, it is characterised in that
During the low temperature calcination, calcination time is 1～5 hour.
6. the processing method of feeding injected by recovery zirconia ceramics as claimed in claim 3, it is characterised in that the ball milling mistake
The journey time is 6～72 hours.
7. the processing method of feeding injected by recovery zirconia ceramics as claimed in claim 1 or 2, it is characterised in that the general
Except the slurry after iron is dried in step, dried using 2～24 hours at a temperature of 40～100 DEG C.
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| CN106220148A (en) * | 2016-07-08 | 2016-12-14 | 苏州珂玛材料技术有限公司 | A kind of aluminium oxide ceramics green compact feed back processing method |
| CN107377867B (en) * | 2017-08-22 | 2019-10-18 | 汉川市石金科技有限公司 | A kind of steel moulder's paint and preparation method thereof |
| CN112517902B (en) * | 2019-09-17 | 2021-11-19 | 江苏骏派电子科技有限公司 | Recovery method of metal injection molding waste |
| CN116082036A (en) * | 2022-07-19 | 2023-05-09 | 广东爱斯库生物材料有限公司 | Zirconia recovery method and application thereof |
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| CN100515997C (en) * | 2007-06-08 | 2009-07-22 | 湖南正阳精密陶瓷有限公司 | Zirconia injection molding process |
| US8940256B2 (en) * | 2011-12-07 | 2015-01-27 | Xylon Technical Ceramics, Inc. | Method for recycling of rare earth and zirconium oxide materials |
| CN102531588B (en) * | 2012-03-03 | 2015-01-14 | 虔东稀土集团股份有限公司 | Method for preparing zirconium oxide ceramic by recycling zirconium oxide ceramic grinding wastes |
| CN102701279B (en) * | 2012-06-15 | 2013-07-03 | 深圳爱尔创科技股份有限公司 | Aftertreatment method for doped nano-zirconia powder |
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Address after: 518000, Shenzhen, Guangdong province Baoan District manhole street new two community Nanling Road, No. 21, B building on the first floor, two floor Patentee after: Shenzhen City, Germany and advanced ceramics Limited by Share Ltd Address before: 518000 Guangdong city of Shenzhen province Baoan District manhole street two community Nanling Road No. 21 building two floor B Patentee before: Shenzhen Shangde Advanced Ceramic Co., Ltd. |
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