CN110981195A - Process method for preparing microcrystalline heat-insulation decorative board by utilizing limestone powder - Google Patents
Process method for preparing microcrystalline heat-insulation decorative board by utilizing limestone powder Download PDFInfo
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- CN110981195A CN110981195A CN201911315114.4A CN201911315114A CN110981195A CN 110981195 A CN110981195 A CN 110981195A CN 201911315114 A CN201911315114 A CN 201911315114A CN 110981195 A CN110981195 A CN 110981195A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0063—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing waste materials, e.g. slags
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/08—Other methods of shaping glass by foaming
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/026—Pelletisation or prereacting of powdered raw materials
Abstract
The invention provides a process method for preparing a microcrystalline heat-insulating decorative plate by using limestone powder, belonging to the field of recycling of inorganic non-metallic materials. The process method comprises the steps of sequentially preparing a raw material of a decorative layer, preparing a raw material of a heat-insulating layer, distributing materials in a layered manner, carrying out foaming crystallization heat treatment, and carrying out cold machining on a sintered plate to finally form the heat-insulating layer, wherein the total addition amount of the limestone powder is 68-77% in the processes of preparing the raw material of the decorative layer and preparing the raw material of the heat-insulating layer. According to the invention, the Qing mountain flour is modified through selection and content regulation of additives such as a specific foaming agent, a stabilizer, a blank reinforcing agent, a high-temperature fluxing agent, a strength modifier and the like, so that the modified Qing mountain flour has good high-temperature foaming performance and sintering performance with a microcrystalline decorative surface, and then the heat-insulation decorative board with low cost, excellent physical performance and high added value is produced through a specific temperature system, so that the utilization rate of the Qing mountain flour is up to 77%, and the problem of environmental damage of the low-calcium Qing mountain flour is effectively solved.
Description
Technical Field
The invention relates to the field of recycling of inorganic non-metallic materials, in particular to a process method for preparing a microcrystalline heat-insulating decorative plate by utilizing limestone powder.
Background
The heat-insulating decorative plate is a novel external heat-insulating material for the external wall, has heat-insulating and decorative functions, can greatly save the installation time in the building construction process and save the labor and time cost, and is a new direction of the external heat-insulating technology for the external wall.
The heat-insulating decorative board on the market at present mainly has two main types of once firing and secondary bonding: most of the primary sintering materials are made of inorganic materials through high-temperature foaming sintering, so that the bonding strength and reliability are high, and the service life is long; in the secondary bonding mode, the heat-insulating layer and the decorative layer are bonded together through an organic bonding agent, and the risk of aging failure is gradually increased along with the lapse of time.
At present, a production technology for producing the heat-insulation decorative plate by using slag as a raw material and a one-step sintering process of layered distribution is available, but a literature document for producing the heat-insulation decorative plate by using low-calcium Qing mountain flour as a main raw material is unavailable.
And the limestone powder of the invention has low calcium content, if used for producing cement, additional modifier is needed, which causes the cost to rise sharply, and simultaneously the obtained product has low added value and no economic benefit, thus forming a tail mine by long-term accumulation and seriously damaging the local environment.
Disclosure of Invention
The invention aims to solve the technical problems that the existing Qing mountain flour with low calcium content cannot be used for producing cement, has higher cost and lower product added value, is accumulated for a long time to form a tail mine and seriously damages the local environment.
The invention provides a process method for preparing a microcrystalline heat-insulation decorative plate by using limestone powder, which comprises the steps of preparing a decorative layer raw material, preparing a heat-insulation layer raw material, distributing materials in a layered manner, carrying out foaming crystallization heat treatment, and carrying out cold machining on a sintered plate to finally form, wherein the mass percentage of the total addition of the limestone powder in the processes of preparing the decorative layer raw material and preparing the heat-insulation layer raw material is 68-77%.
Preferably, the components of the green stone powder are as follows: 63-71% of silicon dioxide, 17-20% of aluminum oxide, 0-1% of calcium oxide, 2-6% of magnesium oxide, 1-7% of ferric oxide, 1-3% of potassium oxide, 2-7% of sodium oxide and the balance less than 5%.
