CN111454046B - Grouting ceramic slurry preparation method, prepared slurry and grouting ceramic - Google Patents
Grouting ceramic slurry preparation method, prepared slurry and grouting ceramic Download PDFInfo
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Abstract
The invention relates to the field of grouting ceramics, and discloses a grouting ceramic slurry preparation method, prepared slurry and grouting ceramics, wherein the grouting ceramic slurry preparation method aims at the preparation of the grouting ceramic slurry of a quartz, kaolin, ball clay and calcined coke system, and after the green body is prepared by grouting the grouting ceramic slurry, the effect of reducing the sintering temperature of the green body is achieved, and meanwhile, the ceramic yield is improved, and the occurrence probability of karst cave defects is reduced; the obtained grouting ceramic has white green body color, low firing temperature and high yield.
Description
Technical Field
The invention relates to the field of grouting ceramic preparation, in particular to a grouting ceramic slurry preparation method, prepared slurry and grouting ceramic.
Background
The grouting ceramic is obtained by producing a blank by a grouting forming method and firing the blank. The slip casting method is that the slurry made by the blank is injected into the plaster model, the water in the slurry near the inner wall of the plaster model is sucked by the porous plaster by utilizing the water absorption of the plaster, and then a mud layer with the same shape as the inner wall of the plaster model is formed on the inner wall of the plaster model, the mud layer is thickened along with the increase of time, after the mud layer stays for a period of time, the surplus slurry in the process of throwing is poured, and the mud layer near the inner wall of the plaster model is remained in the plaster model; after a further period of time, the mud layer naturally shrinks and separates from the gypsum pattern, and the formed green body can be removed. Therefore, the components of the slurry become another important determining factor besides the firing temperature in the production process of the grouting ceramics, and influence the profile condition of the blank and the quality of the ceramics obtained after firing.
Most of the existing slurry is made of clay, pottery clay, talc and the like, for example, the Chinese patent with the publication number of CN105712697B entitled "sanitary ceramic slurry and preparation process thereof" discloses ceramic slurry which mainly comprises the following raw materials in parts by weight: 30-70 parts of illite clay, 5-15 parts of kaolin, 6-14 parts of ball clay, 8-13 parts of potash feldspar, 5-10 parts of pyrophyllite, 5-10 parts of sericite, 0.1-3 parts of dolomite and 40-45 parts of water. In the prior art, in order to reduce the ceramic firing temperature, the slurry is improved, such as mica, marble and the like are added, and the ceramic sintering temperature is reduced by reducing the average melting point of solids in a green body during application. However, due to the doping of the raw material with low melting point, molten holes (irregular colored or colorless pits appear on the surface of the blank) appear in the fired ceramic, and the phenomenon of the molten holes is increased along with the increase of the temperature control fluctuation.
Proportioning by using slurry: 13-15 parts by mass of quartz, 10-21 parts by mass of kaolin, 32-36 parts by mass of ball clay and 33-38 parts by mass of calcined flint clay are taken as examples, 7-8 parts by mass of sericite is added, the sintering temperature is reduced from 1220 ℃ to 1120 ℃ at present, but the rejection rate after the original sintering is 7-8% and is increased to 10-15%, wherein the proportion of fusion holes in the waste is increased from 13-15% to 34-40%, so that the yield is reduced, and if the process temperature is improperly controlled, the sintering temperature is increased to 1150 ℃, the rejection rate can be further increased, and the proportion of fusion holes in the waste reaches 38-45%.
Therefore, the use of the technique for lowering the sintering melting point is limited, and further improvement thereof is desired.
Disclosure of Invention
Aiming at the defects in the prior art, the first object of the invention is to provide a preparation method of ceramic slurry for grouting, which has the effect of reducing the sintering temperature of ceramic, improves the yield of the ceramic and reduces the occurrence probability of the karst cave defect;
the second purpose of the invention is to provide ceramic slurry for grouting, the sintering temperature of a green blank obtained by grouting production is reduced, energy is saved, and the yield is high;
the third purpose of the invention is to provide the grouting ceramic, which has white green body color, low firing temperature and high yield.
In order to achieve the first object, the invention provides the following technical scheme:
a preparation method of ceramic slurry for grouting comprises the following steps of:
quartz, wherein the quartz is powder;
the waste porcelain powder is powder, and the component in the waste porcelain powder is SiO2：66.31～67.38wt％，Al2O3：24.06～25.13wt％，TiO2：0.64～0.75wt％，Fe2O3：1.44～1.76wt％，CaO：0.64～1.07wt％，MgO：0.48～0.7wt％，K2O：3.1～3.53wt％，Na2O：1.18～1.50wt％；
Kaolin, wherein the kaolin is powder;
ball soil, wherein the ball soil is powder;
calcining a flint clay, wherein the flint clay is powder, and the flint clay is calcined flint clay;
the low melting material is powder mica, the maximum particle size is less than 20 mu m, the total content of Fe and Cu of the mica is less than 3.6wt%, and the water content is less than 1 wt%;
the main components of the firing auxiliary materials are one or more of aluminum hydroxide and magnesium hydroxide, the using amount of the firing auxiliary materials is related to the using amount of the low-melting-point material, and the volume-to-low-melting-point volume ratio of the firing auxiliary materials is 1.02 after one or more of aluminum oxide and magnesium oxide are used as the firing auxiliary materials;
the preparation method comprises the following steps of,
s1, mixing the low melting materials and the firing auxiliary materials, uniformly mixing, then heating and firing at 960-980 ℃, wherein the firing time is 30min, and crushing after the fired product is cooled to obtain a mixed firing material with the particle size of 8 mu m;
s2: mixing 13-15 parts of quartz, 8-10 parts of waste porcelain powder, 5-8 parts of kaolin, 32-36 parts of ball clay, 33-38 parts of calcined flint clay, 14-18 parts of mixed sintering material and water according to the parts by weight, and performing ball milling to obtain coarse grinding slurry,
s3: keeping stirring the rough grinding slurry, and carrying out ageing for 3 days, supplementing water to the rough grinding slurry according to the water evaporation capacity of the rough grinding slurry during ageing, and keeping the volume of the slurry stable to obtain the slurry for grouting ceramics.
