A kind of crystal white porcelain blank and its preparation method
The crystal white porcelain blank prepared through specific ratios and processes solves the balance of plasticity and grouting performance, and realizes high whiteness and strength daily porcelain products, reducing the difficulty of production system and management.
Patent Information
- Application Number
- CN202310622298.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-30
- Publication Date
- 2025-07-04
- Estimated Expiration
- 2043-05-30
AI Technical Summary
Existing daily ceramic blanks are difficult to balance between plasticity and grouting performance, resulting in increased production system and management difficulties, and molding defects such as shrinkage and cracking.
A specific proportion of raw materials such as Longyan mud washing, Longyan raw ore, potassium feldspar, sodium feldspar, high white mud washing, calcined talc, composite whiskers, quartz powder, zircon sand and cobalt sulfate powder are used to prepare crystal white porcelain blanks through wet ball milling and vacuum kneading processes, and composite whiskers are added to enhance mechanical properties and whiteness.
The prepared crystal white porcelain blanks have good plasticity and grouting properties at the same time, reducing production difficulty, improving the whiteness and mechanical stability of daily porcelain, and reducing molding defects.
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Figure BDA0004255737950000081
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of crystal white porcelain blanks, and in particular relates to a crystal white porcelain blank and a preparation method thereof. Background Art
[0002] White porcelain is a type of ceramic with a wide variety of applications. Because its glaze contains no or very small amounts of colorants, it appears plain white after firing. Because of its simple and unpretentious characteristics, it is deeply loved by consumers and is widely used in daily-use ceramics.
[0003] At present, most of the daily-use ceramic blank formulas are designed according to the product's porcelain-forming performance requirements. For example, in the production of high-temperature white porcelain blanks, the iron and titanium content should be low, and the aluminum oxide content should be relatively high to overcome its deformation defects. However, due to the production of matching tableware, some large pieces need to be rolled and formed, which requires good plasticity, while some special-shaped pieces need to be formed by grouting. The plasticity-formed clay is used for grouting, and there is a problem of unsatisfactory mud performance. Clay with good grouting performance is used to produce large rolling products, which is prone to shrinkage cracking defects. For this reason, in order to solve this problem, some ceramic material technicians use the method of making two kinds of clay and use them separately, which increases the difficulty of the production system and brings troubles to production management.
[0004] In order to reduce the difficulty in production system and production management, and make daily-use ceramic blanks have good plasticity and good grouting performance, a crystal white porcelain blank and a preparation method thereof are proposed. Summary of the invention
[0005] The object of the present invention is to provide a crystal white porcelain blank and a preparation method thereof, so as to solve the problems in the background technology.
[0006] The purpose of the present invention can be achieved through the following technical solutions:
[0007] A crystal white porcelain blank, comprising the following raw materials in parts by mass:
[0008] 28-38 parts of Longyan washed mud, 20-30 parts of Longyan ore, 6-15 parts of potassium feldspar ore, 12-20 parts of sodium feldspar ore, 6-14 parts of high white washed mud, 2-5 parts of calcined talc, 2-5 parts of composite whiskers, 5-12 parts of quartz powder, 0.5-1.5 parts of zircon sand, 1-5 parts of cattle bone ash and 10 parts of cobalt sulfate powder -5 share.
[0009] The method for preparing the crystal white porcelain blank comprises the following steps:
[0010] Step 1: Mix Longyan washed mud, Longyan raw ore, potassium feldspar ore, albite ore, high-white washed mud, calcined talc, composite whiskers, quartz powder, zircon sand, cattle bone ash and cobalt sulfate powder by wet ball milling in proportion, then sieve through a 300-325 mesh sieve, and use an electromagnetic iron remover to remove iron under a magnetic induction intensity of 10,000 Gs to obtain a mixed material;
[0011] Step 2: Transfer the mixed material to a vacuum clay kneader, knead it into clay segments under the condition of a vacuum degree of -0.08 to -0.096 MPa, control the water content of the clay segments to be 22% - 24%, let it age for 1 - 2 days, and then knead the clay segments for 1 - 2 h under the condition of a vacuum degree of -0.08 to -0.096 MPa to obtain a crystal white porcelain blank.
