CN111116169A - Process ceramic slurry prepared from tailings and preparation method thereof - Google Patents
Process ceramic slurry prepared from tailings and preparation method thereof Download PDFInfo
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- CN111116169A CN111116169A CN201911330639.5A CN201911330639A CN111116169A CN 111116169 A CN111116169 A CN 111116169A CN 201911330639 A CN201911330639 A CN 201911330639A CN 111116169 A CN111116169 A CN 111116169A
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
- C04B2235/321—Dolomites, i.e. mixed calcium magnesium carbonates
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
- C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Abstract
The invention relates to slurry for process ceramics prepared by using tailings and a preparation method thereof, wherein the slurry for process ceramics comprises the following raw materials in percentage by weight: 30-50% of tailings, 12-18% of potash-soda feldspar, 16-26% of kaolin, 15-25% of high-strength porcelain clay, 2-5% of dolomite and 3-6% of calcined talc. The slurry for the process ceramic uses a large amount of low-price tailings as raw materials, changes waste into valuable, fully utilizes resources, and plays a role in reducing energy consumption, cost and efficiency.
Description
Technical Field
The invention relates to the technical field of ceramic processes, in particular to slurry for process ceramics prepared by using tailings, a preparation method thereof and processes for forming, glazing and sintering by using the slurry.
Background
Ceramic, english: china. The pottery was invented by Chinese in 8000- & 2000 years (the age of the New Stone wares) before the public. The ware fired with pottery clay is called pottery, and the ware fired with porcelain clay is called porcelain. The pottery is a general term for pottery, stoneware and porcelain. Ancient people called pottery Ou. The pottery clay and porcelain clay are used as raw materials, and the ware prepared by the technical processes of proportioning, forming, drying, roasting and the like can be called as ceramic.
The ceramics mainly comprise three types according to the application: domestic ceramics, technical ceramics and industrial ceramics. Wherein, the technical ceramic is ornamental and playable; can be used and can also be used for investing and collecting art varieties, such as vases, sculptures, garden ceramics, utensils, photo frames, murals, furnishing articles and the like. The craft ceramic forms a unique ceramic culture by the exquisite decorative beauty, the illusion artistic conception beauty, the unique personality beauty of ceramic art and the unique material beauty, and is popular with people.
The raw materials used by the existing process ceramic slurry are high-quality raw materials with less impurities, high purity, good plasticity and high price. However, mineral resources are impossible to regenerate, and high-quality resources are increasingly reduced. Therefore, how to prepare the slurry for the process ceramics with the same quality by using the inferior raw materials so as to save the utilization rate of the preferable mineral resources and reduce the manufacturing cost becomes a technical problem to be solved by the technical personnel in the field.
Disclosure of Invention
In order to solve the technical problems, the invention provides the slurry for the technical ceramics, which is prepared by fully utilizing the low-price tailing raw material and can reach or even exceed the performance level of the slurry sold in the market.
The specific scheme is as follows:
one of the purposes of the invention is to provide a slurry for process ceramics prepared by using tailings, which comprises the following raw materials in percentage by weight: 30-50% of tailings, 12-18% of potash-soda feldspar, 16-26% of kaolin, 15-25% of high-strength porcelain clay, 2-5% of dolomite and 3-6% of calcined talc.
Further, the slurry for the technical ceramics comprises the following chemical components in percentage by weight: SiO 2258-68％，Al2O318-24％，Fe2O30.3-1.0％，TiO20-0.5％，CaO 0.5-1.2％，MgO 1-4％，K2O 3-5％，Na20.5 to 1 percent of O and the balance of impurities.
Further, the slurry for the technical ceramic has the following properties: yield value of 15-20dyn/cm2, drying strength of 2.8-3.5MPa, drying shrinkage of 2.5-3.5%, sintering shrinkage of 9-10%, and total shrinkage of 1-13%.
Further, the physicochemical indexes of the tailings are as follows: SiO 2281-83％，Al2O310-12％，Fe2O30.2-0.4％，TiO20.01-0.07％，CaO 0.01-0.09％，MgO 0.01-0.13％，K2O 1.5-3.0％，Na20.01-0.10% of O and 2-3% of loss on ignition.