By adopting the technical scheme, the definition explanation is given to some nouns used in the invention:
base material: the ceramic slurry occupies the raw materials of solid components in the ceramic slurry, and has important influence on obtaining the physicochemical properties of the ceramic such as color, strength, density and the like by firing;
green body: the ceramic slurry is injected into a gypsum mould for dehydration and demoulding to obtain the product;
blank body: the qualified green body is obtained by high-temperature firing and sintering;
ceramic: the qualified green body is obtained by high-temperature firing and sintering, or is obtained by continuous firing after the qualified green body is glazed;
quartz, waste ceramic powder, kaolin, ball clay, calcined flint clay, low-melting materials and sintering auxiliary materials are used as base materials of the ceramic slurry, and the white background color of the green body is determined by the quartz, the waste ceramic powder, the kaolin, the ball clay and the calcined flint clay, so that the color purity of the green body is improved, and meanwhile, the requirement on the surface flaws of the green body is further improved;
waste ceramic powder is added, and the broken components of the waste ceramic are partially recycled, so that the generation of waste materials is reduced, and the environment is protected;
the low-melting material of the mica is added, the total content of Fe and Cu of the mica is required to be less than 3.6wt%, ceramic spots and flaws caused by adding a compound carrying a large amount of iron and a compound of copper into the low-melting material are avoided, and the temperature required by integral sintering of a mud blank obtained by grouting is reduced;
in the preparation process, the low melting material and the sintering auxiliary material are sintered together, free water, crystal water and most of bound water in the low melting material are removed in the sintering process, and the part of water is bound in the low melting material minerals or mineral particles and is water which is difficult to remove by a gypsum mould, so that the original water content of the low melting material is reduced;
the sintering auxiliary material is selected from aluminum hydroxide or magnesium hydroxide, the adsorbability of the aluminum hydroxide or magnesium hydroxide is better, the aluminum hydroxide or magnesium hydroxide is better in mixing compatibility with the low-melting material, when the aluminum hydroxide or magnesium hydroxide is mixed and sintered, the sintering auxiliary material is dehydrated to form an oxide firstly, a large number of pore channels are left in the moisture release process, the low-melting material is continuously lifted to be molten along with the temperature and then permeates into the oxide along the pore channels, the aluminum hydroxide or magnesium hydroxide and the oxide are mixed and sintered compactly, the pores in the mixed sintering material are reduced, and the permeability of the mixed sintering material is reduced;
meanwhile, the sintering temperature reaches the melting requirement of the low-melting material and is far lower than the melting temperature of the oxide, and moisture is released and volatilized in the process of forming the oxide by dehydrating the sintering auxiliary material, so that the compactness between oxide particles is poor, the oxide collapses along with sintering, the oxide wraps the molten low-melting material to protect the low-melting material, a barrier layer is formed by partially or integrally wrapping the surface of the low-melting material, and the possibility of water absorption of the low-melting material in the mixed sintering material is reduced; on the other hand, the crushing surface is also cracked along the interface of oxide-oxide when the mixed sintering material is crushed;
the components of the low-melting material in the green body are homogenized after the low-melting material is sintered in the front, the water content is reduced, the subsequent water absorption is less, the phenomenon that the local volume changes are not uniform to form depressions due to non-uniform components is avoided when the low-melting material is melted in the firing process of the green body, the surface depressions due to the fact that water is vaporized, blown air is firstly released and then collapsed during the melting of the low-melting material are avoided, the depression degree of the molten holes generated on the surface of the green body due to the addition of the low-melting material is further reduced, the original possibly generated deeper molten holes are converted into shallower molten holes, and the originally possibly generated shallower molten holes are eliminated;
the oxide obtained after the auxiliary sintering material is dehydrated and decomposed can also improve the strength, the corrosion resistance and the like of the green body, and especially the color and the appearance are obviously improved;
on the other hand, the low-melting material and the sintering auxiliary material are sintered together and then crushed to obtain a mixed sintering material, the low-melting material in the mixed sintering material and an oxide obtained by dehydrating the sintering auxiliary material are kept in a mixed state, the existing mode of the original sheet structure of the low-melting material is destroyed, so that the low-melting material is uniformly mixed with other solid components and water in the ceramic slurry, the low-melting material in the ceramic slurry is prevented from being attached to each other to form large aggregated particles or aggregated blocks, the low-melting material is prevented from melting to flow around to form a recess in situ when the density of the local low-melting material in a green body is too high during sintering, and the possibility of generating defects of a molten hole is further reduced.
The present invention in a preferred example may be further configured to: the mixing method of the low-melting materials and the sintering auxiliary materials in the step S1 is as follows: adding low-melting powder into one or mixed solution of aluminum chloride and magnesium chloride, stirring to make the low-melting powder roll in the solution, adding pH regulator to make Al exist correspondingly3+、Mg2+One or more of them are precipitated in the form of hydroxide gel, coated with low-melting powder particles, filtered, washed with water, dried to remove free water, and then fired in S1.
By adopting the technical scheme, the low-melting-material powder is dispersed in the chloride solution to serve as a 'nucleus' for promoting the hydroxide (auxiliary sintering material) to be separated out, the auxiliary sintering material is separated out by taking the low-melting-material powder as a center and coats the low-melting-material powder, the coating effect of the auxiliary sintering material on the low-melting-material powder is improved, the coating effect of oxides in the mixed sintering material on the low melting material is improved, the effect of inhibiting the low melting material from absorbing water again is improved, and the dilution and dispersion effects of the low melting material in the mixed sintering material are improved.
