CN105198476A - Preparation method of inorganic porous ceramic membrane - Google Patents
Preparation method of inorganic porous ceramic membrane Download PDFInfo
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Abstract
The invention relates to a preparation method of an inorganic porous ceramic membrane. The preparation method includes the following steps: weighing, namely weighing raw materials, a pore former and a sintering aid according to a certain proportion, and mixing them; wet-grinding and dry-grinding a mixture; pelleting a resulting product; performing compression moulding forming; sintering a formed product. Made ceramic has the advantages of large flux, high compressive strength and high reproducibility, and the ceramic membrane is uniform in porosity; the inorganic porous ceramic membrane has the advantages of resistance to high temperature and acid and alkali corrosion, high compressive strength, high reproducible utilization rate and freeness of secondary pollution. Rates of removing COD, oil and suspended solid in water are 82.3%, 85.3% and 89.6% respectively, and good deoiling effect can be realized. A modified ceramic membrane is back-washed under a washing condition of 0.05MPa for reproduction, and clean water flux of the modified ceramic membrane can be restored to 94.7%.
Description
Technical field
The invention belongs to environmental protection technical field, be specifically related to a kind of preparation method of inorganic porous ceramic film.
Background technology
In water technology, ceramic membrane has the many merits such as separation efficiency is high, effect stability, chemical stability are good, acid and alkali-resistance, organic solvent-resistant, resistance to bacterium, high temperature resistant, antipollution, physical strength are high, film regenerability is good, sepn process is simple, energy consumption is low, simple and convenient operation and maintenance, film long service life, be subject to a large amount of favors, be widely used in water treatment applications;
(1) process oily(waste)water: the oily(waste)water that all can produce different properties, different content in industries such as oil, machinery and food food and drink, the utilization of process oily(waste)water be the microvoid structure of ceramic membrane inside, oil droplet is separated with water.In cold rolling wastewater process, inorganic ceramic film and organic membrane are contrasted, the treatment effect of both discoveries is suitable, but ceramic membrane demonstrates its absolute advantage in working cost.
(2) process petrochemical wastewater: usually can produce in chemical industry and petroleum chemical industry some have strong acid, highly basic or severe corrosive containing particle waste water; organic membrane is often difficult to be competent at; and mineral membrane is due to the chemical stability of its excellence, when processing these waste water, there is certain advantage.
(3) reverse osmosis seawater desalting pre-treatment: in seawater desalinization pretreatment system, introduce ceramic membrane treatment technology, utilize the micro-filtration performance of ceramic membrane, the pre-treatment for sea water desaltination provides new method.
(4) drink water purifying: utilize microporous membrane to carry out the process of surface water.Its main advantage has can ensure better and more reliable water quality, does not add chemical substance.Be specially adapted to high value added product.
(5) in treatment of dyeing and printing and heavy metal wastewater thereby: a large amount of pollutent of oil-containing in dyeing waste water, mainly contains: suspended substance, BOD, COD, SYNTHETIC OPTICAL WHITNER, heavy metal (as lead, chromium etc.) and colourity etc., intractability is relatively large.Ceramic membrane dynamic filtration technology and flocculation technique are combined, is then applied in waste water from dyestuff and bleaching and dyeing wastewater and processes, find advantage and the advantage that fully can demonstrate dynamic filtration and ceramic membrane like this, treatment effect is quite remarkable.
The preparation of ceramic membrane in the past mainly contains following: (1) Polymeric sponge method; The people such as Schwartzwalder in 1963 adopt organic foam plastic infused ceramic slurry the earliest, burn organic foam, be prepared into porous ceramics after drying.Tsing-Hua University utilized the method to prepare void content is 70 ~ 80%, its mean pore size is greatly about the porous hydroxyapatite of 200 ~ 300 μm; Xi'an Communications University mixes as ceramic slurry using biological glass powder and hydroxylapatite powder, adopt silicon sol as solvent and binding agent, Walocel MT 20.000PV, as rheological agent, has prepared aperture between 450 ~ 500 μm and the multiporous biological active ceramic that communicates of hole by the method.The three-dimensional netted skeleton structure of special drilling type that the method relies on organic foam to have, is coated on organic reticulate body equably by ceramic size, obtains the porous ceramic film material with mesh-type ventilate after the sintering.With the porous ceramics that the method prepares, void content can up to 70 ~ 90%.The method preparation-obtained pore shape is close to identical with the structure of organic foam presoma used, and size also depends primarily on the pore dimension of the organic foam of employing, and relevant with the drying of the coating thickness on parent and slurry and sintering shrinkage.