The invention also aims to provide a preparation method of the slurry for the technical ceramics prepared by the tailings, which comprises the following steps:
(1) the ball mill uses a high-alumina lining and adopts high-alumina ball milling;
(2) weighing the raw materials according to the weight percentage, adding a debonding agent and water, and carrying out ball milling to obtain ball-milled slurry;
(3) and (3) discharging the slurry obtained in the step (2) after ball milling, sieving with a 100-mesh sieve, removing iron twice by high magnetism, ageing, and pugging to obtain a finished product.
Further, the dispergator comprises the following components in percentage by weight: water glass accounting for 0.5-1.1% of the total weight of the raw materials, and alkali powder accounting for 0.15% of the total weight of the raw materials; the addition amount of the water is 41-43% of the total weight of the raw materials.
Further, the slurry ball-milled in the step (2) requires that the 325-mesh sieve residue is less than 5%, and the slurry with the particle size of less than 10um accounts for 60-68% of the total mass of the slurry.
The invention also aims to provide a process ceramic molding process, which adopts the slurry for process ceramic prepared by using the tailings as a raw material and adopts rolling, grouting or blank drawing means for molding.
The invention also aims to provide a glazing process of the technical ceramic, which adopts the slurry for the technical ceramic prepared by the tailings as a raw material, adopts a glaze pouring or glazing method to carry out glazing, and the glaze is transparent glaze.
The invention also aims to provide a firing process of the technical ceramic, which adopts the slurry for the technical ceramic prepared by the tailings as a raw material and adopts a shuttle kiln to fire, wherein the firing temperature is controlled at 1200-1230 ℃, and the firing time is 7-10 hours.
Wherein:
the tailings are tailings generated in the process of producing the high-strength porcelain clay, and are usually directly discarded in the traditional production process, but the tailings with fine particles and good whiteness are obtained by washing and deironing the tailings, so that the tailings are utilized, the price is low, and the tailings play a role of quartz and partial potash feldspar in a blank body. Wherein, the quartz plays a role of a framework in the blank body, can reduce shrinkage and deformation, and enhances mechanical strength; the potash feldspar acts as a flux in the green body, so that the sintering temperature can be reduced, the slurry viscosity can be reduced, and the drying shrinkage and drying time can be reduced.
The optimal use amount of the tailings is as follows: 30-50%, the reason for this is that: if the proportion of the tailings exceeds 50%, the prepared slurry has high silicon content and poor plasticity, and is not suitable for grouting forming; if the proportion of the tailings is lower than 30%, the content of aluminum in the prepared slurry is high, the firing temperature requirement is high, and a semi-finished product wet blank prepared by forming is soft and easy to denature.
The potash albite has the effects of reducing drying shrinkage and deformation of a blank, improving drying performance and shortening drying time. When in sintering, the material can be used as a fusing agent to reduce the sintering temperature, promote the quartz and kaolin to be fused and accelerate the formation of mullite (a high-quality refractory material). The feldspar glass body generated in the fusion of the potash albite is filled among mullite grains of the blank body, so that the blank body is compact, the gap is reduced, and the mechanical strength of the blank body is improved. The best usage amount of the potash albite is as follows: 12-18%, the reason for this is that: if the proportion of the potash-soda feldspar exceeds 18%, the content of alkali metal in the prepared slurry is high, the sintering temperature is low, and the product is easy to deform; if the proportion of the potash-soda feldspar is lower than 12%, the content of alkali metal in the prepared slurry is low, and the requirement on the sintering temperature is high.
The kaolin has the function of introducing Al into the ceramic2O3Is beneficial to the generation of mullite and improves the chemical stability and the sintering strength of the mullite. During firing, kaolin is decomposed to generate mullite, a main frame of the green body strength is formed, the deformation of the ceramic product can be prevented, the firing temperature is widened, and the green body has certain whiteness. Meanwhile, the kaolin has certain plasticity, caking property and suspension property. The best usage amount of the kaolin is as follows: 16-26%, the reason for this is: if the kaolin proportion exceeds 26 percent, the prepared mud Al2O3The content is high, and the firing temperature requirement is high; if the kaolin proportion is less than 16%, the prepared mud Al2O3Low content, and poor plasticity, caking property and suspension property of the slurry.