The present invention in a preferred example may be further configured to: and after the low-melting material is screened, powder with the particle size of less than 2 mu m is screened and separated by adopting water washing, and the powder with the particle size of less than 2 mu m in the low-melting material accounts for less than 2 wt%.
By adopting the technical scheme, the low-melting material can generate particles with the particle size of less than 2 mu m in the crushing and iron screening processes, the dispersing effect of the excessively fine low-melting material particles in the chlorination solution is poor, the excessively fine low-melting material powder can be gathered and bonded into loose large particles, and free water is entrained in the large particles and is difficult to remove; large particles are sintered after being coated by the auxiliary sintering material, a cavity formed in the original position is larger than the fused volume of the low melting material, so that the sintering uniformity of the mixed sintering material is poor, the number of tiny holes is increased, the diffusion and permeation effect of the obtained sintering powder is reduced when the obtained sintering powder is used for sintering a blank, the shrinkage of the obtained ceramic is inconsistent, and the rejection rate of cracking is increased;
the low melting material powder and the auxiliary sintering material powder are dispersed in the auxiliary sintering material precursor chloride solution, and then the auxiliary sintering material is separated out and mixed, so that most of particles with the particle size smaller than 2 mu m are separated from the low melting material powder and the auxiliary sintering material powder, and the rejection rate of inconsistent ceramic shrinkage is prevented from being increased.
The present invention in a preferred example may be further configured to: the slurry raw material comprises, by mass, 13 parts of quartz, 8 parts of waste porcelain powder, 5 parts of kaolin, 32 parts of ball clay, 35 parts of calcined flint clay and 18 parts of mixed sintering material, wherein the mixed sintering material is prepared by directly mixing and sintering low-melting material and sintering auxiliary material according to the mass ratio of 0.4331.
The present invention in a preferred example may be further configured to: the slurry comprises the raw materials of, by mass, 15 parts of quartz, 9 parts of waste porcelain powder, 7 parts of kaolin, 35 parts of ball clay, 34 parts of calcined flint clay and 18 parts of mixed sintering materials, wherein the sintering auxiliary material is aluminum hydroxide.
In order to achieve the second object, the invention provides the following technical scheme:
the ceramic slurry for grouting is prepared by the preparation method of the ceramic slurry for grouting.
In order to achieve the third object, the invention provides the following technical solutions:
the grouting ceramic comprises a blank body, wherein the grouting slurry used by the blank body is the ceramic slurry for grouting.
In conclusion, the invention has the following beneficial effects:
1. when preparing the grouting ceramic slurry, sintering the low melting material and the sintering auxiliary material together, mixing the oxide dehydrated and decomposed by the sintering auxiliary material with the molten low melting material to obtain a densely sintered mixed sintering material, reducing the original water content of the low melting material in the sintering process, and coating the molten low melting material by the oxide in the obtained mixed sintering material, the low-melting material is separated, the possibility of water absorption of the low-melting material in the mixed sintering material is reduced, the components of the low-melting material in the green body are homogenized after the low-melting material is sintered in the front, the water content is reduced, the subsequent water absorption is less, the problem that the low-melting material is uneven in the green body sintering process, the surface depression is formed due to the fact that the low-melting material is vaporized, blown first and released and then collapsed when the low-melting material is melted is avoided, and the depression degree of the molten holes generated on the surface of the green body due to the addition of the low-melting material is reduced, converting the originally possibly generated deeper molten holes into shallower molten holes, and eliminating the originally possibly generated shallower molten holes;
2. the low melting material and the sintering auxiliary material are sintered together and then crushed to obtain a mixed sintering material, the oxide obtained by dehydrating the low melting material and the sintering auxiliary material in the mixed sintering material keeps a mixed state, the existing mode of the original sheet structure of the low melting material is damaged, the low melting material is convenient to be uniformly mixed with other solid components and water in the ceramic slurry, the low melting material in the ceramic slurry is prevented from being attached to each other to form large aggregated particles or aggregated blocks, the low melting material is prevented from melting to flow around to form a recess in situ when the density of the local low melting material in a green body is too high for sintering, and then the possibility of generating a fusion hole defect is reduced;
3. the mixing mode of the low melting materials and the sintering auxiliary materials adopts the low melting material powder dispersed in the auxiliary sintering material precursor chloride (one or more of aluminum chloride and magnesium chloride) solution as a 'nucleus' for promoting the precipitation of the auxiliary sintering materials, improves the coating effect of the sintering auxiliary materials on the low melting material powder, thereby improving the coating effect of oxides in the mixed sintering materials on the low melting materials, improving the effect of inhibiting the low melting materials from absorbing water again and improving the effect of diluting and dispersing the low melting materials in the mixed sintering materials, further improving the green body sintering yield and further reducing the occurrence rate of fusion holes in waste products;
4. for the low-melting material powder and the auxiliary sintering material powder, the low-melting material is dispersed in the auxiliary sintering material precursor chloride solution, and then the auxiliary sintering material is separated and mixed, most of particles with the particle size smaller than 2 mu m are separated, so that the rejection rate of inconsistent ceramic shrinkage is avoided being increased, and the yield is improved.
Detailed Description
Some of the terms used in the present invention are given a defined interpretation here:
base material: the raw materials occupying the solid components in the ceramic slurry influence the important influence on the physicochemical properties of the ceramic such as color, strength, density and the like obtained by firing.
Green body: the ceramic slurry is injected into a gypsum mould for dehydration and demoulding to obtain the product.
Blank body: and sintering the qualified green body at high temperature to obtain the finished product.
Ceramic: and the qualified green body is obtained by high-temperature firing and sintering, or is obtained by continuously firing after glazing the qualified green body.
[ raw materials ]
Quartz, a powder, was purchased from the filter materials Ltd of the military from the chenchenchen tai, and was crushed and sieved to obtain a powder having a particle size of 10 μm.
