CN115849865A - Preparation method of high-performance ball clay for ceramic sanitary ware - Google Patents
Preparation method of high-performance ball clay for ceramic sanitary ware Download PDFInfo
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- CN115849865A CN115849865A CN202211692766.1A CN202211692766A CN115849865A CN 115849865 A CN115849865 A CN 115849865A CN 202211692766 A CN202211692766 A CN 202211692766A CN 115849865 A CN115849865 A CN 115849865A
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- ball clay
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- clay
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- 239000010427 ball clay Substances 0.000 title claims abstract description 54
- 239000000919 ceramic Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000002002 slurry Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 32
- 150000001875 compounds Chemical class 0.000 claims abstract description 28
- 239000004927 clay Substances 0.000 claims abstract description 16
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 14
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 14
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000001110 calcium chloride Substances 0.000 claims abstract description 13
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 97
- 239000000835 fiber Substances 0.000 claims description 73
- 239000000377 silicon dioxide Substances 0.000 claims description 48
- 239000002121 nanofiber Substances 0.000 claims description 41
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 38
- 239000002131 composite material Substances 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 35
- 235000012239 silicon dioxide Nutrition 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 21
- 239000004964 aerogel Substances 0.000 claims description 18
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 238000010041 electrostatic spinning Methods 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 8
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 8
- SZHIIIPPJJXYRY-UHFFFAOYSA-M sodium;2-methylprop-2-ene-1-sulfonate Chemical compound [Na+].CC(=C)CS([O-])(=O)=O SZHIIIPPJJXYRY-UHFFFAOYSA-M 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 7
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 7
- 238000003837 high-temperature calcination Methods 0.000 claims description 6
- -1 polyoxyethylene Polymers 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 2
- 230000008093 supporting effect Effects 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 230000000087 stabilizing effect Effects 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 239000007788 liquid Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 229920001577 copolymer Polymers 0.000 description 6
- 239000010440 gypsum Substances 0.000 description 6
- 229910052602 gypsum Inorganic materials 0.000 description 6
- 230000001976 improved effect Effects 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000011499 joint compound Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- 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
Landscapes
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of high-performance ball clay for ceramic sanitary ware, which comprises the following steps: 1) Preparing raw materials; 2) Mixing and proportioning kaolin, raw ore mud and secondary clay in raw materials, adding water to form slurry, removing impurities, and adding calcium chloride to obtain high-purity slurry; 3) And adding the dispergation compound into the high-purity slurry, uniformly mixing, and performing filter pressing and dehydration. The high-performance ball clay has a nano skeleton structure with supporting and stabilizing functions in the high-performance ball clay, so that the ball clay can keep the structure stable when being subjected to an external force, has good strength, can promote the fluidity of ceramic slurry to be increased when being applied to ceramic products, achieves the aim of high degumming effect, and ensures that water in the ceramic slurry is easily absorbed under the action of capillary force, so that the high-performance ball clay has good slurry absorption capacity, thereby being beneficial to improving the quality of the ceramic products and promoting the rapid high-quality development of the ceramic industry.
Description
Technical Field
The invention relates to the technical field of ceramic raw materials, in particular to a preparation method of high-performance ball clay for ceramic sanitary ware.
Background
The ball clay of the ceramic sanitary ware is specially applied to the production of the ceramic sanitary ware, and has fine particles, so that the natural particle shape is kept, and the ball clay has strong ion exchange capacity and can improve the performance of slurry; the high-strength and high-plasticity composite material meets the grouting requirements of large and complex products, and has high strength, good plasticity and relatively low sintering temperature. Due to these features, ball clay plays a very critical role in ceramic sanitary ware.