Preferably, the process method specifically comprises the following steps:
(1) preparing raw materials of the decorative layer: the raw material of the decorative layer is obtained by rough mixing of ingredients containing the Qingshi powder, melt water quenching and particle size screening;
(2) preparing raw materials of the heat-insulating layer: the insulation layer raw material is obtained by batching, grinding, water mixing and slurry mixing, spray granulation and ageing of the raw material containing the Qing mountain flour;
(3) layering and distributing: arranging the decorative layer raw material obtained in the step (1) and the heat insulation layer raw material obtained in the step (2) in a mould on a kiln car layer by layer through a material distributor;
(4) foaming crystallization heat treatment: the kiln car which finishes the material distribution in the step (3) enters a tunnel kiln to carry out high-temperature heat treatment, and a sintered plate is obtained through a preheating dehydration, sintering shrinkage, foaming crystallization, quick cooling and foam stabilization, stress relief annealing, cooling and discharging from the kiln, foaming crystallization and heat treatment system which are sequentially carried out;
(5) and (3) cold machining of the fired plate: and (5) performing thickness setting, polishing, cutting, packaging and packaging on the fired plate obtained in the step (4) to obtain the finished microcrystal heat-insulation decorative plate.
Preferably, the preparation steps of the raw materials of the decorative layer in the step (1) are as follows: 36-54 parts of green stone powder, 3-5 parts of potassium feldspar, 3-5 parts of albite, 12-18 parts of calcite, 8-16 parts of quartz sand, 1-3 parts of titanium dioxide, 2-4 parts of zinc oxide, 1-3 parts of borax, 2-4 parts of spodumene, 4-7 parts of barium carbonate, 4-7 parts of sodium nitrate and 1-2 parts of glass clarifier are uniformly mixed according to a proportion, then the mixture is conveyed into a melting furnace by a conveyor belt, melted at 1650 ℃ for 4 hours and then flows into a supercooling liquid to obtain amorphous particles, and the amorphous particles are ground and screened to obtain a decorative layer raw material with the particle size of 12-80 meshes.
Preferably, the preparation steps of the raw materials of the heat-insulating layer in the step (2) are as follows: mixing 71-89 parts of green stone powder, 1-3 parts of foaming agent, 0.5-2 parts of stabilizing agent, 0.5-1 part of embryo reinforcing agent, 7-25 parts of high-temperature fluxing agent, 1-3 parts of strength modifier, 2-5 parts of slurry modifier and water, feeding the mixture into a continuous ball mill, grinding and sieving to obtain slurry with the specific gravity of 1.63-1.68 passing through a 200-mesh screen; drying in a spray drying tower to obtain powder balls with diameter of 0.2-0.6mm and water content of 2-4%; and ageing for 24-36 hours to obtain the raw material of the heat-insulating layer.
Preferably, in the layering and distributing process in the step (4): the thickness of the raw material of the decorative layer is 1-12mm, and the thickness of the raw material of the heat-insulating layer is 15-270 mm.
Preferably, the foaming crystallization heat treatment system in the step (4) is as follows:
preheating and dehydrating: heating to 580-640 ℃ at the heating rate of 11-14 ℃/min, and keeping the temperature for 0.1-3 h;
sintering shrinkage: heating to 690 and 770 ℃ at the heating rate of 7-10 ℃/min, and keeping the temperature for 0.1-3 h;
foaming and crystallizing: heating to 1030-1050 ℃ at the heating rate of 4-6 ℃/min, and keeping the temperature for 0.5-5 h;
fast cooling and foam stabilizing: cooling to 880-910 ℃ at a cooling rate of 14-16 ℃/min, and keeping the temperature for 0.5-1 h;
stress relief annealing: cooling to 550 ℃ and 680 ℃ at the cooling rate of 5-7 ℃/min, and preserving heat for 0.5-2 h;
cooling and discharging: cooling to 80 ℃ at the cooling rate of 10-12 ℃/min, and leaving the shuttle kiln to obtain the sintered plate.
Preferably, the foaming agent is one or more of silicon carbide, light calcium powder, heavy calcium powder, titanium hydride, magnesium carbonate, sodium carbonate, manganese dioxide, sodium nitrate, ammonium nitrate, potassium nitrate and calcium sulfate; the stabilizer is one or more of sodium hexametaphosphate, boric acid, borax, phosphorus pentoxide and chromium oxide; the high-temperature fluxing agent is one or more of silicon tetrafluoride, spodumene, calcium fluoride and potash feldspar; the strength modifier is one or more of zirconia, nickel oxide and zirconium silicate; the slurry modifier is one or more of dehydrating agent, sodium methyl cellulose, ammonium chloride, kaolin and clay.