(2) sol-gel method; Sol-gel method (sol-gel) is mainly applicable to prepare aperture tiny microporous membrane, particularly nano level ceramic membrane, and the product obtained by the method has high regularity.Its basic preparation process is as follows: be dissolved in the middle of lower alcohol by the alkoxide of metal, instills water droplet gradually with the reaction that is hydrolyzed, then obtains the colloidal sol of corresponding metal oxide; Further adjust ph size, makes organism produce polyreaction, flocks together, form the gel of amorphous network structure between oxide particle, dry, gets rid of organism, just obtains porous ceramic film after sintering.With the aperture that sol-gel method obtains, aperture is approximately all nano level, the size and surface-area etc. of control punch is come by the potential of hydrogen of regulator solution, it can improve the control of porous ceramic film pore size distribution, phase transformation and microstructure, but due to the unbodied polyreaction of organism, cause the shape of goods to be not easy to control.
(3) granulation mass area method; Ceramic membrane particle is generally have difform geometry polyhedron, and it piles up the structure getting up can be formed porous.Can in ceramic membrane aggregate, add the ceramic fine particle of same composition or add binding agent thus aggregate is coupled together.Because fine particle is easily sintered together, so macrobead aggregate sintering can be got up at a certain temperature.The people such as Wu Daozheng are by adopting SiO
2-Al
2o
3-R
2o-RO (R refers to organic group) as binding agent, the liquid phase at high temperature produced by it, thus the α-Al of certain particle size
2o
3aggregate bonds mutually, its research draws: pile up for isometrical spheroid, void content and granular size have nothing to do, and it is relevant with the mode of piling up, aggregate particles distribution is narrower, the void content value obtained is larger, and aperture is also more even, its sintering temperature should be selected in higher than binding agent melt temperature but lower than particle sintering temperature in.
(4) pore-forming material method is added; By adding pore-forming material, in sintering process, forming due to the volatilization carbonization of pore-forming material the hole communicated with each other in a large number in inside, thus larger molecular organics is separated with water.This method is by adding volatility or flammable pore-creating material in ceramic batch, utilizing these materials volatilize at a certain temperature or burn, and then leave hole in ceramic body.Utilize the method can obtain complex-shaped and that pore structure is different porous material, its key is to select the type of pore-forming material, size and consumption.
(5) solid particles sintering process; Solid particles sintering process is mixed with medium by inorganic powder, forms stable suspension, then suspension is become Homogeneous phase mixing powder through art breading, and powder makes green compact through technique, then drying, finally at high temperature thermal sintering.Solid particles sintering process is exactly that briquet is placed on thermally equivalent in suitable environment, through a series of physical and chemical changes, viscosity between powder granule changes, along with the continuation of temperature is risen, contraction due to briquet causes physical strength and density to increase, and in briquet, mixing of pore-forming material makes system total energy in sintering process reduce.In sintering process, under number of mechanisms acting in conjunction, briquet changes to stable state.In order to make particle itself change completely to stable state, need to be heated to certain temperature.In sintering process, the temperature rise rate of the physical strength of finished product and performance and sintering, sintering temperature, soaking time and rate of cooling all have much relations.Due to ceramic film support intensity and porosity, between pore size and shrinking percentage etc., itself there is restrictive function, so suitable sintering method can only be selected, so just can avoid product defects, and obtain support body material of good performance.
In sum, adopt that the pottery membrane flux prepared of previous methods is little, ultimate compression strength is low, also lower to COD in water body, oleaginousness, suspended solids content clearance.