For example, the invention patent with publication number CN101844913A discloses a preparation method of ball clay for high-grade sanitary ware, which takes black mud, plaster and kaolin as raw materials to prepare the ball clay, overcomes the defects caused by the change of the raw material components due to the content of organic impurities and sand in the ball clay, and forms the ball clay with stable whiteness, strength and viscosity and good grouting fluidity, and can be widely applied to the high-grade ceramic industry; although the ball clay obtained by the process method has good fluidity, the slurry absorption performance of the formed ball clay is poor, the strength of the ceramic cannot be obviously improved when the ball clay is applied to the ceramic, and the fluidity of the ball clay cannot meet the development requirements of the modern ceramic industry because particles in the raw materials have different charges and have the tendency of adsorption and agglomeration, the fluidity can be further improved by adding a deflocculant outside, but the adsorption quantity of the deflocculant on clay particles in the ceramic is limited, so that the electrostatic repulsion among the clay particles is weak, the high-efficiency dispersion of the clay particles cannot be promoted, the comprehensive performance of the ball clay is poor, and the requirements of increasingly developed high-grade ceramics on the quality of the ball clay cannot be met.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of high-performance ball clay for ceramic sanitary ware, the high-performance ball clay has a nano skeleton structure with supporting and stabilizing functions inside, so that the ball clay can keep the structure stable when being subjected to external force, thereby having good strength and meeting the requirement of high strength.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of high-performance ball clay for ceramic sanitary ware specifically comprises the following steps:
1) Preparing raw materials, weighing kaolin, raw slime, secondary clay, calcium chloride, a peptizing compound and water;
2) Mixing and proportioning kaolin, raw ore mud and secondary clay, adding water, fully stirring and mixing to form slurry, removing impurities by using a vibrating screen, adding calcium chloride, and settling to obtain high-purity slurry;
3) And adding the peptized compound into the high-purity slurry, uniformly mixing, and performing filter pressing and dehydration on the uniformly mixed material to obtain the required high-performance ball clay.
As a further preferable scheme of the invention, the raw materials comprise, by weight, 15-30 parts of kaolin, 10-16 parts of raw ore mud, 8-12 parts of secondary clay, 0.4-0.8 part of calcium chloride, 2-4 parts of dispergation compound and 20-28 parts of water.
As a further preferable embodiment of the present invention, the preparation method of the dispergation compound is as follows:
adding sodium bisulfite into deionized water, fully stirring for dissolving, heating, adding acrylic acid, sodium methallyl sulfonate and ammonium persulfate, uniformly mixing, adding porous fiber composite gel, keeping the temperature for reaction for 2-5h, naturally cooling after the reaction is finished, and adjusting the pH value to 7.5-8.0 by using a sodium hydroxide solution to obtain the dispergation compound.
As a further preferable embodiment of the present invention, the usage ratio of the sodium bisulfite, the deionized water, the acrylic acid, the sodium methallyl sulfonate, the ammonium persulfate and the porous fiber composite gel is (3-6) g: (150-260) mL: (38-45) g: (8-13) g: (0.3-0.8) g: (8-15) g;
the heating temperature is 50-56 ℃;
naturally cooling to 40-43 ℃;
the concentration of the sodium hydroxide solution is 30-35wt%.
As a further preferable embodiment of the present invention, the preparation method of the porous fiber composite gel is as follows:
1) Mixing and stirring ethyl orthosilicate, water, ethanol and anhydrous oxalic acid until the mixture is clear to obtain silicon dioxide sol, crushing a silicon dioxide fiber membrane, dispersing the silicon dioxide fiber membrane into a polyethylene oxide solution, adding the silicon dioxide sol, homogenizing to obtain a silicon dioxide fiber dispersion solution, and calcining at high temperature for 2-5 hours after freeze drying to obtain silicon dioxide fiber aerogel;
2) Adding anhydrous oxalic acid into a mixed solution consisting of dimethyl sulfoxide and water, stirring until the anhydrous oxalic acid is completely dissolved, adding methyltrimethoxysilane, stirring for 30-50min, dripping ammonia water, uniformly mixing, adding porous nano fibers, and dispersing uniformly to obtain a mixed sol;
3) Adding the silicon dioxide fiber aerogel into the mixed sol, fully stirring, sealing in a container, putting into a drying oven for heat preservation, taking out the product, performing solvent replacement by using ethanol, drying, transferring into a calcining furnace, calcining at high temperature, and crushing to obtain the porous fiber composite gel.
As a further preferable embodiment of the present invention, in the step 1), the amount ratio of ethyl orthosilicate, water, ethanol and anhydrous oxalic acid in the silica sol is (1-5) g: (4-15) g: (10-30) g: (0.01-0.05) g;
the dosage proportion of the silica fiber membrane, the polyethylene oxide solution and the silica sol is (1-3) g: (200-500) g: (0.26-0.32) g;
the concentration of the polyoxyethylene solution is 0.01-0.03wt%;
the high-temperature calcination temperature is 800-900 ℃.