The high-strength porcelain clay is a porcelain clay with better whiteness in China, is rich in illite mineral components, and has the characteristics of long crack generation time, good plasticity, small drying shrinkage, higher dry flexural strength and higher manufacturing cost. The optimal usage amount of the high-strength porcelain clay is as follows: 15-25%, the reason for this is: if the proportion of the high-strength porcelain clay exceeds 25%, the slurry-taking speed of the prepared slurry is low, and the slurry is not suitable for grouting forming; if the proportion of the high-strength porcelain clay is less than 15%, the prepared slurry has poor plasticity and low drying strength and is easy to crack.
The dolomite and the calcined talc have the function of introducing a large amount of CaO and MgO into the green body, thereby reducing the melting temperature and the viscosity of the green body, and the green body is easy to wet Al2O3、SiO2The particles can rapidly promote the sintering of the green body, play the role of a strong mineralizer and shorten the sintering time. The optimal use amount of the dolomite is as follows: 2-5%, the best usage amount of the calcined talc is: 3-6%, the reason for this is: dolomite and calcined talc are fluxing agent raw materials, the consumption is large, the loss of the slurry caused by burning is large, the slurry burning temperature is low, and the product is easy to deform; the usage amount is small, the mud firing temperature is high, and the product is not easy to fire.
The chemical compositions of the raw materials used in the present invention are shown in table 1.
TABLE 1 list of chemical composition of raw materials (wt%)
The properties of the slurry for technical ceramics prepared by the present invention are shown in Table 2.
TABLE 2 modulation Properties of the finished slurries prepared according to the invention
| Item | Parameter(s) |
| Concentration (g/200mL) | 355-360 |
| Temperature (. degree.C.) | 20-28 |
| V0 (second/100 mL) | 50-60 |
| V30 (second/100 mL) | 90-105 |
| Eating pulp speed (mm/45 min) | 5.6-6.3 |
| Yield value (dyn/cm)2) | 15-20 |
| Dry Strength (MPa) | 2.8-3.5 |
| Drying shrinkage (%) | 2.5-3.5 |
| Firing shrinkage (%) | 9-10 |
| Total shrinkage (%) | 11-13 |
| Whiteness (%) | 72-78 |
| Water absorption (%) | 0.1-0.5 |
As can be seen from Table 2, the slurry of the invention adopts a formula of low-cost raw materials, and can obtain good performance on indexes such as slurry thickness, dry strength, drying shrinkage, firing shrinkage, total shrinkage, whiteness, concentration, temperature, V0, V30, yield value and the like, thereby achieving the performance level even exceeding that of the slurry sold in the market, replacing the existing slurry sold in the market and saving the production cost.
Has the advantages that:
the slurry for the process ceramic uses a large amount of low-price tailings as raw materials, changes waste into valuable, fully utilizes resources, and plays a role in reducing energy consumption, cost and efficiency.
Detailed Description
The following detailed description of embodiments of the invention is intended to be illustrative, and is not to be construed as limiting the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1:
table 3 examples 1-3 tabulated weight percent (wt%) of each material
| Example 1 | Example 2 | Example 3 | |
| Tailings | 30 | 40 | 50 |
| Potassium-sodium feldspar | 17 | 15 | 12 |
| Kaolin clay | 20.5 | 18.5 | 13 |
| High-strength porcelain clay | 25 | 18 | 20 |
| Dolomite | 3 | 2.5 | 2 |
| Calcined talc | 4.5 | 6 | 3 |
A preparation method of slurry for process ceramics prepared by using tailings comprises the following steps:
(1) the ball mill uses a high-alumina lining and adopts high-alumina ball milling;
(2) weighing the raw materials according to the weight percentage in the table 3, adding a debonding agent and water, and carrying out ball milling to obtain ball-milled slurry;
(3) and (3) discharging the slurry obtained in the step (2) after ball milling, sieving with a 100-mesh sieve, removing iron twice by high magnetism, ageing, pugging and obtaining a finished product.