The waste porcelain powder is powder, and the particle size of the powder is 8 mu m after screening. The waste porcelain powder is from waste porcelain produced by the factory and contains SiO2：66.31～67.38wt％，Al2O3：24.06～25.13wt％，TiO2：0.64～0.75wt％，Fe2O3:1.44～1.76wt％，CaO：0.64～1.07wt％，MgO：0.48～0.7wt％，K2O：3.1～3.53wt％，Na2O: 1.18 to 1.50 wt% and other impurities as the rest.
Kaolin, a powder material, was purchased from Chenghou Chenghu and mineral processing plants and was crushed and sieved to obtain a powder material with a particle size of 8 μm.
Ball clay, called ball clay, is purchased from Hongyang refractory material factories in Jilin, and is crushed and sieved to obtain powder with the particle size of 12 μm.
Calcining the flint clay, wherein the 45# calcined flint clay obtained from ZiboRui refractory material Co., Ltd is less than 8 mu m in particle size; low melting stock, mica powder, which is purchased from GB-8 sericite powder and sericite customized products of Chuzhou Kerui mining company Limited liability company, the maximum grain diameter is less than 20 mu m, the total content of Fe and Cu is less than 3.6wt%, and the density is 2.65-2.68 g/cm3The water content is less than 1 wt%.
The total content of Fe and Cu in the low-melting materials is less than 3.6wt%, according to the using amount of the invention, after the total content of Fe and Cu in the low-melting materials is more than 3.6wt%, the rejection rate is obviously improved due to the formation of spots on the surface of the blank, and after the total content of Fe and Cu in the low-melting materials is more than 3.6wt%, the significance to the actual production is not large, and the influence on the rejection rate is large.
The firing auxiliary material is one or more of aluminum hydroxide gel and magnesium hydroxide gel and is prepared by self.
The process was carried out in preparation example 1,
processing of low melting stock:
mica with the total content of Fe and Cu less than 3.6wt% is crushed, ground and airflow milled to obtain mica powder, and the mica powder with the maximum particle size less than 20 microns is screened to obtain low melting material. The crushed products of the Chuzhou Kerui mining company Limited liability company are directly purchased, the powder with the granularity larger than 20 mu m is sieved to remove the powder to obtain the low melting material, the low melting material is sampled and detected, the granularity range detection, the water content detection, the [ total content of Fe and Cu ] detection and the real density detection are independently carried out, and the detection results are shown in the following table 1.
TABLE 1 particle size distribution of low melt in preparation example 1
In the preparation example 2, the following procedures were carried out,
processing of low melting stock:
mica with the total content of Fe and Cu of less than 3.6wt% is selected to be crushed, ground and crushed by an airflow mill to obtain mica powder, the mica powder with the maximum particle size of less than 20 mu m is obtained by screening, the crushed mica powder is directly purchased from Chuzhou Kerui mining company Limited liability company, the powder with the particle size of more than 20 mu m is removed by screening, the powder with the maximum particle size of less than 20 mu m is washed by water and filtered, the powder with the particle size of less than 2 mu m is removed, and the dried powder is used as low melting material. The low melting material sampling detection, the particle size range detection, the water content detection, [ total content of Fe and Cu ] detection and the real density detection are independently carried out, and the detection results are shown in the following table 2.
TABLE 2 particle size distribution of the low melt in preparation example 2
In the preparation example 3, the following procedures were carried out,
the preparation of sintering auxiliary materials (aluminum hydroxide) comprises the following steps:
preparing 30 wt% aluminum chloride solution by taking aluminum chloride as a raw material, adding sodium hydroxide powder into the 30 wt% aluminum chloride solution, and adjusting the pH value of the mixed solution to 11;
continuously stirring for 30min, adding 18 wt% hydrochloric acid while stirring to adjust pH to 4.7, filtering, washing the filtrate with water, and oven drying at 60 deg.C;
pressing the dried filtrate into blocks according to 500g, putting the blocks into a mould, and putting the blocks into a mould H2：N2The molar ratio is 1: 1, heating to 300 ℃ for 3min in a reducing atmosphere, heating to 970 ℃ within 10min, firing at 970 ℃ for 30min, cooling in a step manner at 800 ℃, 500 ℃ and 200 ℃ at room temperature, wherein the time of each cooling process is 8min, cooling to 800 ℃, 500 ℃ and 200 ℃, standing for 3min, and cooling to room temperature to obtain a sintered block;
crushing the sintered cake to obtain sintering auxiliary material powder with the granularity of 5 mu m and the real density of 3.92g/m3。
In the preparation example 4, the following procedures were carried out,
the preparation of sintering auxiliary materials (magnesium hydroxide) comprises the following steps:
preparing a magnesium chloride solution with the concentration of 30 wt% by taking magnesium chloride as a raw material, adding sodium hydroxide powder into the magnesium chloride solution with the concentration of 30 wt% while stirring, adjusting the pH value of the mixed solution to 10, filtering, washing the filtrate with water, and drying the filtrate at 60 ℃ for later use; pressing the dried filtrate into blocks according to 500g, putting the blocks into a mould, and putting the blocks into a mould H2：N2The molar ratio is 1: 1, heating to 300 ℃ for 3min in a reducing atmosphere, heating to 970 ℃ within 10min, firing at 970 ℃ for 30min, cooling in a step manner at 800 ℃, 500 ℃ and 200 ℃ at room temperature, wherein the time of each cooling process is 8min, cooling to 800 ℃, 500 ℃ and 200 ℃, standing for 3min, and cooling to room temperature to obtain a sintered block;
crushing the sintered cake to obtain sintering auxiliary material powder with the particle size of 5 mu m and the density of 3.58g/m3。
In the case of the preparation example 5,
the preparation of sintering auxiliary materials (compounding aluminum hydroxide and magnesium hydroxide) comprises the following steps:
preparing an aluminum chloride solution with the concentration of 30 wt% by taking aluminum chloride as a raw material, preparing a magnesium chloride solution with the concentration of 30 wt% by taking magnesium chloride as a raw material, and mixing the aluminum chloride solution with the concentration of 30 wt% and the magnesium chloride solution with the concentration of 30 wt% according to a mass ratio of 1: mixing at a ratio of 0.8;
taking 10kg of mixed solution, adding sodium hydroxide powder while stirring, adjusting the pH value of the mixed solution to 11;
continuing stirring for 30min, adding 18 wt% hydrochloric acid while stirring to adjust pH to 4.7, stirring for 10min, washing the filtrate with water, and oven drying at 60 deg.C;
pressing the dried filtrate into blocks according to 500g, putting the blocks into a mould, and putting the blocks into a mould H2：N2The molar ratio is 1: 1, heating to 300 ℃ for 3min in a reducing atmosphere, heating to 970 ℃ within 10min, firing at 970 ℃ for 30min, cooling in a step manner at 800 ℃, 500 ℃ and 200 ℃ at room temperature, wherein the time of each cooling process is 8min, cooling to 800 ℃, 500 ℃ and 200 ℃, standing for 3min, and cooling to room temperature to obtain a sintered block;
the agglomerates were crushed to obtain powders of sintering aid having a particle size of 5 μm.