As a further preferable embodiment of the present invention, in the step 2), the ratio of the amount of the anhydrous oxalic acid, dimethyl sulfoxide, water, methyltrimethoxysilane, ammonia water and porous nanofiber is (0.34-0.45) g: (170-190) g: (52-60) g: (2-5) g: (1-3) mL: (5-10) g;
the concentration of the ammonia water is 22-25wt%.
As a further preferable embodiment of the present invention, in the step 3), the mass volume ratio of the silica fiber aerogel to the mixed sol is 1g: (10-20) mL;
the temperature in the oven is kept for 2-5h at 70-75 ℃;
the high-temperature calcination temperature is 950-1000 ℃.
As a further preferable embodiment of the present invention, the preparation method of the porous nanofiber comprises the following steps:
1) Adding polyacrylonitrile into N, N-dimethylformamide, fully stirring to obtain a dispersion solution, carrying out electrostatic spinning on the dispersion solution, and drying to obtain nano fibers;
2) And heating the nanofiber in an air atmosphere and preserving heat for 2-5h, then heating and preserving heat for 4-9h in a nitrogen atmosphere, and cooling to room temperature to obtain the porous nanofiber.
As a further preferable aspect of the present invention, in the dispersion solution, the ratio of the amount of polyacrylonitrile to N, N-dimethylformamide used is (6 to 8) g: (50-80) mL;
the electrostatic spinning parameters are as follows: the receiving distance is 15-20cm, the voltage is 8-10kV, and the flow rate is 0.02-0.05mL/min;
heating to 260-300 ℃ in the air atmosphere, wherein the heating rate is 1-3 ℃/min;
and heating to 750-800 ℃ in the nitrogen atmosphere, wherein the heating rate is 3-6 ℃/min.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, silica fiber is taken as a construction element, freezing-drying and high-temperature calcining are combined to prepare silica fiber aerogel with a stable fiber network structure, the fiber network structure can effectively transfer and disperse acting force, so that the silica fiber aerogel has good mechanical property and good resistance to external force, the silica fiber aerogel is taken as a supporting framework, and a sol impregnation method is adopted to obtain composite gel with a double-network structure, the multi-level network structure of the silica fiber aerogel is reserved in the composite gel, so that the material has good mechanical property, meanwhile, the structure of the material is stable and is not easy to damage due to the fact that the silica fiber aerogel is taken as the supporting framework, and the material has good structural stability through introducing the nano-framework structure of the silica fiber aerogel, so that the ball clay can play a better supporting and stabilizing role, the ball clay can keep the structural stability under the action of external force, so that the ball clay has good strength, and the requirement of high strength can be met; meanwhile, in order to further improve the porosity of the composite gel and improve the structural stability of the composite gel, the porous nanofiber composite gel is obtained by adding the porous nanofibers into the sol, and the introduction of the porous nanofibers can further increase the porosity of the porous fiber composite gel on one hand, so that the ball clay has a loose structure, the structure of the ceramic slurry is loose, the internal water is easily absorbed under the action of capillary force, the ball clay has good slurry absorption capacity, and meanwhile, the cross-linking density of a multilevel network structure in the porous fiber composite gel is increased by the mutual cross-linking of the porous nanofibers, so that the stability of a nanometer skeleton structure can be further improved, the resistance of the porous fiber composite gel to external force is further improved, and the strength of the ball clay is remarkably improved.
In the invention, porous fiber composite gel is used as a matrix, acrylic acid and sodium methallyl sulfonate are used as monomers, ammonium persulfate and sodium bisulfite are used as redox initiation systems, a copolymer is deposited on the porous fiber composite gel through copolymerization reaction, and the formed copolymer contains-COO - and-SO 3 - The group ionization makes the argil granule surface in the pottery go up the same kind of electric charge to form the diffusion bilayer, along with the adsorption capacity of glue breaking compound on argil granule surface increases, the bilayer structure of formation thickens gradually, make the electrostatic repulsion reinforcing between the argil granule, the static steric hindrance effect reinforcing of formation, impel its mutual dispersion, thereby make the flocculation structure disintegration of ceramic thick liquids, release the moisture that is wrapped up, thereby make the mobility of ceramic thick liquids increase, thereby reach the purpose of high glue breaking effect.