[0012] Furthermore, the composite whiskers are prepared through the following steps:
[0013] Step S1: Mix lithium fluoride and tetraethyl orthosilicate, then add zirconium chloride, stir at 300 - 500 r / min for 15 - 20 min, then add absolute ethanol and continue to stir for 3 - 5 min to obtain a precursor solution; reflux the precursor solution at 110 °C for 24 h, then vacuum dry at 60 - 100 °C, and transfer it to a sintering furnace to keep it warm at 400 ± 5 °C for 30 - 60 min to obtain a precursor powder;
[0014] Step S2: Heat sodium molybdate at 100 °C for 1 - 2 h to remove the crystal water to obtain anhydrous sodium molybdate, add the anhydrous sodium molybdate to the precursor powder, ball mill at 300 - 500 r / min for 30 - 60 min, then filter and discharge, calcine at 850 ± 5 °C for 100 - 120 min, add the calcined product to hydrofluoric acid with a mass fraction of 20%, stir under ultrasonic assistance for 20 - 40 min, filter, wash the filter residue with deionized water 3 - 5 times, and then vacuum dry at 60 - 100 °C to obtain zirconium silicate whiskers.
[0015] Step S3: Add zirconium silicate whiskers and zinc hydroxide powder to a shear disperser to shear and disperse for 1 - 2 h to obtain a mixed powder; transfer the mixed powder to a high-temperature reduction furnace, and reduce and roast it in a hydrogen atmosphere at 850 - 900 °C for 40 - 60 min to obtain composite whiskers.
[0016] Furthermore, the dosage ratio of lithium fluoride, tetraethyl orthosilicate, zirconium chloride and absolute ethanol is 9.5 g : 245 g : 233 g : 1000 mL.
[0017] Furthermore, the dosage ratio of anhydrous sodium molybdate and the precursor powder is 1 g : 2 g.
[0018] Furthermore, the dosage ratio of zirconium silicate whiskers to zinc hydroxide powder is 20 g : 15 - 20 g.
[0019] Advantages of the present invention:
[0020] The crystal white porcelain body of the present invention has both good plastic properties and good slip casting properties, which is beneficial to reducing the difficulty in the production system and production management. The raw material composition of the crystal white porcelain body is rationally proportioned and has a relatively wide firing temperature. Zirconium silicate, aluminum sulfate, and cattle bone ash help to increase the whiteness of daily-use porcelain. The composite whiskers have a toughening effect and help to adjust the mechanical properties of the crystal white porcelain body. During the preparation of zirconium silicate whiskers, sodium molybdate melts to form a liquid phase at high temperature, and zirconium silicate grows crystals with sodium molybdate as the molten salt, which helps to prevent whisker agglomeration and is beneficial to obtaining zirconium silicate whiskers with complete growth and uniform size. After pickling and washing with water, pure zirconium silicate whiskers are reduced at high temperature with zinc hydroxide, and metal zinc adheres to the zirconium silicate whiskers to obtain composite whiskers. In the form of composite whiskers, it helps to disperse the metal evenly, prevent agglomeration, and play a fluxing role, which helps daily-use porcelain to obtain better thermal shock resistance and brightness, thereby greatly improving the whiteness of daily-use porcelain and increasing the mechanical properties and stability of daily-use porcelain. Specific embodiments
[0021] Next, in combination with the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention.
[0022] Example 1
[0023] This example provides a composite whisker, including the following implementation steps:
[0024] Step S1: Mix 9.5 kg of lithium fluoride and 245 kg of tetraethyl orthosilicate, then add 233 kg of zirconium chloride, stir at 300 r / min for 15 min, then add 1000 L of absolute ethanol and continue to stir for 3 min to obtain a precursor solution; reflux the precursor solution at 110 °C for 24 h, then vacuum dry at 60 °C, and transfer it to a sintering furnace to keep it warm at 400 ± 5 °C for 30 min to obtain a precursor powder.
[0025] Step S2: Heat sodium molybdate at 100 °C for 1 h to remove the crystal water and obtain anhydrous sodium molybdate. Add 200 kg of anhydrous sodium molybdate to 400 kg of precursor powder, ball mill at 300 r / min for 30 min, then filter and discharge. Calcinate the product at 850 ± 5 °C for 100 min. Add the calcined product to hydrofluoric acid with a mass fraction of 20%, stir under ultrasonic assistance for 20 min, filter, wash the filter residue 3 times with deionized water, and then vacuum dry at 60 °C to obtain zirconium silicate whiskers.
