CN115536359A - Preparation method for low-temperature sintering high-strength building ceramic body by adopting low-cost raw materials and product thereof - Google Patents

Preparation method for low-temperature sintering high-strength building ceramic body by adopting low-cost raw materials and product thereof Download PDF

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CN115536359A
CN115536359A CN202211146518.7A CN202211146518A CN115536359A CN 115536359 A CN115536359 A CN 115536359A CN 202211146518 A CN202211146518 A CN 202211146518A CN 115536359 A CN115536359 A CN 115536359A
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pug
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梁健
刘方波
陈拥强
江伟辉
劳新斌
苗立锋
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Jingdezhen Ceramic Institute
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Abstract

The invention discloses a preparation method for firing a high-strength building ceramic blank at low temperature by adopting low-cost raw materials, wherein the building ceramic blank consists of a base material and a composite additive; the base material comprises the raw materials of 38-45 wt% of precast pug, 16-21 wt% of potassium feldspar, 15-18 wt% of shale, 12-20 wt% of wollastonite and 8-11 wt% of talc; the composite additive consists of 0.1-0.15 wt% of base material, 0.05-0.1 wt% of guar gum, 0.05-0.1 wt% of sodium carboxymethyl cellulose and sodium humate. According to the invention, through optimizing a formula system, low-temperature firing is realized, the flexural strength of a ceramic blank is effectively improved, the reduction of the product thickness is facilitated, the thin-wall lightweight of the architectural ceramic blank is realized, the development of light-weight and thin architectural ceramic products is facilitated while resources are protected, energy is saved, carbon is reduced, and environmental pollution is reduced, so that the production and transportation cost of the products is reduced, and the method has a wide market application prospect.

Description

Preparation method for low-temperature sintering high-strength building ceramic body by adopting low-cost raw materials and product thereof
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a preparation method of a building ceramic body and a product thereof.
Background
China is a large ceramic production country, and the yield of three traditional ceramic products, namely daily use, building and sanitation, is the first world, wherein the yield of the building sanitary ceramic also occupies the half-wall Jiangshan of the total world yield, a large amount of mineral resources and fuel energy are required to be consumed every year, and the thicker the thickness and the higher the quality, the larger the consumption of raw materials and energy is. When the low-carbon era comes, under the large background of national advocation of energy conservation, consumption reduction and transformation development, the green, low-carbon, energy conservation and environmental protection become irremediable missions of building ceramics. The building sanitary ceramic industry is also a three-high industry with high pollution, high energy consumption and high resource consumption, so that the establishment of an energy-saving emission-reducing green ceramic production mode with technical innovation has profound significance for the development of the building sanitary ceramic industry.
The low-temperature sintering can obtain remarkable energy-saving benefit. According to the related heat balance principle and experience, the fuel can be saved by 15-20% when the firing temperature is more than 1000 ℃ and is reduced by 100 ℃, the firing time is reduced by 10% and the heat consumption is reduced by 4%. Meanwhile, the low-temperature firing can improve the productivity, reduce the loss of kiln refractory materials and kiln furniture, prolong the service life of the kiln, select low-price materials and reduce the production cost.
In the prior art, the thickness of the building sanitary ceramic product is about 8-14 mm, and the thickness is thicker; the thickness of the ceramic thin plate is less than 5.5mm, materials can be saved to a great extent, but the flexural strength is generally 50-70 MPa, the ceramic thin plate is generally lower, the firing temperature is generally about 1200 ℃, the service life of the kiln furniture is not prolonged, more energy is consumed, and the influence on the environment is not small. The strength of the blank is an important performance index in the production process of the building ceramic, and has important influence on the production yield of the building ceramic. Therefore, the bending strength of the green body must be greatly improved, and the thin-wall and light-weight of the building sanitary ceramic green body is realized, so that the consumption of raw materials and energy sources can be reduced, the transportation and installation cost can be reduced, the requirements of building a resource-saving and environment-friendly society are met, and the development of low-carbon economy and dual-carbon plan realization is promoted.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a preparation method for firing a high-strength architectural ceramic blank at low temperature by adopting low-cost raw materials, so as to relieve the problems of high firing temperature and high raw material cost, realizes low-temperature firing by optimizing a formula system, and effectively improves the flexural strength of the ceramic blank, thereby being beneficial to reducing the thickness of a product, realizing the thin-wall and light-weight architectural ceramic blank, protecting resources, saving energy, reducing low carbon, reducing environmental pollution, and simultaneously being beneficial to the development of light-weight and thin architectural ceramic products, thereby reducing the production and transportation cost of the product. The invention also aims to provide a product prepared by the preparation method.
The purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method for firing a high-strength building ceramic blank at low temperature by adopting low-cost raw materials, wherein the building ceramic blank consists of a base material and a composite additive; the base material comprises the raw materials of 38-45 wt% of precast pug, 16-21 wt% of potassium feldspar, 15-18 wt% of shale, 12-20 wt% of wollastonite and 8-11 wt% of talc; the composite additive consists of 0.1 to 0.15 weight percent of guar gum, 0.05 to 0.1 weight percent of sodium carboxymethyl cellulose and 0.05 to 0.1 weight percent of sodium humate; the raw materials of the prefabricated pug comprise 19-23 wt% of washed sand, 8-14 wt% of kaolin, 37-45 wt% of washed mud, 14-18 wt% of flower mud and 8-14 wt% of coffee mud; the preparation method comprises the following steps:
(1) Preparing raw materials of the prefabricated pug, performing wet ball milling, drying, sieving, and performing powder granulation to obtain mixed prefabricated pug; mixing the mixed precast pug, potassium feldspar, shale, wollastonite, talc and a composite additive, performing wet ball milling, drying and sieving the obtained slurry, and performing powder granulation to obtain a material with a median particle size of 60-80 meshes;
(2) After the granulated material is pressed and molded, the temperature is raised to 1100-1140 ℃ from the room temperature at the heating rate of 5-15 ℃/min, the temperature is kept for 30-60 min, the temperature is reduced along with the furnace, and the material is naturally cooled to the room temperature, so that the low-temperature sintered high-strength architectural ceramic blank is obtained.
Furthermore, the median particle size of the mixed precast pug is 60-80 meshes, and the particle sizes of the potash feldspar, the shale, the wollastonite and the talc are all 60-120 meshes. The pressure of the compression molding in the step (2) is 4-6 MPa, and the compression time is 20-30 s.
According to the product prepared by the preparation method, the main crystalline phases of the building ceramic blank body are anorthite, quartz and diopside, the breaking strength of the ceramic blank body is 85.45-102.53 MPa, and the water absorption is 0.13-0.43%.
The invention has the following beneficial effects:
(1) The raw materials adopted by the invention are mostly low-cost raw materials, and meanwhile, the potassium feldspar is introduced as a fluxing agent, so that the potassium feldspar and Ca and Mg components in wollastonite and talc can play a role of a multi-element flux at high temperature, the firing temperature is greatly reduced, a liquid phase is formed at a lower temperature, and the formation of crystal nuclei and the growth process of crystals are promoted; the talc can be co-melted with the potassium feldspar, and a small amount of talc is added into the blank, so that the liquid phase viscosity can be reduced, the low-temperature co-melting process of the free quartz and the potassium feldspar is promoted, the closed porosity and the water absorption are reduced, and the breaking strength of the blank is improved; besides, the CaO and MgO components can also reduce the thermal expansion coefficient of the green body, and can play a good role in stabilizing the size of a product under the condition of ensuring the adaptability of the architectural ceramic blank glaze; guar gum, sodium carboxymethylcellulose and sodium humate are used as composite additives, so that on one hand, the interaction among dry powder particles can be enhanced, the phenomenon of layer cracking in the compression molding process is reduced, and the breaking strength of a green body is enhanced; on the other hand, when the ceramic particles are sintered at high temperature, a certain amount of the composite additive is added to promote the densification of the green body, compared with the green body without the composite additive, the content of the ceramic particles is increased under the same volume, the density of the green body is correspondingly increased, and the flexural strength of the green body is further increased.