In order to promote the deposition of the copolymer on the porous fiber composite gel, in the invention, the nanofiber is obtained based on electrostatic spinning, and the porous nanofiber is obtained by high-temperature calcination in an air atmosphere and a nitrogen atmosphere, wherein in the preparation process of the porous nanofiber, nitrogen atoms are introduced into a carbon matrix through high-temperature calcination to generate more defect structures in the porous nanofiber, so that more random holes are generated in the porous nanofiber and more active sites are exposed in the porous nanofiber due to the formation of the random holes, although the mechanical property of the porous nanofiber is reduced to a certain extent, the activity of the porous fiber composite gel is improved, and more copolymer can be deposited on the porous fiber composite gel to form a dispergation compound; the copolymer with the gel-dissolving capacity is deposited on the porous fiber composite gel, and the contact area between the copolymer and the argil particles can be increased by utilizing the high specific surface area of the porous fiber composite gel, so that the adsorption of a gel-dissolving compound on the surfaces of the argil particles can be promoted, the thickness of a double-electronic-layer structure is increased, and the high fluidity of the ceramic slurry is realized.
The high-performance ball clay has a nano skeleton structure with supporting and stabilizing functions in the high-performance ball clay, so that the ball clay can keep stable in structure when being subjected to external force, has good strength and can meet the requirement of high strength.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of high-performance ball clay for ceramic sanitary ware specifically comprises the following steps:
1) Preparing raw materials according to parts by weight, weighing 15 parts of kaolin, 10 parts of raw slime, 8 parts of secondary clay, 0.4 part of calcium chloride, 2 parts of dispergation compound and 20 parts of water;
2) Mixing and proportioning kaolin, raw ore mud and secondary clay, adding water, fully stirring and mixing to form slurry, removing impurities by using a vibrating screen, adding calcium chloride, and settling to obtain high-purity slurry;
3) And adding the peptized compound into the high-purity slurry, uniformly mixing, and performing filter pressing and dehydration on the uniformly mixed material to obtain the required high-performance ball clay.
The preparation method of the dispergation compound comprises the following steps:
adding 3g of sodium bisulfite into 150mL of deionized water, fully stirring and dissolving, heating to 50 ℃, adding 38g of acrylic acid, 8g of sodium methallyl sulfonate and 0.3g of ammonium persulfate, uniformly mixing, adding 8g of porous fiber composite gel, keeping the temperature for reaction for 2 hours, after the reaction is finished, naturally cooling to 40 ℃, and adjusting the pH value to 7.5 by using 30wt% of sodium hydroxide solution to obtain the dispergation compound.
The preparation method of the porous fiber composite gel comprises the following steps:
1) Mixing and stirring 1g of tetraethoxysilane, 4g of water, 10g of ethanol and 0.01g of anhydrous oxalic acid until the mixture is clear to obtain silicon dioxide sol, crushing 1g of silicon dioxide fiber membrane, dispersing the crushed silicon dioxide fiber membrane into 200g of polyoxyethylene solution with the concentration of 0.01wt%, adding 0.26g of silicon dioxide sol, homogenizing to obtain silicon dioxide fiber dispersion liquid, freeze-drying, and calcining at the high temperature of 800 ℃ for 2 hours to obtain silicon dioxide fiber aerogel;
2) Adding 0.34g of anhydrous oxalic acid into a mixed solution consisting of 170g of dimethyl sulfoxide and 52g of water, stirring until the anhydrous oxalic acid is completely dissolved, adding 2g of methyltrimethoxysilane, stirring at 150r/min for 30min, dropwise adding 1mL of 22wt% ammonia water, uniformly mixing, adding 5g of porous nanofiber, and uniformly dispersing to obtain a mixed sol;
3) According to the mass-to-volume ratio of 1g: and 10mL, adding the silica fiber aerogel into the mixed sol, fully stirring, sealing in a container, placing in a 70 ℃ oven, preserving the temperature for 2h, taking out the product, performing solvent replacement by using ethanol, drying, transferring to a calcining furnace, calcining at a high temperature of 950 ℃ for 3h, and crushing to obtain the porous fiber composite gel.