Summary of the invention
The technical problem to be solved in the present invention is: overcome the deficiencies in the prior art, provides a kind of preparation method of inorganic porous ceramic film, solves the defect that the ceramic membrane oil removal rate in the past prepared is low.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of inorganic porous ceramic film, comprises the following steps:
1., weigh: raw material, pore-forming material, sintering aid are weighed according to certain ratio, and mix; Described raw material choose diatomite, described pore-forming material comprises sawdust, Graphene and CaCO
3, described sintering aid is TiO2;
2., wet-milling: choose ball mill, load weighted material, agate bead and distilled water are together loaded in ball mill, the ratio of material, agate bead and distilled water is 2:1:1, and described material comprises raw material, pore-forming material, sintering aid, fully rotate through ball mill, make material grind evenly;
3., dry grind: the liquid in ball mill is filtered through screen cloth, obtain material liquid, then material liquid is put into oven for drying, material liquid puts into ball mill after having dried together with agate bead, ratio between agate bead and material is 2:1, relies on ball mill again to grind evenly to material;
4., granulation: screen out agate bead through screen cloth, take out material powders and also load in beaker, add appropriate distilled water, limit edged is stirred to powder and darkens and have and form block; Then in 60 object sieve granulations, by pressurizeing crushed for powder 60 mesh sieve with hand, the powder after crushed is placed in culture dish ageing;
5., compression molding: select electro-hydraulic servo universal press, the material measuring ageing is placed in mould, and electro-hydraulic servo universal press works, and makes compact formation, needs to ensure full pressure 3min after each malleation and back-pressure;
6., sintering: after ceramic membrane compacting, film base is put into baking oven and dry 24h and all volatilize to the moisture of film base.
Further, described TiO
2content is 1% of material total amount, and described pore-forming material is 35% of material total amount; Sawdust in described pore-forming material: Graphene: the component ratio of calcium carbonate is 2:2:1.
Further, described step 6. in sintering comprise four-stage, front three phases is carbonization volatilization period, and fourth stage is the sinter molding stage;
First stage: be warming up to 340 DEG C, and be incubated 0.5h; Subordinate phase: be warming up to 600 DEG C, and be incubated 1h, the phase III: be warming up to 780 DEG C, and be incubated 0.5h; Fourth stage: be warming up to 1100 DEG C, and be incubated 0.5h.
Further, described step 2. in, during ball milling, rotating speed is 220r/min, it is a ball milling cycle with 50min, have in each cycle and rotate forward grinding and reversion grinding two portions, each 20min respectively, can suspend 10min after 40min running, then manually start the grinding of next cycle, milling time carries out 4 cycles.
Further, described step 3. in, the rotating speed of dry grinding is 220r/min, 50min is a ball milling cycle, and each cycle has to rotate forward grinding and reverse grinds each 20min, after 40min running, suspend 10min, then the grinding of next cycle is manually started, dry grinding 2 cycles of grinding.
Further, described step 5. in, positive pressure pressure is 11kN, and back-pressure pressure is 13kN.
The invention has the beneficial effects as follows: obtained pottery has that flux is large, ultimate compression strength is high, recyclability is good, and ceramic membrane porosity is even; Inorganic ceramic film has high temperature resistant, the feature such as acid-alkali-corrosive-resisting performance is good, ultimate compression strength is high, reproducible utilization rate is high, non-secondary pollution.82.3%, 85.3% and 89.6% is respectively to COD in water body, oleaginousness, suspended solids content clearance, good deoiling effect can be reached; Modified ceramic film carries out back flushing regeneration under 0.05MPa washing conditions, and its clear water flux can return to 94.7%.
Inorganic modified ceramic membrane performance analysis and sign display, it is narrow that this ceramic membrane has aperture, is evenly distributed, separation efficiency high.Belong to microfiltration membrane, effectively can remove the pollution substance such as oils in water body, the process being applied to oily(waste)water is feasible.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further described.
In Fig. 1 ceramic membrane, sawdust and Graphene content are on the schematic diagram of the impact of porosity;
Sawdust and CaCO in Fig. 2 ceramic membrane
3content is on the schematic diagram of the impact of porosity;
Graphene and CaCO in Fig. 3 ceramic membrane
3content is on the schematic diagram of the impact of porosity
Embodiment
The present invention is further illustrated in conjunction with specific embodiments now.The schematic diagram that these accompanying drawings are simplification only illustrates basic structure of the present invention in a schematic way, and therefore it only shows the formation relevant with the present invention.