(2) The prefabricated pug and the shale have higher silicon content, so that more quartz crystal phase and glass phase are remained besides the generation of diopside and anorthite crystal phase, the dispersion toughening effect of the quartz crystal phase, the pinning effect of the generated anorthite and diopside crystal phase in the glass phase and the like are ensured, and under the combined action of the factors, the synergistic enhancement effect can be generated, the breaking strength of the building ceramic product is greatly improved, the preparation of light and thin products is facilitated, and the firing temperature and the raw material cost are reduced, so that the energy conservation and the environmental protection are facilitated; the pre-formed mud and the shale simultaneously contain a certain amount of Fe 2 O 3 The sintering aid has a certain fluxing function, reduces the sintering temperature, promotes the sintering densification process of the green body, and has wide market application prospect.
Drawings
The invention will be described in further detail below with reference to examples and figures:
FIG. 1 is a scanning electron micrograph (a: 15000 times, b:10000 times) of a ceramic body prepared according to an example of the present invention;
fig. 2 is an XRD spectrum of the ceramic body prepared in the example of the present invention.
Detailed Description
The first embodiment is as follows:
the embodiment relates to a preparation method for firing a high-strength building ceramic blank at low temperature by adopting low-cost raw materials, wherein the building ceramic blank consists of a base material and a composite additive; the raw materials of the base material comprise 40wt% of prefabricated pug, 18wt% of potassium feldspar, 16wt% of shale, 16wt% of wollastonite and 10wt% of talc, and the particle sizes are 60 meshes; the composite additive consists of 0.1wt%, 0.05wt% and 0.05wt% of guar gum, sodium carboxymethylcellulose and sodium humate; wherein the raw materials of the prefabricated paste comprise 21wt% of washed sand, 11wt% of kaolin, 41wt% of washed mud, 16wt% of flower mud and 11wt% of coffee mud; the preparation method comprises the following steps:
(1) Preparing raw materials of the precast pug, performing wet ball milling for 40min (material: ball: water = 1: 2: 1), drying the obtained slurry in an oven at 120 ℃ for 3h, sieving the dried slurry by a 100-mesh sieve, and performing powder granulation to obtain mixed precast pug with the median particle size of 60 meshes; mixing the mixed precast pug, potassium feldspar, shale, wollastonite, talc and a composite additive, and then carrying out the treatment of the steps to obtain a material with a median particle size of 65 meshes;
(2) Pressing and molding the granulated material under the pressure of 4MPa for 30s; after pressing, the mixture is put into a box-type resistance sintering furnace to be heated from room temperature to 1140 ℃ at the heating rate of 15 ℃/min, the temperature is kept for 30min, the temperature is reduced along with the furnace, and the mixture is naturally cooled to room temperature, so that a low-temperature sintered high-strength building ceramic blank is obtained.
Example two:
the embodiment is a preparation method for firing a high-strength building ceramic blank at low temperature by adopting low-cost raw materials, wherein the building ceramic blank consists of a base material and a composite additive; the raw material composition of the base material is that prefabricated pug 38wt%, potash feldspar 17wt%, shale 15wt%, wollastonite 20wt%, talcum 10wt%, the granularity is 65 meshes; the composite additive consists of 0.15wt%, 0.1wt% and 0.1wt% of guar gum, sodium carboxymethylcellulose and sodium humate; wherein the raw materials of the prefabricated paste comprise 21wt% of washed sand, 11wt% of kaolin, 41wt% of washed mud, 16wt% of Guangdong flower mud and 11wt% of coffee mud; the preparation method comprises the following steps:
(1) Mixing the raw materials of the precast pug, carrying out wet ball milling for 40min (material: ball: water = 1: 2: 1), putting the obtained slurry into an oven, drying for 3h at the temperature of 120 ℃, sieving by a 100-mesh sieve, and carrying out powder granulation to obtain mixed precast pug with the median particle size of 65 meshes; mixing the mixed precast pug, potassium feldspar, shale, wollastonite, talc and a composite additive, and then carrying out the treatment of the steps to obtain a material with a median particle size of 70 meshes;
(2) Pressing and molding the granulated material under the pressure of 4MPa for 30s; after the pressing is finished, the ceramic blank is put into a box-type resistance sintering furnace to be heated from room temperature to 1140 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 30min, the temperature is reduced along with the furnace, and the ceramic blank is naturally cooled to room temperature, so that the low-temperature sintered high-strength building ceramic blank is obtained.