In the case of the preparation example 6,
the preparation of the mixed sintering material (aluminum hydroxide and low melting material) comprises the following steps:
preparing 30 wt% aluminum chloride solution by taking aluminum chloride as a raw material, adding 1000kg of 30 wt% aluminum chloride solution into sodium hydroxide powder, adjusting the pH value of the mixed solution to 11, and continuing stirring for 30 min; adding 76.01kg of the low melting material of preparation example 1 into the solution, stirring after adding to keep the low melting material powder particles in the solution to roll, adding 18 wt% hydrochloric acid to adjust the pH to 4.7, filtering, washing the filtrate with water, drying the filtrate at 60 ℃, and weighing 251.5 kg;
pressing the dried filtrate into blocks according to 500g, putting the blocks into a mould, and putting the blocks into a mould H2：N2The molar ratio is 1: 1, sintering in a reducing atmosphere, heating to 300 ℃ for 3min, heating to 970 ℃ within 10min, firing at 970 ℃ for 30min, cooling in a step manner at 800 ℃, 500 ℃ and 200 ℃ at room temperature, wherein the time of each cooling process is 8min, cooling to 800 ℃, 500 ℃ and 200 ℃, standing for 3min, and cooling to room temperature to obtain a sintered block;
the agglomerates were crushed to obtain a powder of mixed clinker having a particle size of 8 μm.
In the case of the preparation example 7,
the preparation of the mixed sintering material (magnesium hydroxide and low melting material) comprises the following steps:
preparing a 30 wt% magnesium chloride solution by taking magnesium chloride as a raw material, adding 92.16kg of the low melting material of the preparation example 1 into 10kg of the 30 wt% magnesium chloride solution, stirring after adding to keep the low melting material powder particles in the solution to roll, adding sodium hydroxide powder, adjusting the pH of the mixed solution to 10, filtering, washing the filtrate with water, drying the filtrate at 60 ℃, and weighing 275.92 kg;
pressing the dried filtrate into blocks according to 500g, putting the blocks into a mould, and putting the blocks into a mould H2：N2The molar ratio is 1: 1, heating to 300 deg.C for 3min, heating to 970 deg.C within 10min, and firing at 970 deg.C for 30min at 800 deg.CCooling at 500 deg.C and 200 deg.C in a stepwise manner at room temperature for 8min, cooling to 800 deg.C, 500 deg.C, and 200 deg.C, standing for 3min, and cooling to room temperature to obtain sintered cake;
the agglomerates were crushed to obtain a powder of mixed clinker having a particle size of 8 μm.
In the preparation of example 8, the following examples were conducted,
the preparation of the mixed sintering material (compounding aluminum hydroxide, magnesium hydroxide and low-melting material) comprises the following steps:
preparing an aluminum chloride solution with the concentration of 30 wt% by taking aluminum chloride as a raw material, preparing a magnesium chloride solution with the concentration of 30 wt% by taking magnesium chloride as a raw material, and mixing the aluminum chloride solution with the concentration of 30 wt% and the magnesium chloride solution with the concentration of 30 wt% according to a mass ratio of 1: mixing according to the proportion of 0.8 to obtain a mixed solution;
adding 84.86kg of the low melting material of preparation example 1 into 10kg of the mixed solution, stirring after adding to ensure that the low melting material powder particles are kept rolling in the solution, adding sodium hydroxide powder, adjusting the pH value of the mixed solution to 11, continuing stirring for 3min, adding 18 wt% hydrochloric acid to adjust the pH value to 4.7, stirring for 5min, washing the filtrate with water, drying the filtrate at 60 ℃, and weighing 264.03 kg.
Pressing the dried filtrate into blocks according to 500g, putting the blocks into a mould, and putting the blocks into a mould H2：N2The molar ratio is 1: 1, heating to 300 ℃ for 3min in a reducing atmosphere, heating to 970 ℃ within 10min, firing at 970 ℃ for 30min, cooling in a step manner at 800 ℃, 500 ℃ and 200 ℃ at room temperature, wherein the time of each cooling process is 8min, cooling to 800 ℃, 500 ℃ and 200 ℃, standing for 3min, and cooling to room temperature to obtain a sintered block;
the agglomerates were crushed to obtain a powder of mixed clinker having a particle size of 8 μm.
In the preparation of example 9, the following examples were carried out,
preparation of a mixed clinker (magnesium hydroxide and low-melting material) the same as in preparation example 6, except that the low-melting material of preparation example 2 was used, the amount of the low-melting material added was 76.88kg, and the filtrate weighed 252.37kg after drying at 60 ℃.