A preparation method for inorganic porous ceramic film, comprises the following steps:
1., weigh: raw material, pore-forming material, sintering aid are weighed according to certain ratio, and mix; Described raw material choose diatomite, described pore-forming material comprises sawdust, Graphene and CaCO
3, sintering aid is TiO
2;
2., wet-milling: choose ball mill, load weighted material, agate bead and distilled water are together loaded in ball mill, the ratio of material, agate bead and distilled water is 2:1:1, and material comprises raw material, pore-forming material, sintering aid, fully rotate through ball mill, make material grind evenly;
During ball milling, rotating speed is 220r/min, is a ball milling cycle with 50min, has rotate forward grinding and reversion grinding two portions in each cycle, each 20min respectively, can suspend 10min after 40min running, then manually start the grinding of next cycle, milling time carries out 4 cycles.
3., dry grind: the liquid in ball mill is filtered through screen cloth, obtain material liquid, then material liquid is put into oven for drying, material liquid puts into ball mill after having dried together with agate bead, ratio between agate bead and material is 2:1, relies on ball mill again to grind evenly to material;
The rotating speed of dry grinding is 220r/min, 50min is a ball milling cycle, and each cycle has to rotate forward grinding and reverse grinds each 20min, suspends 10min, then manually starts the grinding of next cycle, dry grinding 2 cycles of grinding after 40min running.
4., granulation: screen out agate bead through screen cloth, take out material powders and also load in beaker, add appropriate distilled water, limit edged is stirred to powder and darkens and have and form block; Then in 60 object sieve granulations, by pressurizeing crushed for powder 60 mesh sieve with hand, the powder after crushed is placed in culture dish ageing.
5., compression molding: select electro-hydraulic servo universal press, the material measuring ageing is placed in mould, and electro-hydraulic servo universal press works, and makes compact formation, needs to ensure full pressure 3min after each malleation and back-pressure; Positive pressure pressure is 11kN, and back-pressure pressure is 13kN.
6., sintering: after ceramic membrane compacting, film base is put into baking oven and dry 24h and all volatilize to the moisture of film base.
Sintering comprises four-stage, and front three phases is carbonization volatilization period, and fourth stage is the sinter molding stage; First stage: be warming up to 340 DEG C, and be incubated 0.5h; Subordinate phase: be warming up to 600 DEG C, and be incubated 1h, the phase III: be warming up to 780 DEG C, and be incubated 0.5h; Fourth stage: be warming up to 1100 DEG C, and be incubated 0.5h.
Graphene is very fast 600 DEG C of place's heat absorption volatilizations, therefore needs to be incubated 1h.After sintering terminates, close baking oven power supply, allow temperature in baking oven slowly fall, at this moment can't to take the method cooling of directly opening fire door, otherwise may cause hold baking oven instantaneously health is damaged and with the air meeting of contact and the too fast division causing ceramic membrane of lowering the temperature.Because the temperature of ceramic membrane sintering is when reaching 1200 DEG C, ceramic membrane shrinking percentage can become large, there is the phenomenon of distortion and bonding, than being easier to fracture and color is comparatively dark, section is smooth stone planar, has very bright gloss, representing fractures is because the fracture of crystal grain itself, the defect that crystal grain itself is existing a lot of is described, the hole of inside configuration is fully sintered extremely, cannot for the treatment of water.So show that test selects 1100 DEG C to sinter.
TiO
2content is 1% of material total amount, and pore-forming material is 35% of material total amount; Sawdust in pore-forming material: Graphene: the component ratio of calcium carbonate is 2:2:1.