Example three:
the embodiment is a preparation method for firing a high-strength building ceramic blank at low temperature by adopting low-cost raw materials, wherein the building ceramic blank consists of a base material and a composite additive; the raw material composition of the base material is that prefabricated pug 40wt%, potash feldspar 21wt%, shale 16wt%, wollastonite 12wt%, talcum 11wt%, the granularity is 70 mesh; the composite additive consists of 0.1wt%, 0.05wt% and 0.05wt% of guar gum, sodium carboxymethylcellulose and sodium humate; wherein the raw materials of the prefabricated paste comprise 21wt% of washed sand, 11wt% of kaolin, 41wt% of washed mud, 16wt% of Guangdong flower mud and 11wt% of coffee mud; the preparation method comprises the following steps:
(1) Mixing the raw materials of the precast pug, performing wet ball milling for 40min (material: ball: water = 1: 2: 1), putting the obtained slurry into an oven, drying for 3h at the temperature of 120 ℃, sieving by a 100-mesh sieve, and performing powder granulation to obtain mixed precast pug with the median particle size of 70 meshes; mixing the mixed precast pug, potassium feldspar, shale, wollastonite, talc and a composite additive, and then carrying out the treatment of the steps to obtain a material with a median particle size of 75 meshes;
(2) Pressing and molding the granulated material under the pressure of 6MPa for 20s; after pressing, putting the mixture into a box-type resistance sintering furnace, heating the mixture from room temperature to 1120 ℃ at the heating rate of 10 ℃/min, preserving the heat for 60min, cooling the mixture along with the furnace, and naturally cooling the mixture to room temperature to obtain a low-temperature sintered high-strength building ceramic blank.
Example four:
the embodiment is a preparation method for firing a high-strength building ceramic blank at low temperature by adopting low-cost raw materials, wherein the building ceramic blank consists of a base material and a composite additive; the raw material composition of the base material is that prefabricated pug 45wt%, potash feldspar 16wt%, shale 18wt%, wollastonite 13wt%, talcum 8wt%, the granularity is 75 meshes; the composite additive consists of 0.15wt%, 0.1wt% and 0.1wt% of guar gum, sodium carboxymethylcellulose and sodium humate; wherein the raw materials of the prefabricated paste comprise 21wt% of washed sand, 11wt% of kaolin, 41wt% of washed mud, 16wt% of Guangdong flower mud and 11wt% of coffee mud; the preparation method comprises the following steps:
(1) Preparing raw materials of the precast pug, performing wet ball milling for 40min (material: ball: water = 1: 2: 1), drying the obtained slurry in an oven at 120 ℃ for 3h, sieving the dried slurry by a 100-mesh sieve, and performing powder granulation to obtain mixed precast pug with the median particle size of 75 meshes; mixing the mixed precast pug, potassium feldspar, shale, wollastonite, talc and a composite additive, and then carrying out the treatment of the steps to obtain a material with a median particle size of 80 meshes;
(2) Pressing and molding the granulated material under the pressure of 6MPa for 20s; after pressing, putting the mixture into a box-type resistance sintering furnace, heating the mixture from room temperature to 1120 ℃ at the heating rate of 5 ℃/min, preserving the heat for 60min, cooling the mixture along with the furnace, and naturally cooling the mixture to room temperature to obtain a low-temperature sintered high-strength building ceramic blank.
The chemical composition of the raw materials used in the examples of the present invention is shown in table 1.
TABLE 1 chemical composition of raw materials used in the examples of the present invention (wt%)
Figure BDA0003855521380000051
The ceramic bodies produced in the examples of the present invention contained anorthite, quartz and diopside crystalline phases (see fig. 2), and the microstructure of fig. 1 also shows the presence of anorthite and diopside crystalline phases.