The preparation method of the porous nanofiber comprises the following steps:
1) Adding 6g of polyacrylonitrile into 50mLN, N-dimethylformamide, fully stirring to obtain a dispersion solution, carrying out electrostatic spinning on the dispersion solution, setting the acceptance distance to be 15cm, carrying out electrostatic spinning at the flow rate of 8kV and 0.02mL/min, and drying the obtained fiber in an oven at 60 ℃ for 15 hours to obtain the nanofiber;
2) Heating the nanofiber to 260 ℃ in the air atmosphere, controlling the heating rate to be 1 ℃/min, preserving heat for 2h, then heating to 750 ℃ in the argon atmosphere, controlling the heating rate to be 3 ℃/min, preserving heat for 4h, and cooling to room temperature to obtain the porous nanofiber.
Example 2
A preparation method of high-performance ball clay for ceramic sanitary ware specifically comprises the following steps:
1) Preparing raw materials according to parts by weight, weighing 25 parts of kaolin, 12 parts of raw slime, 10 parts of secondary clay, 0.5 part of calcium chloride, 3 parts of dispergation compound and 24 parts of water;
2) Mixing and proportioning kaolin, raw ore mud and secondary clay, adding water, fully stirring and mixing to form slurry, removing impurities by using a vibrating screen, adding calcium chloride, and settling to obtain high-purity slurry;
3) And adding the peptized compound into the high-purity slurry, uniformly mixing, and performing filter pressing and dehydration on the uniformly mixed material to obtain the required high-performance ball clay.
The preparation method of the dispergation compound comprises the following steps:
adding 5g of sodium bisulfite into 200mL of deionized water, fully stirring and dissolving, heating to 53 ℃, adding 42g of acrylic acid, 10g of sodium methallyl sulfonate and 0.5g of ammonium persulfate, uniformly mixing, adding 12g of porous fiber composite gel, keeping the temperature and reacting for 3h, after the reaction is finished, naturally cooling to 42 ℃, and adjusting the pH value to 7.5 by using 32wt% of sodium hydroxide solution to obtain the dispergation compound.
The preparation method of the porous fiber composite gel comprises the following steps:
1) Mixing and stirring 3g of ethyl orthosilicate, 10g of water, 20g of ethanol and 0.03g of anhydrous oxalic acid until the mixture is clear to obtain silicon dioxide sol, crushing 2g of silicon dioxide fiber membrane, dispersing the crushed silicon dioxide fiber membrane into 400g of polyoxyethylene solution with the concentration of 0.02wt%, adding 0.3g of silicon dioxide sol, homogenizing to obtain silicon dioxide fiber dispersion liquid, and calcining the silicon dioxide fiber dispersion liquid at 850 ℃ for 3 hours after freeze drying to obtain silicon dioxide fiber aerogel;
2) Adding 0.42g of anhydrous oxalic acid into a mixed solution consisting of 180g of dimethyl sulfoxide and 58g of water, stirring until the anhydrous oxalic acid is completely dissolved, adding 3g of methyltrimethoxysilane, stirring at 200r/min for 40min, dropwise adding 2mL of 23wt% ammonia water, uniformly mixing, adding 8g of porous nanofiber, and uniformly dispersing to obtain a mixed sol;
3) According to the mass-to-volume ratio of 1g:15mL, adding the silica fiber aerogel into the mixed sol, fully stirring, sealing in a container, placing in a 72 ℃ oven, preserving the temperature for 3h, taking out the product, performing solvent replacement by using ethanol, drying, transferring to a calcining furnace, calcining at a high temperature of 980 ℃ for 5h, and crushing to obtain the porous fiber composite gel.