In the preparation of example 10, the following examples were conducted,
preparation of a mixed clinker (magnesium hydroxide and low-melting material) the same as in preparation example 7 was conducted except that the low-melting material of preparation example 2 was used, the amount of the low-melting material added was 93.21kg, and the filtrate weighed 276.96kg after drying at 60 ℃.
In the preparation of example 11, the following examples were conducted,
the preparation of the mixed clinker (compounding of aluminum hydroxide, magnesium hydroxide and a low-melting material) was the same as that of preparation example 8, except that the low-melting material of preparation example 2 was used, the amount of the low-melting material added was 84.86kg, and the filtrate weighed 264.03kg after being dried at 60 ℃.
In the examples 1 to 6, the following examples were conducted,
the preparation method of the ceramic slurry for grouting comprises the following steps:
s1, selecting and mixing the powder with the low melting point in the preparation example 1 or the preparation example 2 and the powder with the sintering auxiliary material in the preparation examples 3-5 (the mixing ratio is shown in the following table 3), uniformly mixing, pressing into a block according to 500g, and putting into a mold;
pressing the dried filtrate into blocks according to 500g, putting the blocks into a mould, and putting the blocks into a mould H2：N2The molar ratio is 1: 1, heating to 300 ℃ for 3min in a reducing atmosphere, heating to 970 ℃ within 10min, firing at 970 ℃ for 30min, cooling in a step manner at 800 ℃, 500 ℃ and 200 ℃ at room temperature, wherein the time of each cooling process is 8min, cooling to 800 ℃, 500 ℃ and 200 ℃, standing for 3min, and cooling to room temperature to obtain a sintered block;
crushing the sintered blocks to obtain powder of mixed sintering material with the granularity of 8 mu m;
s2: weighing 140kg of quartz, 90kg of waste porcelain powder, 60kg of kaolin, 340kg of ball clay, 380kg of calcined flint clay and 170kg of mixed sintering material, mixing the solid mixing material with water according to a ratio of 1:0.3, and performing ball milling to obtain coarse grinding slurry;
s3: keeping stirring the rough grinding slurry, and carrying out ageing for 3 days, supplementing water to the rough grinding slurry according to the water evaporation capacity of the rough grinding slurry during ageing, and keeping the volume of the slurry stable to obtain the slurry for grouting ceramics.
Specific parameters of the low melting materials and the firing aids of examples 1-6 are shown in Table 3 below.
TABLE 3 specific parameters for the low melting and firing adjuvants of examples 1-6
In the embodiments 7 to 12, the following examples are given,
the preparation method of the ceramic slurry for grouting comprises the following steps:
s1, selecting powder of the mixed sintering material in the preparation examples 6-11;
s2: weighing 140kg of quartz, 90kg of waste porcelain powder, 60kg of kaolin, 340kg of ball clay, 380kg of calcined flint clay and 170kg of mixed sintering material according to the mass parts, mixing the solid mixing material with water according to a ratio of 1:0.3, and performing ball milling to obtain coarse grinding slurry;
s3: keeping stirring the rough grinding slurry, and carrying out ageing for 3 days, supplementing water to the rough grinding slurry according to the water evaporation capacity of the rough grinding slurry during ageing, and keeping the volume of the slurry stable to obtain the slurry for grouting ceramics.
Specific parameters of the mixed fuel in examples 7 to 12 are shown in Table 4 below.
TABLE 4 specific parameters for low melting and firing adjuvants of examples 7-12
| Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | |
| Mixed sintering material | Preparation example 6 | Preparation example 7 | Preparation example 8 | Preparation example 9 | Preparation example 10 | Preparation example 11 |
The grouting ceramic slurry prepared according to the embodiments 7-12 is used for grouting to prepare ceramic samples, wherein the samples are hollow ceramics with the external dimension of 10cm x 5cm, the green body wall thickness is 0.8 +/-0.1 cm, and the number of formed samples prepared in each group of embodiments is 1000.
The ceramic sample obtained by grouting in the embodiment 7-12 is fired at 1120 ℃, the free oxygen content of the firing atmosphere is controlled to be 4-5% (volume), and the firing time is 7 h. The quality of the fired samples was measured and the results are shown in Table 5.
In the comparative example 1,
a ceramic slurry for grouting, based on example 1, is characterized in that the amount of mixed sintering material is 0, low melting material and sintering auxiliary material are directly added and mixed in S2 to obtain solid mixture, and grouting ceramic slurry is prepared.
In a comparative example 2,
a ceramic slurry for grouting, based on example 2, is characterized in that the amount of mixed sintering material is 0, low melting material and sintering auxiliary material are directly added and mixed in S2 to obtain solid mixture, and grouting ceramic slurry is prepared.
In a comparative example 3,
a ceramic slurry for grouting, based on example 3, is different in that the amount of the mixed sintering material is 0, and a low melting material and a sintering auxiliary material are directly added and mixed in S2 to obtain a solid mixture, and a grouting ceramic slurry is prepared.
The slurry prepared in comparative examples 1 to 3 was used for slurry casting to prepare ceramic samples, wherein the samples were required to be hollow ceramics having an outer dimension of 10cm by 5cm and a green thickness of 0.8 ± 0.1cm, and the number of formed samples prepared in each set of examples was 1000.
Firing the ceramic sample obtained by grouting in the comparative examples 1 to 3, wherein the firing temperature is 1120 ℃, the free oxygen content of the firing atmosphere is controlled to be 4 to 5 percent (volume), and the firing time is 7 hours. The quality of the fired samples was measured and the results are shown in Table 5.
TABLE 5 test results of the grouting ceramic samples obtained in examples 1 to 12 and comparative examples 1 to 3
As can be seen from Table 5, the rejection rate and the occurrence rate of the craters in the scrap in example 1 are lower than those in comparative example 1, the rejection rate and the occurrence rate of the craters in the scrap in example 2 are lower than those in comparative example 2, and the rejection rate and the occurrence rate of the craters in the scrap in example 2 are lower than those in comparative example 2, so that the invention mixes and fires the low melting material and the auxiliary firing material first and then breaks the mixture to obtain the mixed firing material, and then mixes the mixed firing material with other base materials to prepare the grouting ceramic slurry, the rejection rate of the ceramic can be reduced, and the occurrence rate of the craters in the scrap can be reduced.