The ceramic body using the precast pug as the raw material was used as a comparative example (i.e., no potash feldspar, shale, wollastonite, talc, composite additive were added). The ceramic body prepared by the embodiment of the invention and the performance test of the comparative ceramic body are as follows:
(1) Determination of the flexural Strength: the measurement is carried out according to the GB/T17657-2013 (the static bending strength is measured by a three-point bending method), and the formula is shown as the formula (1):
Figure BDA0003855521380000061
in the formula:
b- -static bending strength of the test piece in MegaPascals (MPa);
fmax-maximum load in newtons (N) when the test piece fails;
l- -distance between two supports, in millimeters (mm);
b- -specimen width in millimeters (mm);
t-specimen thickness in millimeters (mm).
(2) Measurement of Water absorption: according to GB/T3299-2011 (vacuum method), the formula is shown as formula (2):
Figure BDA0003855521380000062
in the formula:
ω - -Water absorption,% -, of the sample;
m 0 -mass of dried sample in grams (g);
m 1 the mass of the water-saturated sample in grams (g).
The test results are shown in table 2.
TABLE 2 Performance index of the inventive examples and comparative architectural ceramic bodies
Figure BDA0003855521380000063
Note: taking the first example as an example, in the green body bending strength test, the green body bending strength of the sample without adding the composite additive of 0.1wt% of guar gum, 0.05wt% of sodium carboxymethylcellulose and 0.05wt% of sodium humate is 2.01MPa after the powder is pressed and formed under the pressure of 4MPa and dried, and the green body bending strength of the sample without calcination is 3.48MPa, which is increased by 73.13%.

Claims (4)

1. A preparation method for firing a high-strength building ceramic blank at low temperature by adopting low-cost raw materials is characterized by comprising the following steps of: the building ceramic body consists of a base material and a composite additive; the base material comprises the raw materials of 38-45 wt% of prefabricated pug, 16-21 wt% of potassium feldspar, 15-18 wt% of shale, 12-20 wt% of wollastonite and 8-11 wt% of talc; the composite additive consists of 0.1 to 0.15 weight percent of guar gum, 0.05 to 0.1 weight percent of sodium carboxymethyl cellulose and 0.05 to 0.1 weight percent of sodium humate; the raw materials of the prefabricated pug comprise 19-23 wt% of washed sand, 8-14 wt% of kaolin, 37-45 wt% of washed mud, 14-18 wt% of flower mud and 8-14 wt% of coffee mud; the preparation method comprises the following steps:
(1) Preparing raw materials of the prefabricated pug, performing wet ball milling, drying, sieving, and performing powder granulation to obtain mixed prefabricated pug; mixing the mixed prefabricated pug, the potash feldspar, the shale, the wollastonite, the talc and the composite additive, then carrying out wet ball milling, drying and sieving the obtained slurry, and then carrying out powder granulation to obtain a material with a median particle size of 60-80 meshes;
(2) After the granulated material is pressed and molded, the temperature is raised to 1100-1140 ℃ from room temperature at the heating rate of 5-15 ℃/min, the temperature is kept for 30-60 min, the temperature is reduced along with a furnace, and the granulated material is naturally cooled to room temperature, so that a low-temperature sintered high-strength architectural ceramic blank is obtained.
2. The method for preparing a low-temperature-fired high-strength architectural ceramic blank by using low-cost raw materials according to claim 1, wherein the method comprises the following steps: the median particle size of the mixed precast pug is 60-80 meshes, and the particle sizes of the potassium feldspar, the shale, the wollastonite and the talc are all 60-120 meshes.
3. The method for preparing a low-temperature sintered high-strength architectural ceramic blank body by using low-cost raw materials according to claim 1, which is characterized by comprising the following steps: the pressure of the compression molding in the step (2) is 4-6 MPa, and the compression time is 20-30 s.
4. The product obtained by the production method according to any one of claims 1 to 3, characterized in that: the main crystalline phases of the architectural ceramic blank body are anorthite, quartz and diopside, the breaking strength of the ceramic blank body is 85.45-102.53 MPa, and the water absorption is 0.13-0.43%.
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