Wherein the content of the first and second substances,
the dispergator comprises the following components in percentage by weight: water glass accounting for 0.5 percent of the total weight of the raw materials and alkali powder accounting for 0.15 percent of the total weight of the raw materials; the addition amount of the water is 43 percent of the total weight of the raw materials; the slurry ball-milled in the step (2) requires that the 325-mesh sieve residue is less than 5 percent, and the slurry with the granularity less than 10um accounts for 68 percent of the total mass of the whole slurry.
Example 2:
the preparation method of the embodiment 2 is basically the same as the embodiment 1, except that in the embodiment 2: the dispergator comprises the following components in percentage by weight: 1.1 percent of water glass and 0.15 percent of alkaline surface by weight of the raw materials; the addition amount of the water is 42 percent of the total weight of the raw materials; the slurry ball-milled in the step (2) requires that the 325-mesh sieve residue is less than 5 percent, and the slurry with the granularity less than 10um accounts for 65 percent of the total mass of the whole slurry.
Example 3:
the preparation method of example 3 is substantially the same as that of example 1, except that in example 3: the dispergator comprises the following components in percentage by weight: water glass accounting for 1 percent of the total weight of the raw materials and alkali surface accounting for 0.15 percent of the total weight of the raw materials; the addition amount of the water is 41 percent of the total weight of the raw materials; the slurry ball-milled in the step (2) requires that the 325-mesh sieve residue is less than 5 percent, and the slurry with the granularity less than 10um accounts for 60 percent of the total mass of the whole slurry.
Comparative example 1:
table 4 tabulated weight percent (wt%) of each of comparative examples 1-6
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Tailings | 30 | 40 | 50 | 0 | 20 | 60 |
| Potassium-sodium feldspar | 15 | 16 | 15 | 18 | 20 | 8 |
| Kaolin clay | 25.5 | 22.5 | 25 | 30 | 25.5 | 15 |
| High-strength porcelain clay | 22.5 | 14 | 6 | 41 | 26.5 | 9 |
| Dolomite | 2.5 | 3 | 2 | 5 | 3.5 | 4 |
| Calcined talc | 4.5 | 4.5 | 2 | 6 | 4.5 | 4 |
A method of making the slurries of comparative examples 1-6, comprising the steps of:
(1) the ball mill uses a high-alumina lining and adopts high-alumina ball milling;
(2) weighing the raw materials of comparative examples 1-6 according to the weight percentage in the table 4, adding a dispergator and water, and carrying out ball milling to obtain well ball-milled slurry;
(3) and (3) discharging the slurry obtained in the step (2) after ball milling, sieving with a 100-mesh sieve, removing iron twice by high magnetism, ageing, pugging and obtaining a finished product.
Wherein the content of the first and second substances,
the dispergator comprises the following components in percentage by weight: water glass accounting for 0.5 percent of the total weight of the raw materials and alkali powder accounting for 0.15 percent of the total weight of the raw materials; the addition amount of the water is 43 percent of the total weight of the raw materials; the slurry ball-milled in the step (2) requires that the 325-mesh sieve residue is less than 5 percent, and the slurry with the granularity less than 10um accounts for 68 percent of the total mass of the whole slurry.
And (3) experimental test:
the properties of the slurries prepared in examples 1 to 3 and comparative examples 1 to 6 were tested.
The test method comprises the following steps:
concentration: weight of mud measured using a 200mL volumetric flask, unit: g/200 mL.
Temperature: and a thermometer is adopted to detect the temperature of the slurry.
V0, V30: the time taken for a 100mL volume of mud flow was measured using a nonstandard testing instrument, marrio tube.
Slurry feeding speed: the thickness of the slurry taken after 45 minutes of slurry taking time was circular using a non-standard piece of gypsum.
Yield value: the yield value of the slurry was measured using a rotational viscometer.
The drying strength, drying shrinkage, firing shrinkage and total shrinkage are detected according to the corresponding methods of the national standard GB/T26742-2011 raw material clay for building sanitary ceramics.
Water absorption: the detection is carried out according to the corresponding method of the national standard GB/T6952-2015 sanitary ware.