The preparation method of the porous nanofiber comprises the following steps:
1) Adding 7g of polyacrylonitrile into 60mLN, N-dimethylformamide, fully stirring to obtain a dispersion solution, carrying out electrostatic spinning on the dispersion solution, setting the acceptance distance to be 18cm, carrying out electrostatic spinning at the flow rate of 9kV and 0.03mL/min, and drying the obtained fiber in an oven at 70 ℃ for 16 hours to obtain the nanofiber;
2) Heating the nanofiber to 280 ℃ in the air atmosphere, controlling the heating rate to be 2 ℃/min, preserving heat for 3h, then heating to 780 ℃ in the argon atmosphere, controlling the heating rate to be 5 ℃/min, preserving heat for 8h, and cooling to room temperature to obtain the porous nanofiber.
Example 3
A preparation method of high-performance ball clay for ceramic sanitary ware specifically comprises the following steps:
1) Preparing raw materials according to parts by weight, weighing 30 parts of kaolin, 16 parts of raw slime, 12 parts of secondary clay, 0.8 part of calcium chloride, 4 parts of dispergation compound and 28 parts of water;
2) Mixing and proportioning kaolin, raw ore mud and secondary clay, adding water, fully stirring and mixing to form slurry, removing impurities by using a vibrating screen, adding calcium chloride, and settling to obtain high-purity slurry;
3) And adding the peptization compound into the high-purity slurry, uniformly mixing, and performing filter pressing and dehydration on the uniformly mixed material to obtain the required high-performance ball clay.
The preparation method of the dispergation compound comprises the following steps:
adding 6g of sodium bisulfite into 260mL of deionized water, fully stirring for dissolving, heating to 56 ℃, adding 45g of acrylic acid, 13g of sodium methallyl sulfonate and 0.8g of ammonium persulfate, uniformly mixing, adding 15g of porous fiber composite gel, keeping the temperature for reaction for 5 hours, naturally cooling to 43 ℃ after the reaction is finished, and adjusting the pH value to 8.0 by using 35wt% of sodium hydroxide solution to obtain the dispergation compound.
The preparation method of the porous fiber composite gel comprises the following steps:
1) Mixing and stirring 5g of ethyl orthosilicate, 15g of water, 30g of ethanol and 0.05g of anhydrous oxalic acid until the mixture is clear to obtain silicon dioxide sol, crushing 3g of silicon dioxide fiber membrane, dispersing the crushed silicon dioxide fiber membrane into 500g of polyoxyethylene solution with the concentration of 0.03wt%, adding 0.32g of silicon dioxide sol, homogenizing to obtain silicon dioxide fiber dispersion liquid, and calcining the silicon dioxide fiber dispersion liquid at the high temperature of 900 ℃ for 5 hours after freeze drying to obtain silicon dioxide fiber aerogel;
2) Adding 0.45g of anhydrous oxalic acid into a mixed solution consisting of 190g of dimethyl sulfoxide and 60g of water, stirring until the anhydrous oxalic acid is completely dissolved, adding 5g of methyltrimethoxysilane, stirring at 300r/min for 50min, dropwise adding 3mL of 25wt% ammonia water, uniformly mixing, adding 10g of porous nanofiber, and uniformly dispersing to obtain a mixed sol;
3) According to the mass-to-volume ratio of 1g: and 20mL, adding the silica fiber aerogel into the mixed sol, fully stirring, sealing in a container, putting into a 75 ℃ oven, preserving the temperature for 5h, taking out the product, performing solvent replacement by using ethanol, drying, transferring to a calcining furnace, calcining at a high temperature of 1000 ℃ for 6h, and crushing to obtain the porous fiber composite gel.
The preparation method of the porous nanofiber comprises the following steps:
1) Adding 8g of polyacrylonitrile into 80mLN, N-dimethylformamide, fully stirring to obtain a dispersion solution, carrying out electrostatic spinning on the dispersion solution, setting the acceptance distance to be 20cm, carrying out electrostatic spinning at the flow rate of 10kV and 0.05mL/min, and drying the obtained fiber in an oven at the temperature of 80 ℃ for 18 hours to obtain the nanofiber;
2) Heating the nanofiber to 300 ℃ in the air atmosphere, controlling the heating rate to be 3 ℃/min, preserving heat for 5h, then heating to 800 ℃ in the argon atmosphere, controlling the heating rate to be 6 ℃/min, preserving heat for 9h, and cooling to room temperature to obtain the porous nanofiber.