Porosity, refers to the volume of sample mesoporosity and the long-pending percentage of sample population.As shown in Figure 1, when calcium carbonate content is 10%, along with the increase of sawdust content, originally porosity is reduce, but along with the increase of sawdust content, situation there occurs transformation, and porosity increases thereupon; This is because pore-forming material sawdust main chemical compositions is made up of C, H, when massfraction is less than 7.5%, the space that pore-forming material occupies is less than base substrate particle itself and piles up the hole formed at random, therefore the increase of pore-forming material sawdust is little to Porosity Rate Influence, the contrary rising due to temperature now, the contraction change of base substrate is greater than the formation of hole, and the porosity therefore when massfraction is less than 7.5% reduces; When sawdust massfraction is greater than 7.5%, the hole piled up between base substrate particle is not enough to hold the space needed for pore-forming material, and the distribution serialization transition of pore-forming material, thus porosity significantly increases, and the hole now formed obviously is greater than the contraction change of base substrate.Along with the increase of Graphene content, originally porosity is also reduce, but along with the increase of Graphene content, porosity starts to increase.Wherein, porosity maximum value is 46.5%, and the sawdust content at this some place is 15%, and Graphene content is 10%.
As shown in Figure 2, when Graphene content is 10%, along with the increase of sawdust content, originally porosity reduces, and along with the continuation of sawdust content increases, porosity is increase tendency.Along with the increase of calcium carbonate content, originally porosity increases thereupon, and when waiting calcium carbonate content to reach 10%, porosity reaches maximum, and subsequently along with the increase of calcium carbonate content, porosity reduces on the contrary.Calcium carbonate at high temperature volatile carbon changes into calcium oxide and carbonic acid gas.Can obtain porosity maximum value from figure is 46.5%, now sawdust content 15%, calcium carbonate content 10%.
As shown in Figure 3, when sawdust content is 10%, along with the increase of Graphene content, originally porosity reduces, but increases along with the continuation of sawdust content, and porosity is increase tendency; This is because pore-forming material Graphene main chemical compositions is C, when massfraction is less than 6%, the space that pore-forming material occupies is less than base substrate particle itself and piles up the hole formed at random, therefore the increase of pore-forming material Graphene is little to Porosity Rate Influence, the contrary rising due to temperature now, the contraction change of base substrate is greater than the formation of hole, and the porosity therefore when massfraction is less than 6% reduces; When sawdust massfraction is greater than 6%, the hole piled up between base substrate particle is not enough to hold the space needed for pore-forming material, and the distribution serialization transition of pore-forming material, thus porosity significantly increases, and the hole now formed obviously is greater than the contraction change of base substrate.And along with the increase of calcium carbonate content, originally porosity increases, and when waiting calcium carbonate content to reach 10%, porosity reaches maximum, and subsequently along with the increase of calcium carbonate content, porosity reduces on the contrary thereupon.As can be seen from the figure porosity maximum value is 39.5%, and now Graphene content is 15%, and calcium carbonate content is 10%.Utilize Design-Expert software to be optimized, obtain top condition: sawdust content 20%, Graphene content 20%, calcium carbonate content 11.21%, porosity is 56.9% to the maximum.
At top condition sawdust content: Graphene content: calcium carbonate content=20%:20%:11.21% ≈ 2:2:1, prepare ceramic membrane sample, prepare ceramic membrane pore-forming material sawdust, Graphene and calcium carbonate content according to the method described above and be followed successively by 14%, 14%, 7%.
Therefore, use sawdust in pore-forming material: Graphene: when the component ratio of calcium carbonate is 2:2:1, ceramic membrane cloth hole is even, and surface is very level and smooth.Ceramic membrane porosity is even.
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to right.
Claims (6)
1. a preparation method for inorganic porous ceramic film, is characterized in that, comprises the following steps:
1., weigh: raw material, pore-forming material, sintering aid are weighed according to certain ratio, and mix; Described raw material choose diatomite, described pore-forming material comprises sawdust, Graphene and CaCO
3, described sintering aid is TiO2;
2., wet-milling: choose ball mill, load weighted material, agate bead and distilled water are together loaded in ball mill, the ratio of material, agate bead and distilled water is 2:1:1, and described material comprises raw material, pore-forming material, sintering aid, fully rotate through ball mill, make material grind evenly;
3., dry grind: the liquid in ball mill is filtered through screen cloth, obtain material liquid, then material liquid is put into oven for drying, material liquid puts into ball mill after having dried together with agate bead, ratio between agate bead and material is 2:1, relies on ball mill again to grind evenly to material;
4., granulation: screen out agate bead through screen cloth, take out material powders and also load in beaker, add appropriate distilled water, limit edged is stirred to powder and darkens and have and form block; Then in 60 object sieve granulations, by pressurizeing crushed for powder 60 mesh sieve with hand, the powder after crushed is placed in culture dish ageing;
5., compression molding: select electro-hydraulic servo universal press, the material measuring ageing is placed in mould, and electro-hydraulic servo universal press works, and makes compact formation, needs to ensure full pressure 3min after each malleation and back-pressure;
6., sintering: after ceramic membrane compacting, film base is put into baking oven and dry 24h and all volatilize to the moisture of film base.