And (3) performance comparison:
TABLE 5 comparative lists of the properties of examples 1-3 and comparative examples 1-6
From the comparative test results in table 5, it can be seen that:
1. the performance and the product of the slurry prepared by the invention can be compared favorably with the performance and the product of the slurry prepared by the traditional high-price raw material, and the invention fully uses the tailing raw material, reduces the cost of the slurry by about 30 percent, changes waste into valuable and is beneficial to environmental protection.
2. The requirements of the invention on the proportion of the raw materials are very strict, and the slurry of the invention can be affected if the proportion exceeds or falls below the proportion, such as:
comparative example 4 no tailing was used, the mud yield value was high, the value of V30 was large, drying shrinkage was large, the mud viscosity was large, the fluidity was poor, and the product was prone to cracking;
comparative example 5 the tailing ratio is 20%, the prepared slurry has high water absorption rate and the required sintering temperature is high;
compared with the comparative example 6, the tailing ratio is 60 percent, the slurry prepared by the method has low slurry feeding speed, small drying shrinkage, large sintering shrinkage, and easy cracking of the product in the sintering process.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The slurry for the technical ceramics prepared by the tailings is characterized by comprising the following raw materials in percentage by weight: 30-50% of tailings, 12-18% of potash-soda feldspar, 16-26% of kaolin, 15-25% of high-strength porcelain clay, 2-5% of dolomite and 3-6% of calcined talc.
2. The process ceramic mud prepared by the tailings according to claim 1, wherein the process ceramic mud comprises the following chemical components in percentage by weight: SiO 2258-68％，Al2O318-24％，Fe2O30.3-1.0％，TiO20-0.5％，CaO 0.5-1.2％，MgO 1-4％，K2O 3-5％，Na20.5 to 1 percent of O and the balance of impurities.
3. The process ceramic slurry prepared by using the tailings according to claim 1, wherein the properties of the process ceramic slurry are as follows: yield value of 15-20dyn/cm2The drying strength is 2.8-3.5MPa, the drying shrinkage is 2.5-3.5%, the sintering shrinkage is 9-10%, and the total shrinkage is 1-13%.
4. The process ceramic slurry prepared from the tailings according to claim 1, wherein the tailings have physical and chemical indexes as follows: SiO 2281-83％，Al2O310-12％，Fe2O30.2-0.4％，TiO20.01-0.07％，CaO 0.01-0.09％，MgO 0.01-0.13％，K2O 1.5-3.0％，Na20.01-0.10% of O and 2-3% of loss on ignition.
5. The method for preparing the slurry for the technical ceramics by using the tailings as claimed in any one of claims 1 to 4, characterized by comprising the steps of:
(1) the ball mill uses a high-alumina lining and adopts high-alumina ball milling;
(2) weighing the raw materials according to the weight percentage, adding a debonding agent and water, and carrying out ball milling to obtain ball-milled slurry;
(3) and (3) discharging the slurry obtained in the step (2) after ball milling, sieving with a 100-mesh sieve, removing iron twice by high magnetism, ageing, and pugging to obtain a finished product.
6. The technical ceramic mud prepared by the tailings according to claim 5, wherein the dispergator comprises the following components in percentage by weight: water glass accounting for 0.5-1.1% of the total weight of the raw materials, and alkali powder accounting for 0.15% of the total weight of the raw materials; the addition amount of the water is 41-43% of the total weight of the raw materials.
7. The process ceramic slurry prepared by the tailings according to claim 5, wherein the slurry ball-milled in the step (2) requires a 325-mesh sieve with less than 5% residue, and the slurry with the particle size of less than 10um accounts for 60-68% of the total mass of the slurry.
8. A process for forming a technical ceramic, characterized in that the technical ceramic slurry prepared by the tailings of any one of claims 1 to 4 is used as a raw material and is formed by rolling, grouting or throwing.
9. A process for glazing technical ceramics, characterized in that the slurry for technical ceramics prepared by using the tailings as claimed in any one of claims 1 to 4 is used as a raw material, glazing is carried out by means of glaze pouring or glaze pouring, and the glaze is transparent glaze.
10. The process for firing technical ceramics is characterized in that the technical ceramics prepared by the tailings in the claim 1-4 is used as raw material and is fired by a shuttle kiln, the firing temperature is controlled at 1200-1230 ℃, and the firing time is 7-10 hours.
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