Comparative example 1: this comparative example is essentially the same as example 1, except that no porous fiber composite gel was added during the preparation of the debonded composite.
Comparative example 2: this comparative example is substantially the same as example 1 except that the porous nanofiber was not added in the preparation of the porous fiber composite gel.
Comparative example 3: this comparative example is substantially the same as example 1 except that nanofibers are used instead of porous nanofibers in the preparation of the porous fiber composite gel.
Comparative example 4: this comparative example is essentially the same as example 1 except that the dispergation compound was not included.
Comparative example 5: this comparative example is essentially the same as example 1, except that an equal amount of the dispergator (water glass is selected) was used instead of the dispergated compound.
Test:
using the preparation methods disclosed in examples 1 to 3 and comparative examples 1 to 5, materials were obtained and dehydrated by pressure filtration to obtain slurry samples having a concentration of 360g/200mL, and formation tests were carried out on the slurry samples, and the results are shown in Table 1.
And (3) fluidity measurement: filling a slurry sample into a 4-viscometer (100 mL), pressing a stopwatch while opening an outlet, and recording stopwatch data, namely the fluidity s of the slurry;
and (3) measuring the pulp sucking speed: preparing a gypsum crucible (with the height of 8cm, the inner diameter of 4cm and the wall thickness of 3 cm) from the stir-fried semi-hydrated gypsum by adopting a gypsum crucible method, and drying at 70 ℃; injecting a slurry sample into a crucible, measuring and calculating the initial height mm of the slurry, standing for 45min, measuring the final height mm of the slurry again, performing 5 parallel tests, and calculating an average value, wherein the calculation formula is as follows: the slurry suction speed V = (H1-H2)/t; in the formula, H1 is the height of slurry in the gypsum crucible before standing, H2 is the height of slurry in the gypsum crucible after standing, and t is the standing time s after the slurry is injected into the crucible;
dry flexural strength: pouring the test strip with a gypsum mold for the slurry sample, wherein the length of the test strip is 100mm, the width of the test strip is 10mm, the thickness of the test strip is 10mm, putting the test strip into an oven for drying, placing the test strip on a support with the span of 60mm, and measuring the bending data of the test strip by using an electronic universal tester, namely the bending strength Mpa of the test strip.
As can be seen from the table 1, the ball clay disclosed by the invention is excellent in comprehensive performance, and has good fluidity, slurry absorption speed and drying rupture strength, so that the ball clay is beneficial to improving the quality of ceramic products and promoting the rapid high-quality development of the ceramic industry.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. A preparation method of high-performance ball clay for ceramic sanitary ware is characterized by comprising the following steps:
1) Preparing raw materials, weighing kaolin, raw slime, secondary clay, calcium chloride, a peptizing compound and water;
2) Mixing and proportioning kaolin, raw ore mud and secondary clay, adding water, fully stirring and mixing to form slurry, removing impurities by using a vibrating screen, adding calcium chloride, and settling to obtain high-purity slurry;
3) And adding the peptized compound into the high-purity slurry, uniformly mixing, and performing filter pressing and dehydration on the uniformly mixed material to obtain the required high-performance ball clay.
2. The method for preparing the high-performance ball clay for the ceramic sanitary ware according to claim 1, wherein the raw materials comprise, by weight, 15-30 parts of kaolin, 10-16 parts of raw slime, 8-12 parts of secondary clay, 0.4-0.8 part of calcium chloride, 2-4 parts of a dispergation compound and 20-28 parts of water.
3. The method for preparing the high-performance ball clay for the ceramic sanitary appliance according to claim 1, wherein the peptized compound is prepared by the following steps:
adding sodium bisulfite into deionized water, fully stirring for dissolving, heating, adding acrylic acid, sodium methallyl sulfonate and ammonium persulfate, uniformly mixing, adding porous fiber composite gel, keeping the temperature for reaction for 2-5h, naturally cooling after the reaction is finished, and adjusting the pH value to 7.5-8.0 by using a sodium hydroxide solution to obtain the dispergation compound.