2. the preparation method of inorganic porous ceramic film according to claim 1, is characterized in that, described TiO2 content is 1% of material total amount, and described pore-forming material is 35% of material total amount; Sawdust in described pore-forming material: Graphene: the component ratio of calcium carbonate is 2:2:1.
3. the preparation method of inorganic porous ceramic film according to claim 1, is characterized in that, described step 6. in sintering comprise four-stage, front three phases is carbonization volatilization period, and fourth stage is the sinter molding stage;
First stage: be warming up to 340 DEG C, and be incubated 0.5h; Subordinate phase: be warming up to 600 DEG C, and be incubated 1h, the phase III: be warming up to 780 DEG C, and be incubated 0.5h; Fourth stage: be warming up to 1100 DEG C, and be incubated 0.5h.
4. the preparation method of inorganic porous ceramic film according to claim 1, it is characterized in that, described step 2. in, during ball milling, rotating speed is 220r/min, is a ball milling cycle with 50min, has rotate forward grinding and reversion grinding two portions in each cycle, each 20min respectively, can suspend 10min after 40min running, then manually start the grinding of next cycle, milling time carries out 4 cycles.
5. the preparation method of inorganic porous ceramic film according to claim 1, it is characterized in that, described step 3. in, the rotating speed of dry grinding is 220r/min, 50min is a ball milling cycle, and each cycle has to rotate forward grinding and reverse grinds each 20min, after 40min running, suspend 10min, then the grinding of next cycle is manually started, dry grinding 2 cycles of grinding.
6. the preparation method of inorganic porous ceramic film according to claim 1, is characterized in that, described step 5. in, positive pressure pressure is 11kN, and back-pressure pressure is 13kN.
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| CN105854632A (en) * | 2016-05-15 | 2016-08-17 | 东北电力大学 | Method for preparing diatomite hollow fiber ceramic membrane |
| CN107051407A (en) * | 2017-06-01 | 2017-08-18 | 浙江永续环境工程有限公司 | Industrial reuse method for treating water |
| CN108484209B (en) * | 2018-04-09 | 2020-11-03 | 四川兴凯歌建设工程有限公司 | Flat ceramic membrane and preparation process thereof |
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| CN108706685A (en) * | 2018-05-29 | 2018-10-26 | 佛山市盟发净水科技有限公司 | A kind of ceramic film water purifier |
| CN108610085A (en) * | 2018-05-30 | 2018-10-02 | 佛山市航祥千安科技有限公司 | A kind of preparation method of the ceramic membrane based on natural polymer |
| CN108840703A (en) * | 2018-08-16 | 2018-11-20 | 北京工业大学 | A method of desalination hydrophobic porous cordierite ceramic film is prepared by raw material low cost of high silicon industrial solid castoff |
| CN112545066A (en) * | 2020-12-25 | 2021-03-26 | 深圳市康泓威科技有限公司 | Heatable graphene porous ceramic, atomizing core and preparation method thereof |
| CN112545066B (en) * | 2020-12-25 | 2024-03-29 | 海宁新纳陶科技有限公司 | Graphene porous ceramic capable of heating, atomization core and preparation method thereof |
| CN113336537A (en) * | 2021-05-12 | 2021-09-03 | 四川凯歌微纳科技有限公司 | Tubular ceramic membrane for industrial sewage treatment and preparation process |
| CN114368961A (en) * | 2022-01-27 | 2022-04-19 | 中钢集团马鞍山矿山研究总院股份有限公司 | Preparation method and new application of iron tailing ceramic filter material |
| CN115321948A (en) * | 2022-08-25 | 2022-11-11 | 山西工程技术学院 | Method for preparing ceramic filtering membrane by using wulan thea-crystal stone |
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