[0026] Step S3: Add 200 kg of zirconium silicate whiskers and 150 kg of zinc hydroxide powder to a shear disperser and shear disperse for 1 h to obtain a mixed powder; transfer the mixed powder to a high-temperature reduction furnace and reduce it in a hydrogen atmosphere at 850 °C for 40 min to obtain composite whiskers.
[0027] Example 2
[0028] This example provides a composite whisker, including the following implementation steps:
[0029] Step S1: Mix 9.5 kg of lithium fluoride and 245 kg of tetraethyl orthosilicate, then add 233 kg of zirconium chloride, stir at 400 r / min for 18 min, then add 1000 L of anhydrous ethanol and continue to stir for 4 min to obtain a precursor solution; reflux the precursor solution at 110 °C for 24 h, then vacuum dry at 80 °C, and transfer it to a sintering furnace to keep warm at 400 ± 5 °C for 45 min to obtain precursor powder.
[0030] Step S2: Heat sodium molybdate at 100 °C for 1.5 h to remove the crystal water and obtain anhydrous sodium molybdate. Add 200 kg of anhydrous sodium molybdate to 400 kg of precursor powder, ball mill at 400 r / min for 45 min, then filter and discharge. Calcinate the product at 850 ± 5 °C for 110 min. Add the calcined product to hydrofluoric acid with a mass fraction of 20%, stir under ultrasonic assistance for 30 min, filter, wash the filter residue 4 times with deionized water, and then vacuum dry at 80 °C to obtain zirconium silicate whiskers.
[0031] Step S3: Add 200 kg of zirconium silicate whiskers and 180 kg of zinc hydroxide powder to a shear disperser and shear disperse for 1.5 h to obtain a mixed powder; transfer the mixed powder to a high-temperature reduction furnace and reduce it in a hydrogen atmosphere at 880 °C for 50 min to obtain composite whiskers.
[0032] Example 3
[0033] This example provides a composite whisker, including the following implementation steps:
[0034] Step S1: Mix 9.5 kg of lithium fluoride and 245 kg of tetraethyl orthosilicate, then add 233 kg of zirconium chloride, stir for 20 min under the condition of 500 r / min, then add 1000 L of absolute ethanol and continue to stir for 5 min to obtain a precursor solution; reflux the precursor solution for 24 h under the condition of 110 °C, then vacuum dry under the condition of 100 °C, and transfer it to a sintering furnace to keep warm for 60 min under the condition of 400 ± 5 °C to obtain precursor powder.
[0035] Step S2: Heat sodium molybdate for 2 h under the condition of 100 °C to remove crystal water to obtain anhydrous sodium molybdate. Add 200 kg of anhydrous sodium molybdate to 400 kg of precursor powder, ball mill for 60 min under the condition of 500 r / min, then filter and discharge. Calcinate at 850 ± 5 °C for 120 min. Add the calcined product to hydrofluoric acid with a mass fraction of 20%, stir for 40 min under ultrasonic assistance, filter, wash the filter residue 5 times with deionized water, and then vacuum dry under the condition of 100 °C to obtain zirconium silicate whiskers.
[0036] Step S3: Add 200 kg of zirconium silicate whiskers and 200 kg of zinc hydroxide powder to a shear disperser and shear disperse for 2 h to obtain a mixed powder; transfer the mixed powder to a high-temperature reduction furnace, reduce it for 60 min under a hydrogen atmosphere and the condition of 900 °C to obtain composite whiskers.
[0037] Example 4
[0038] This example provides a crystal white porcelain blank, including the following implementation steps:
[0039] Step 1: Wet ball mill and mix 28 kg of Longyan washed mud, 20 kg of Longyan raw ore, 6 kg of potassium feldspar ore, 12 kg of albite ore, 6 kg of high-white washed mud, 2 kg of calcined talc, 2 kg of the composite whiskers in Example 1, 5 kg of quartz powder, 0.5 kg of zircon sand, 1 kg of yellow cattle bone ash, and 0.01 g of cobalt sulfate powder, then pass through a 300-mesh sieve, and use an electromagnetic iron remover to remove iron under the magnetic induction intensity of 10000 Gs to obtain a mixed material.