The technical scheme of the invention has the following beneficial effects:
the invention provides a direct foaming sintering technology of the Qing Stone powder by analyzing the physicochemical properties and the component structure of the Qing Stone powder with low calcium content, the Qing Stone powder is modified by selecting and regulating the content of additives such as a foaming agent, a stabilizer, a green body reinforcing agent, a high temperature fluxing agent, a strength modifier and the like, so that the modified Qing Stone powder has good high temperature foaming property and sintering property with a microcrystal decorative surface, and then the heat preservation decorative plate with low cost, excellent physical property and high added value is produced by a specific temperature system of the invention, thereby not only enabling the utilization rate of the Qing Stone powder to reach 77%, but also effectively solving the problem of environmental destruction of the low calcium Qing Stone powder.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
The invention aims to solve the technical problems that the existing Qing mountain flour with low calcium content cannot be used for producing cement, has higher cost and lower product added value, is accumulated for a long time to form a tail mine and seriously damages the local environment.
In order to solve the technical problems, the invention provides a process method for preparing a microcrystal heat-insulation decorative plate by using limestone powder, which comprises the steps of sequentially preparing a decorative layer raw material, preparing a heat-insulation layer raw material, distributing materials in layers, carrying out foaming crystallization heat treatment, and carrying out cold machining on a sintered plate to finally form, wherein the total addition amount of the limestone powder in the processes of preparing the decorative layer raw material and preparing the heat-insulation layer raw material is 68-77% by mass.
In particular, the components of the green stone powder are as follows: 63-71% of silicon dioxide, 17-20% of aluminum oxide, 0-1% of calcium oxide, 2-6% of magnesium oxide, 1-7% of ferric oxide, 1-3% of potassium oxide, 2-7% of sodium oxide and the balance less than 5%.
In particular, the process method specifically comprises the following steps:
(1) preparing raw materials of the decorative layer: the raw material of the decorative layer is obtained by rough mixing of ingredients containing the Qingshi powder, melt water quenching and particle size screening;
(2) preparing raw materials of the heat-insulating layer: the insulation layer raw material is obtained by batching, grinding, water mixing and slurry mixing, spray granulation and ageing of the raw material containing the Qing mountain flour;
(3) layering and distributing: arranging the decorative layer raw material obtained in the step (1) and the heat insulation layer raw material obtained in the step (2) in a mould on a kiln car layer by layer through a material distributor;
(4) foaming crystallization heat treatment: the kiln car which finishes the material distribution in the step (3) enters a tunnel kiln to carry out high-temperature heat treatment, and a sintered plate is obtained through a preheating dehydration, sintering shrinkage, foaming crystallization, quick cooling and foam stabilization, stress relief annealing, cooling and discharging from the kiln, foaming crystallization and heat treatment system which are sequentially carried out;
(5) and (3) cold machining of the fired plate: and (5) performing thickness setting, polishing, cutting, packaging and packaging on the fired plate obtained in the step (4) to obtain the finished microcrystal heat-insulation decorative plate.
Particularly, the preparation steps of the raw materials of the decorative layer in the step (1) are as follows: 36-54 parts of green stone powder, 3-5 parts of potassium feldspar, 3-5 parts of albite, 12-18 parts of calcite, 8-16 parts of quartz sand, 1-3 parts of titanium dioxide, 2-4 parts of zinc oxide, 1-3 parts of borax, 2-4 parts of spodumene, 4-7 parts of barium carbonate, 4-7 parts of sodium nitrate and 1-2 parts of glass clarifier are uniformly mixed according to a proportion, then the mixture is conveyed into a melting furnace by a conveyor belt, melted at 1650 ℃ for 4 hours and then flows into a supercooling liquid to obtain amorphous particles, and the amorphous particles are ground and screened to obtain a decorative layer raw material with the particle size of 12-80 meshes.