In addition, the rejection rate and the occurrence rate of the molten holes in the waste are lower than those in the example 1, the rejection rate and the occurrence rate of the molten holes in the waste are lower than those in the example 2, and the rejection rate and the occurrence rate of the molten holes in the waste are lower than those in the example 3 in the example 9.
On the other hand, the low melting materials of the powder with the particle size less than 2 μm are not separated in the examples 1 to 3 and 7 to 9, the low melting materials of the powder with the particle size less than 2 μm are mostly separated in the examples 4 to 6 and 10 to 12,
the rejection rate and the occurrence rate of the molten holes in the waste are lower than those in the embodiment 4 in the embodiment 1, the rejection rate and the occurrence rate of the molten holes in the waste are lower than those in the embodiment 5 in the embodiment 2, and the rejection rate and the occurrence rate of the molten holes in the waste are lower than those in the embodiment 6 in the embodiment 3.
However, for the low-melting-material powder and the auxiliary sintering material powder, the low melting material is dispersed in the auxiliary sintering material precursor chloride solution, and then the auxiliary sintering material is precipitated and mixed, the rejection rate and the occurrence rate of the craters in the waste are lower than those of the example 10, the rejection rate and the occurrence rate of the craters in the waste are lower than those of the example 11, the rejection rate and the occurrence rate of the craters in the waste are lower than those of the example 12,
the dispersing effect of the excessively fine low-melting powder particles in the chlorination solution is poor, the excessively fine low-melting powder particles can be gathered and bonded into loose large particles, and free water is carried in the large particles and is difficult to remove by drying; large particles are sintered after being coated by the auxiliary sintering material, a cavity formed in the original position is larger than the fused volume of the low melting material, so that the sintering uniformity of the mixed sintering material is poor, the number of tiny holes is increased, the diffusion and permeation effect of the obtained sintering powder is reduced when the obtained sintering powder is used for sintering a blank, the shrinkage of the obtained ceramic is inconsistent, and the rejection rate of cracking is increased;
the low-melting material powder and the auxiliary sintering material powder are dispersed in the auxiliary sintering material precursor chloride solution, and then the auxiliary sintering material is separated out and mixed, so that most of particles with the particle size of less than 2 mu m are separated, and the rejection rate can be reduced.
In the embodiments 13 to 15, the following examples are given,
the preparation method of the ceramic slurry for grouting comprises the following steps:
s1, selecting the powder of the low-melting material of the preparation example 1 and the powder of the firing auxiliary material of the preparation example 3, mixing the powder of the low-melting material and the firing auxiliary material according to the mass ratio of 0.4331, uniformly mixing the powder of the low-melting material and the firing auxiliary material, pressing the mixture into blocks according to 500g, and putting the blocks into a mold;
pressing the dried filtrate into blocks according to 500g, putting the blocks into a mould, and putting the blocks into a mould H2：N2The molar ratio is 1: 1, heating to 300 ℃ for 3min in a reducing atmosphere, heating to 970 ℃ within 10min, firing at 970 ℃ for 30min, cooling in a step manner at 800 ℃, 500 ℃ and 200 ℃ at room temperature, wherein the time of each cooling process is 8min, cooling to 800 ℃, 500 ℃ and 200 ℃, standing for 3min, and cooling to room temperature to obtain a sintered block;
crushing the sintered blocks to obtain powder of mixed sintering material with the granularity of 8 mu m;
s2: weighing quartz, waste porcelain powder, kaolin, ball clay, calcined flint clay and mixed sintering materials, mixing to obtain a solid mixed material, mixing the solid mixed material with water according to a ratio of 1:0.3, and performing ball milling to obtain coarse grinding slurry;
s3: keeping stirring the rough grinding slurry, and carrying out ageing for 3 days, supplementing water to the rough grinding slurry according to the water evaporation capacity of the rough grinding slurry during ageing, and keeping the volume of the slurry stable to obtain the slurry for grouting ceramics.
Specific parameters of the base materials of examples 13 to 15 are shown in Table 6.
In the embodiments 16 to 18, the following examples are given,
the preparation method of the ceramic slurry for grouting comprises the following steps:
s1, selecting powder of the mixed sintering material of the preparation example 9;
s2: weighing quartz, waste ceramic powder, kaolin, ball clay, calcined flint clay and mixed sintering materials according to the mass parts, mixing to obtain a solid mixing material, mixing the solid mixing material with water according to the ratio of 1:0.3, and performing ball milling to obtain coarse grinding slurry;
s3: keeping stirring the rough grinding slurry, and carrying out ageing for 3 days, supplementing water to the rough grinding slurry according to the water evaporation capacity of the rough grinding slurry during ageing, and keeping the volume of the slurry stable to obtain the slurry for grouting ceramics.
Specific parameters for the base materials of examples 13-18 are shown in Table 6.
TABLE 6 specific parameters for the base materials of examples 13 to 18
The slurry prepared in examples 13 to 18 was used for slurry casting to prepare ceramic samples, wherein the samples were hollow ceramics having an outer dimension of 10cm by 5cm and a green thickness of 0.8 ± 0.1cm, and the number of formed samples prepared in each group of examples was 1000.
The ceramic samples obtained by grouting in the embodiments 13 to 18 are fired at 1120 ℃, the free oxygen content of the firing atmosphere is controlled to be 4 to 5 percent (volume), and the firing time is 7 hours. The quality of the fired samples was measured and the results are shown in Table 7.