[0040] Step 2: Transfer the mixed material to a vacuum pug mill, knead it into mud segments under the condition of a vacuum degree of -0.08 MPa, control the water content of the mud segments to be 22%, and after aging for 1 day, knead the mud segments for 1 h under the condition of a vacuum degree of -0.08 MPa to obtain a crystal white porcelain blank.
[0041] Example 5
[0042] This example provides a crystal white porcelain blank, including the following implementation steps:
[0043] Step 1: 32 kg of Longyan washed mud, 25 kg of Longyan raw ore, 10.5 kg of potassium feldspar ore, 16 kg of albite ore, 10 kg of high-white washed mud, 3.5 kg of calcined talc, 3.5 kg of the composite whisker in Example 2, 8.5 kg of quartz powder, 1 kg of zircon sand, 3 kg of yellow cattle bone ash, and 0.01 g of cobalt sulfate powder are wet ball-milled and mixed, then passed through a 315-mesh sieve. An electromagnetic iron remover is used to remove iron under a magnetic induction intensity of 10000 Gs to obtain a mixed material.
[0044] Step 2: Transfer the mixed material to a vacuum clay kneader and knead it into clay segments under a vacuum degree of -0.09 Pa. Control the water content of the clay segments to be 23%. After aging for 1.5 days, knead the clay segments for 1.5 h under a vacuum degree of -0.09 MPa to obtain a crystal white porcelain blank.
[0045] Example 6
[0046] This example provides a crystal white porcelain blank, including the following implementation steps:
[0047] Step 1: 38 kg of Longyan washed mud, 30 kg of Longyan raw ore, 15 kg of potassium feldspar ore, 20 kg of albite ore, 14 kg of high-white washed mud, 5 kg of calcined talc, 5 kg of the composite whisker in Example 3, 12 kg of quartz powder, 1.5 kg of zircon sand, 5 kg of yellow cattle bone ash, and 0.01 g of cobalt sulfate powder are wet ball-milled and mixed, then passed through a 325-mesh sieve. An electromagnetic iron remover is used to remove iron under a magnetic induction intensity of 10000 Gs to obtain a mixed material.
[0048] Step 2: Transfer the mixed material to a vacuum clay kneader and knead it into clay segments under a vacuum degree of -0.096 MPa. Control the water content of the clay segments to be 24%. After aging for 2 days, knead the clay segments for 2 h under a vacuum degree of -0.096 MPa to obtain a crystal white porcelain blank.
[0049] Comparative Example 1
[0050] On the basis of Example 6, the composite whisker is not added, and the remaining steps remain unchanged to prepare a crystal white porcelain blank.
[0051] Comparative Example 2
[0052] On the basis of Example 6, cobalt sulfate is not added, and the remaining steps remain unchanged to prepare a crystal white porcelain blank.
[0053] The raw materials in the examples and comparative examples are purchased from Sibelco Minerals Co., Ltd.
[0054] Using the crystal white porcelain blanks in Examples 4 to 6 and Comparative Examples 1 to 2 as raw materials, daily-use porcelain is batch-fired by the rolling forming method and the slip casting method respectively, with 100 pieces in each batch.
[0055] Rolling forming method: Directly roll the crystal white porcelain blank into a rough blank, dry it for 18 ± 2 h under the condition of 90 ± 10 °C, apply clear glaze with a thickness of 0.25 ± 0.05 mm after trimming, and fire it into daily-use porcelain under reducing atmosphere and at 1390 ± 20 °C.
[0056] Slip casting forming method: Add sodium silicate accounting for 0.6 ± 0.1% of its mass and water reducer Xianshui (Jingdezhen Yuni Ceramics Co., Ltd.) accounting for 0.025 ± 0.05% of its mass to the crystal white porcelain blank, control the water content of the slurry to be 32 ± 1%, cast it into a rough blank, dry it for 18 ± 2 h under the condition of 90 ± 10 °C, apply clear glaze with a thickness of 0.25 ± 0.05 mm after trimming, and fire it into daily-use porcelain under reducing atmosphere and at 1390 ± 20 °C.