Particularly, the preparation steps of the raw materials of the heat-insulating layer in the step (2) are as follows: mixing 71-89 parts of green stone powder, 1-3 parts of foaming agent, 0.5-2 parts of stabilizing agent, 0.5-1 part of embryo reinforcing agent, 7-25 parts of high-temperature fluxing agent, 1-3 parts of strength modifier, 2-5 parts of slurry modifier and water, feeding the mixture into a continuous ball mill, grinding and sieving to obtain slurry with the specific gravity of 1.63-1.68 passing through a 200-mesh screen; drying in a spray drying tower to obtain powder balls with diameter of 0.2-0.6mm and water content of 2-4%; and ageing for 24-36 hours to obtain the raw material of the heat-insulating layer.
In particular, in the layering and distributing process in the step (4): the thickness of the raw material of the decorative layer is 1-12mm, and the thickness of the raw material of the heat-insulating layer is 15-270 mm.
Preferably, the foaming crystallization heat treatment system in the step (4) is as follows:
preheating and dehydrating: heating to 580-640 ℃ at the heating rate of 11-14 ℃/min, and keeping the temperature for 0.1-3 h;
sintering shrinkage: heating to 690 and 770 ℃ at the heating rate of 7-10 ℃/min, and keeping the temperature for 0.1-3 h;
foaming and crystallizing: heating to 1030-1050 ℃ at the heating rate of 4-6 ℃/min, and keeping the temperature for 0.5-5 h;
fast cooling and foam stabilizing: cooling to 880-910 ℃ at a cooling rate of 14-16 ℃/min, and keeping the temperature for 0.5-1 h;
stress relief annealing: cooling to 550 ℃ and 680 ℃ at the cooling rate of 5-7 ℃/min, and preserving heat for 0.5-2 h;
cooling and discharging: cooling to 80 ℃ at the cooling rate of 10-12 ℃/min, and leaving the shuttle kiln to obtain the sintered plate.
Particularly, the foaming agent is one or more of silicon carbide, light calcium powder, heavy calcium powder, titanium hydride, magnesium carbonate, sodium carbonate, manganese dioxide, sodium nitrate, ammonium nitrate, potassium nitrate and calcium sulfate; the stabilizer is one or more of sodium hexametaphosphate, boric acid, borax, phosphorus pentoxide and chromium oxide; the high-temperature fluxing agent is one or more of silicon tetrafluoride, spodumene, calcium fluoride and potash feldspar; the strength modifier is one or more of zirconia, nickel oxide and zirconium silicate; the slurry modifier is one or more of dehydrating agent, sodium methyl cellulose, ammonium chloride, kaolin and clay.
The specific process method for preparing the microcrystalline heat-insulating decorative board by using the Qing mountain flour is described by combining the following examples:
TABLE 1 raw material ratio of decorative layer
TABLE 2 insulating layer raw material ratio
| DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION | Qing mountain flour | Foaming agent | Stabilizer | High temperature fluxing agent | Strength modifier | Slurry modifier |
| Example 1 | 71 | 1.4 | 0.8 | 23 | 1.8 | 2 |
| Example 2 | 76 | 1.6 | 1.1 | 16 | 2.3 | 3 |
| Example 3 | 79 | 2.1 | 0.8 | 12 | 2.1 | 4 |
| Example 4 | 82 | 2.3 | 1.8 | 9 | 1.9 | 3 |
| Example 5 | 89 | 1.9 | 0.6 | 4 | 2.5 | 2 |
TABLE 3 selection and proportioning of the components of the slurry modifier, 100%
| DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION | Dehydrating agent | Sodium methyl cellulose | Ammonium chloride | Kaolin clay | Clay clay |
| Example 1 | 13 | 21 | 21 | 31 | 14 |
| Example 2 | 11 | 24 | 27 | 33 | 5 |
| Example 3 | 15 | 18 | 24 | 43 | 0 |
| Example 4 | 14 | 22 | 26 | 25 | 13 |
| Example 5 | 17 | 26 | 22 | 35 | 0 |
TABLE 4 selection and proportioning of blowing agent, foam stabilizer, high temperature flux, strength modifier
TABLE 5 sample Performance test indexes for the respective examples
TABLE 6 Green stone powder component test results of each example
The first embodiment is as follows:
a process method for preparing a microcrystalline heat-insulating decorative board by using limestone powder comprises the following specific steps:
(1) preparing raw materials of the decorative layer: the raw material of the decorative layer is obtained by rough mixing of ingredients containing the Qingshi powder, melt water quenching and particle size screening;
(2) preparing raw materials of the heat-insulating layer: the insulation layer raw material is obtained by batching, grinding, water mixing and slurry mixing, spray granulation and ageing of the raw material containing the Qing mountain flour;
(3) layering and distributing: arranging the decorative layer raw material obtained in the step (1) and the heat insulation layer raw material obtained in the step (2) in a mould on a kiln car layer by layer through a material distributor;
(4) foaming crystallization heat treatment: the kiln car which finishes the material distribution in the step (3) enters a tunnel kiln to carry out high-temperature heat treatment, and a sintered plate is obtained through a preheating dehydration, sintering shrinkage, foaming crystallization, quick cooling and foam stabilization, stress relief annealing, cooling and discharging from the kiln, foaming crystallization and heat treatment system which are sequentially carried out;
(5) and (3) cold machining of the fired plate: and (5) performing thickness setting, polishing, cutting, packaging and packaging on the fired plate obtained in the step (4) to obtain the finished microcrystal heat-insulation decorative plate.