Table 7 test results of the ceramic samples of examples 13 to 18
As can be seen from table 7, when 13 parts by mass of quartz, 8 parts by mass of waste porcelain powder, 5 parts by mass of kaolin, 32 parts by mass of ball clay, 35 parts by mass of calcined flint clay and 18 parts by mass of mixed sintering material were prepared by directly mixing and sintering the sintering auxiliary material and the low melting material (example 13), the yield of the fired body was high and the reduction rate of the craters in the waste was large.
For the low melting material powder and the auxiliary sintering material powder, the low melting material is dispersed in the auxiliary sintering material precursor chloride solution, and then the auxiliary sintering material is separated and mixed, when 15 parts by mass of quartz, 9 parts by mass of waste porcelain powder, 7 parts by mass of kaolin, 35 parts by mass of ball clay, 34 parts by mass of calcined flint clay and 18 parts by mass of mixed sintering material are proportioned (example 17), the yield of the sintered blank is high, and the reduction rate of the fusion holes in the waste is high.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (6)
1. The preparation method of the ceramic slurry for grouting is characterized in that the slurry is prepared by mixing the following raw materials:
quartz, wherein the quartz is powder;
the waste porcelain powder is powder, and the component in the waste porcelain powder is SiO2：66.31~67.38wt%，Al2O3：24.06~25.13wt%，TiO2：0.64~0.75wt%，Fe2O3：1.44~1.76wt%，CaO：0.64~1.07wt%，MgO：0.48~0.7wt%，K2O：3.1~3.53wt%，Na2O：1.18~1.50wt%；
Kaolin, wherein the kaolin is powder;
ball soil, wherein the ball soil is powder;
calcining a flint clay, wherein the flint clay is powder, and the flint clay is calcined flint clay;
the low melting material is powder mica, the maximum particle size is less than 20 mu m, the total content of Fe and Cu of the mica is less than 3.6wt%, and the water content is less than 1 wt%;
the main components of the firing auxiliary materials are one or more of aluminum hydroxide and magnesium hydroxide, the using amount of the firing auxiliary materials is related to the using amount of the low-melting-point material, and the volume-to-low-melting-point volume ratio of the firing auxiliary materials is 1.02 after one or more of aluminum oxide and magnesium oxide are used as the firing auxiliary materials;
the preparation method comprises the following steps of,
s1, mixing the low melting materials and the firing auxiliary materials, uniformly mixing, then heating and firing at 960-980 ℃, wherein the firing time is 30min, and crushing after the fired product is cooled to obtain a mixed firing material with the particle size of 8 mu m;
s2: mixing 13-15 parts of quartz, 8-10 parts of waste porcelain powder, 5-8 parts of kaolin, 32-36 parts of ball clay, 33-38 parts of calcined flint clay, 14-18 parts of mixed sintering material and water according to the parts by weight, and performing ball milling to obtain coarse grinding slurry,
s3: keeping stirring the rough grinding slurry, and ageing for 3 days, supplementing water to the rough grinding slurry according to the water evaporation capacity of the rough grinding slurry during ageing, and keeping the volume of the slurry stable to obtain slurry for grouting ceramics;
the mixing method of the low-melting materials and the sintering auxiliary materials in the step S1 is as follows: adding low-melting powder into one or mixed solution of aluminum chloride and magnesium chloride, stirring to make the low-melting powder roll in the solution, adding pH regulator to make Al exist correspondingly3+、Mg2+One or more of them are precipitated in the form of hydroxide gel, coated with low-melting powder particles, filtered, washed with water, dried to remove free water, and then fired in S1.
2. The method for preparing ceramic slurry for grouting according to claim 1, wherein the low melting material is removed powder with the particle size of less than 2 μm, and the powder with the particle size of less than 2 μm in the low melting material accounts for less than 1 wt%.
3. The preparation method of the ceramic slurry for grouting according to claim 1, wherein the slurry raw material comprises, by mass, 13 parts of quartz, 8 parts of waste porcelain powder, 5 parts of kaolin, 32 parts of ball clay, 35 parts of calcined flint clay and 18 parts of mixed sintering material, and the mixed sintering material comprises low melting material and sintering auxiliary material according to a mass ratio of 0.4331: 1 is obtained by directly mixing and firing.
4. The preparation method of the ceramic slurry for grouting according to claim 1, wherein the slurry raw materials comprise, by mass, 15 parts of quartz, 9 parts of waste porcelain powder, 7 parts of kaolin, 35 parts of ball clay, 34 parts of calcined flint clay and 18 parts of mixed sintering materials, and the sintering auxiliary material is aluminum hydroxide.
5. A ceramic slurry for grouting, characterized by being prepared by the method for preparing a ceramic slurry for grouting according to any one of claims 1 to 4.
6. A grouting ceramic, which is characterized by comprising a blank body, wherein the grouting slurry used for the blank body is the grouting ceramic slurry of claim 5.
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| CN104086157A (en) * | 2014-07-11 | 2014-10-08 | 梁胜光 | Ceramic pug |
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| CN108530020A (en) * | 2018-04-16 | 2018-09-14 | 合肥月煌新型装饰材料有限公司 | A kind of preparation process of ceramic tap |
| CN110078471A (en) * | 2019-05-17 | 2019-08-02 | 江门市东鹏智能家居有限公司 | The high-pressure slip-casting ceramic slurry and preparation method, system recycled based on useless porcelain |
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| US5153155A (en) * | 1990-12-06 | 1992-10-06 | H. C. Spinks Clay Company Inc. | Clay slurry |
| CN104086157A (en) * | 2014-07-11 | 2014-10-08 | 梁胜光 | Ceramic pug |
| CN105712697A (en) * | 2016-01-22 | 2016-06-29 | 福建科福材料有限公司 | Sanitary ceramics slip and preparation technology thereof |
| CN108530020A (en) * | 2018-04-16 | 2018-09-14 | 合肥月煌新型装饰材料有限公司 | A kind of preparation process of ceramic tap |
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