[0057] According to QB / T 1548-2015, statistically analyze the average linear shrinkage rate of daily-use porcelain in different batches, and detect the average whiteness of daily-use porcelain in different batches according to QB / T 1503-2011. The results are shown in Table 1:
[0058] Table 1
[0059]
[0060]
[0061] As can be seen from Table 1, the crystal white porcelain blanks in Examples 4 to 6 prepared into daily-use porcelain by the rolling forming method and the slip casting forming method both have a relatively small shrinkage rate, and the composite whiskers have good strengthening and whitening effects.
[0062] It should be noted that in this article, terms such as "including", "comprising" or any other variant thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements not only includes those elements, but also includes other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.
[0063] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principle and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A crystal white porcelain blank, characterized in that, By mass parts, it includes the following raw materials: 28 - 38 parts of Longyan washed mud, 20 - 30 parts of Longyan raw ore, 6 - 15 parts of potassium feldspar ore, 12 - 20 parts of albite ore, 6 - 14 parts of high - white washed mud, 2 - 5 parts of calcined talc, 2 - 5 parts of composite whiskers, 5 - 12 parts of quartz powder, 0.5 - 1.5 parts of zircon sand, 1 - 5 parts of yellow cattle bone ash and 10 -5 parts; The composite whiskers are prepared through the following steps: Shear and disperse zirconium silicate whiskers and zinc hydroxide powder for 1 - 2 h to obtain a mixed powder; reduce and calcine the mixed powder in a hydrogen atmosphere at 850 - 900 °C for 40 - 60 min to obtain the composite whiskers.
2. A kind of crystal white porcelain blank according to claim 1, characterized in that, The dosage ratio of the zirconium silicate whiskers to the zinc hydroxide powder is 20 g : 15 - 20 g.
3. A kind of crystal white porcelain blank according to claim 1, characterized in that, The zirconium silicate whiskers are prepared through the following steps: Add anhydrous sodium molybdate to the precursor powder, ball mill at 300 - 500 r / min for 30 - 60 min, then filter and discharge. Calcinate at 850 ± 5 °C for 100 - 120 min. Stir and pickle the calcined product under ultrasonic assistance, filter, wash, and dry to obtain the zirconium silicate whiskers.
4. A kind of crystal white porcelain blank according to claim 3, characterized in that, The dosage ratio of the anhydrous sodium molybdate to the precursor powder is 1 g : 2 g.
5. A kind of crystal white porcelain blank according to claim 4, characterized in that, The precursor powder is prepared through the following steps: Mix lithium fluoride and tetraethyl orthosilicate, then add zirconium chloride, stir at 300 - 500 r / min for 15 - 20 min, add absolute ethanol and continue to stir for 3 - 5 min to obtain a precursor solution; Reflux the precursor solution at 110 °C for 24 h, dry and then keep it at 400 ± 5 °C for 30 - 60 min to obtain the precursor powder.
6. The fine white porcelain blank according to claim 5, characterized in that, The dosage ratio of the lithium fluoride, tetraethyl orthosilicate, zirconium chloride, and absolute ethanol is 9.5 g : 245 g : 233 g : 1000 mL.
7. The preparation method of a crystal white porcelain blank according to claim 1, characterized in that, It includes the following steps: Step 1: Wet ball mill and mix Longyan washed mud, Longyan raw ore, potassium feldspar ore, sodium feldspar ore, high - white washed mud, calcined talc, composite whiskers, quartz powder, zircon sand, yellow cattle bone ash, and cobalt sulfate powder in proportion, then pass through a 300 - 325 - mesh sieve. Use an electromagnetic iron remover to remove iron under a magnetic induction intensity of 10000 Gs to obtain a mixed material; Step 2: Transfer the mixed material to a vacuum pug mill, knead it into mud segments under a vacuum degree of - 0.08 - - 0.096 MPa, control the water content of the mud segments to be 22% - 24%, let it age for 1 - 2 days, and then knead the mud segments under a vacuum degree of - 0.08 - - 0.096 MPa for 1 - 2 h to obtain a crystal white porcelain blank.
Citation Information
Patent Citations
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