Wherein, the total addition amount of the limestone powder in the processes of preparing the raw material of the decorative layer and the raw material of the heat-insulating layer is 68 to 77 percent by mass.
Wherein the components of the limestone powder are shown in example 1 in table 6.
The preparation method of the raw materials of the decorative layer in the step (1) comprises the following steps: uniformly mixing the raw materials according to the proportion shown in example 1 in the table 1, conveying the mixture into a melting furnace by a conveyor belt, melting the mixture at 1650 ℃ for 4 hours, then flowing into a supercooled liquid to obtain amorphous particles, and grinding and screening the amorphous particles to obtain the decorative layer raw material with the particle size of 12 meshes.
The preparation method of the heat-insulating layer raw material in the step (2) comprises the following steps: mixing the mixture with water according to the proportion shown in example 1 in the table 2, feeding the mixture into a continuous ball mill for grinding and sieving to obtain slurry with the specific gravity of 1.63 passing through a 200-mesh screen; drying by a spray drying tower to obtain powder pellets with the diameter of 0.2mm and the water content of 2%; and ageing for 36 hours to obtain the raw material of the heat-insulating layer.
Wherein, in the layering and distributing process in the step (4): the thickness of the raw materials of the decoration layer is 1mm, and the thickness of the raw materials of the heat insulation layer is 15 mm.
Wherein the foaming crystallization heat treatment system in the step (4) is as follows:
preheating and dehydrating: heating to 640 ℃ at the heating rate of 14 ℃/min, and keeping the temperature for 0.1 h;
sintering shrinkage: heating to 770 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 0.1 h;
foaming and crystallizing: heating to 1050 ℃ at the heating rate of 6 ℃/min, and keeping the temperature for 0.5 h;
fast cooling and foam stabilizing: cooling to 910 ℃ at a cooling rate of 16 ℃/min, and keeping the temperature for 0.5 h;
stress relief annealing: cooling to 680 ℃ at a cooling rate of 7 ℃/min, and keeping the temperature for 0.5 h;
cooling and discharging: cooling to 80 ℃ at the cooling rate of 12 ℃/min, and leaving the shuttle kiln to obtain the sintered plate.
Wherein, the selection and the proportion of the components of the foaming agent, the foam stabilizer, the high-temperature fluxing agent and the strength modifier are shown in the example 1 in the table 4; the selection and formulation of the slurry modifier components are shown in example 1 of table 3.
The sample performance detection indexes of the finished microcrystalline heat-insulating decorative board are shown in table 5, namely example 1.
Example two:
a process method for preparing a microcrystalline heat-insulating decorative board by using limestone powder comprises the following specific steps:
(1) preparing raw materials of the decorative layer: the raw material of the decorative layer is obtained by rough mixing of ingredients containing the Qingshi powder, melt water quenching and particle size screening;
(2) preparing raw materials of the heat-insulating layer: the insulation layer raw material is obtained by batching, grinding, water mixing and slurry mixing, spray granulation and ageing of the raw material containing the Qing mountain flour;
(3) layering and distributing: arranging the decorative layer raw material obtained in the step (1) and the heat insulation layer raw material obtained in the step (2) in a mould on a kiln car layer by layer through a material distributor;
(4) foaming crystallization heat treatment: the kiln car which finishes the material distribution in the step (3) enters a tunnel kiln to carry out high-temperature heat treatment, and a sintered plate is obtained through a preheating dehydration, sintering shrinkage, foaming crystallization, quick cooling and foam stabilization, stress relief annealing, cooling and discharging from the kiln, foaming crystallization and heat treatment system which are sequentially carried out;
(5) and (3) cold machining of the fired plate: and (5) performing thickness setting, polishing, cutting, packaging and packaging on the fired plate obtained in the step (4) to obtain the finished microcrystal heat-insulation decorative plate.