4. The method for preparing the high-performance ball clay for the ceramic sanitary appliance according to claim 3, wherein the dosage ratio of the sodium bisulfite, the deionized water, the acrylic acid, the sodium methallyl sulfonate, the ammonium persulfate and the porous fiber composite gel is (3-6) g: (150-260) mL: (38-45) g: (8-13) g: (0.3-0.8) g: (8-15) g;
the heating temperature is 50-56 ℃;
naturally cooling to 40-43 ℃;
the concentration of the sodium hydroxide solution is 30-35wt%.
5. The preparation method of the high-performance ball clay for the ceramic sanitary ware according to claim 1, wherein the preparation method of the porous fiber composite gel is as follows:
1) Mixing and stirring ethyl orthosilicate, water, ethanol and anhydrous oxalic acid until the mixture is clear to obtain silicon dioxide sol, crushing a silicon dioxide fiber membrane, dispersing the silicon dioxide fiber membrane into a polyethylene oxide solution, adding the silicon dioxide sol, homogenizing to obtain a silicon dioxide fiber dispersion solution, and calcining at high temperature for 2-5 hours after freeze drying to obtain silicon dioxide fiber aerogel;
2) Adding anhydrous oxalic acid into a mixed solution consisting of dimethyl sulfoxide and water, stirring until the anhydrous oxalic acid is completely dissolved, adding methyltrimethoxysilane, stirring for 30-50min, dropwise adding ammonia water, uniformly mixing, adding porous nanofiber, and uniformly dispersing to obtain a mixed sol;
3) Adding the silica fiber aerogel into the mixed sol, fully stirring, sealing in a container, putting in a drying oven for heat preservation, taking out a product, performing solvent replacement by using ethanol, drying, transferring to a calcining furnace, calcining at high temperature, and crushing to obtain the porous fiber composite gel.
6. The method for preparing the high-performance ball clay for the ceramic sanitary ware according to claim 5, wherein in the step 1), the usage ratio of the ethyl orthosilicate, the water, the ethanol and the anhydrous oxalic acid in the silica sol is (1-5) g: (4-15) g: (10-30) g: (0.01-0.05) g;
the dosage proportion of the silica fiber membrane, the polyoxyethylene solution and the silica sol is (1-3) g: (200-500) g: (0.26-0.32) g;
the concentration of the polyoxyethylene solution is 0.01-0.03wt%;
the high-temperature calcination temperature is 800-900 ℃.
7. The method for preparing high-performance ball clay for ceramic sanitary wares according to claim 5, wherein in the step 2), the ratio of the amount of the anhydrous oxalic acid, the dimethyl sulfoxide, the water, the methyltrimethoxysilane, the ammonia water and the porous nanofibers is (0.34-0.45) g: (170-190) g: (52-60) g: (2-5) g: (1-3) mL: (5-10) g;
the concentration of the ammonia water is 22-25wt%.
8. The method for preparing the high-performance ball clay for the ceramic sanitary appliance according to claim 5, wherein in the step 3), the mass-to-volume ratio of the silica fiber aerogel to the mixed sol is 1g: (10-20) mL;
the temperature in the oven is kept for 2-5h at 70-75 ℃;
the high-temperature calcination temperature is 950-1000 ℃.
9. The method for preparing the high-performance ball clay for the ceramic sanitary appliance according to claim 1, wherein the preparation method of the porous nanofiber comprises the following steps:
1) Adding polyacrylonitrile into N, N-dimethylformamide, fully stirring to obtain a dispersion solution, carrying out electrostatic spinning on the dispersion solution, and drying to obtain nano fibers;
2) And heating the nanofiber in an air atmosphere and preserving heat for 2-5h, then heating and preserving heat for 4-9h in a nitrogen atmosphere, and cooling to room temperature to obtain the porous nanofiber.
10. The method for preparing high-performance ball clay for ceramic sanitary wares according to claim 9, wherein the dosage ratio of polyacrylonitrile to N, N-dimethylformamide in the dispersion solution is (6-8) g: (50-80) mL;
the electrostatic spinning parameters are as follows: the receiving distance is 15-20cm, the voltage is 8-10kV, and the flow rate is 0.02-0.05mL/min;
heating to 260-300 ℃ in the air atmosphere, wherein the heating rate is 1-3 ℃/min;
and heating to 750-800 ℃ in the nitrogen atmosphere, wherein the heating rate is 3-6 ℃/min.
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