Wherein, the total addition amount of the limestone powder in the processes of preparing the raw material of the decorative layer and the raw material of the heat-insulating layer is 68 to 77 percent by mass.
Wherein the components of the limestone powder are shown in example 2 in table 6.
The preparation method of the raw materials of the decorative layer in the step (1) comprises the following steps: uniformly mixing the raw materials according to the proportion shown in example 2 in the table 1, conveying the mixture into a melting furnace by a conveyor belt, melting the mixture at 1650 ℃ for 4 hours, then flowing into a supercooled liquid to obtain amorphous particles, and grinding and screening the amorphous particles to obtain the decorative layer raw material with the granularity of 80 meshes.
The preparation method of the heat-insulating layer raw material in the step (2) comprises the following steps: mixing the mixture with water according to the proportion shown in example 2 in the table 2, feeding the mixture into a continuous ball mill for grinding and sieving to obtain slurry with the specific gravity of 1.63 passing through a 200-mesh screen; drying by a spray drying tower to obtain powder pellets with the diameter of 0.6mm and the water content of 4%; and ageing for 24 hours to obtain the raw material of the heat-insulating layer.
Wherein, in the layering and distributing process in the step (4): the thickness of the raw materials of the decoration layer is 12mm, and the thickness of the raw materials of the heat insulation layer is 270 mm.
Wherein the foaming crystallization heat treatment system in the step (4) is as follows:
preheating and dehydrating: heating to 580 ℃ at the heating rate of 11 ℃/min, and keeping the temperature for 3 h;
sintering shrinkage: heating to 690 ℃ at the heating rate of 7 ℃/min, and keeping the temperature for 3 h;
foaming and crystallizing: heating to 1030 ℃ at the heating rate of 4 ℃/min, and keeping the temperature for 5 hours;
fast cooling and foam stabilizing: cooling to 880 ℃ at a cooling rate of 14 ℃/min, and keeping the temperature for 1 h;
stress relief annealing: cooling to 550 ℃ at a cooling rate of 5 ℃/min, and keeping the temperature for 2 h;
cooling and discharging: cooling to 80 ℃ at the cooling rate of 10 ℃/min, and leaving the shuttle kiln to obtain the sintered plate.
Wherein, the selection and the proportion of the components of the foaming agent, the foam stabilizer, the high-temperature fluxing agent and the strength modifier are shown in the example 2 in the table 4; the slurry modifier components were selected and proportioned as shown in example 2 of table 3.
The sample performance detection indexes of the finished microcrystalline heat-insulating decorative board are shown in Table 5 in example 2.
Example three:
a process method for preparing a microcrystalline heat-insulating decorative board by using limestone powder comprises the following specific steps:
(1) preparing raw materials of the decorative layer: the raw material of the decorative layer is obtained by rough mixing of ingredients containing the Qingshi powder, melt water quenching and particle size screening;
(2) preparing raw materials of the heat-insulating layer: the insulation layer raw material is obtained by batching, grinding, water mixing and slurry mixing, spray granulation and ageing of the raw material containing the Qing mountain flour;
(3) layering and distributing: arranging the decorative layer raw material obtained in the step (1) and the heat insulation layer raw material obtained in the step (2) in a mould on a kiln car layer by layer through a material distributor;
(4) foaming crystallization heat treatment: the kiln car which finishes the material distribution in the step (3) enters a tunnel kiln to carry out high-temperature heat treatment, and a sintered plate is obtained through a preheating dehydration, sintering shrinkage, foaming crystallization, quick cooling and foam stabilization, stress relief annealing, cooling and discharging from the kiln, foaming crystallization and heat treatment system which are sequentially carried out;
(5) and (3) cold machining of the fired plate: and (5) performing thickness setting, polishing, cutting, packaging and packaging on the fired plate obtained in the step (4) to obtain the finished microcrystal heat-insulation decorative plate.
Wherein, the total addition amount of the limestone powder in the processes of preparing the raw material of the decorative layer and the raw material of the heat-insulating layer is 68 to 77 percent by mass.
Wherein the components of the limestone powder are shown in example 3 in table 6.
The preparation method of the raw materials of the decorative layer in the step (1) comprises the following steps: uniformly mixing the raw materials according to the proportion shown in the example 3 in the table 1, conveying the mixture into a melting furnace by a conveyor belt, melting the mixture at 1650 ℃ for 4 hours, then flowing into supercooled liquid to obtain amorphous particles, and grinding and screening the amorphous particles to obtain the decorative layer raw material with the particle size of 40 meshes.
The preparation method of the heat-insulating layer raw material in the step (2) comprises the following steps: mixing the mixture with water according to the proportion shown in example 3 in the table 2, feeding the mixture into a continuous ball mill for grinding and sieving to obtain slurry with the specific gravity of 1.65 passing through a 200-mesh screen; drying by a spray drying tower to obtain powder pellets with the diameter of 0.4mm and the water content of 3 percent; and ageing for 30 hours to obtain the raw material of the heat-insulating layer.
Wherein, in the layering and distributing process in the step (4): the thickness of the raw materials of the decoration layer is 7mm, and the thickness of the raw materials of the heat insulation layer is 140 mm.
Wherein the foaming crystallization heat treatment system in the step (4) is as follows:
preheating and dehydrating: heating to 610 ℃ at the heating rate of 12 ℃/min, and keeping the temperature for 1.5 h;
sintering shrinkage: heating to 730 ℃ at the heating rate of 8 ℃/min, and keeping the temperature for 1.5 h;
foaming and crystallizing: heating to 1040 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 2.7 h;
fast cooling and foam stabilizing: cooling to 890 ℃ at the cooling rate of 15 ℃/min, and keeping the temperature for 0.7 h;
stress relief annealing: cooling to 610 ℃ at the cooling rate of 6 ℃/min, and keeping the temperature for 1.7 h;
cooling and discharging: cooling to 80 ℃ at the cooling rate of 11 ℃/min, and leaving the shuttle kiln to obtain the sintered plate.
Wherein, the selection and the proportion of the components of the foaming agent, the foam stabilizer, the high-temperature fluxing agent and the strength modifier are shown in the embodiment 3 in the table 4; the slurry modifier component selection and formulation is shown in example 3 of table 3.
The sample performance detection indexes of the finished microcrystalline heat-insulating decorative board are shown in Table 5, namely, in example 3.
Example four:
a process method for preparing a microcrystalline heat-insulating decorative board by using limestone powder comprises the following specific steps:
(1) preparing raw materials of the decorative layer: the raw material of the decorative layer is obtained by rough mixing of ingredients containing the Qingshi powder, melt water quenching and particle size screening;
(2) preparing raw materials of the heat-insulating layer: the insulation layer raw material is obtained by batching, grinding, water mixing and slurry mixing, spray granulation and ageing of the raw material containing the Qing mountain flour;
(3) layering and distributing: arranging the decorative layer raw material obtained in the step (1) and the heat insulation layer raw material obtained in the step (2) in a mould on a kiln car layer by layer through a material distributor;
(4) foaming crystallization heat treatment: the kiln car which finishes the material distribution in the step (3) enters a tunnel kiln to carry out high-temperature heat treatment, and a sintered plate is obtained through a preheating dehydration, sintering shrinkage, foaming crystallization, quick cooling and foam stabilization, stress relief annealing, cooling and discharging from the kiln, foaming crystallization and heat treatment system which are sequentially carried out;
(5) and (3) cold machining of the fired plate: and (5) performing thickness setting, polishing, cutting, packaging and packaging on the fired plate obtained in the step (4) to obtain the finished microcrystal heat-insulation decorative plate.
Wherein, the total addition amount of the limestone powder in the processes of preparing the raw material of the decorative layer and the raw material of the heat-insulating layer is 68 to 77 percent by mass.
Wherein the components of the limestone powder are shown in example 4 in table 6.
The preparation method of the raw materials of the decorative layer in the step (1) comprises the following steps: uniformly mixing the raw materials according to the proportion shown in example 4 in the table 1, conveying the mixture into a melting furnace by a conveyor belt, melting the mixture at 1650 ℃ for 4 hours, then flowing into a supercooled liquid to obtain amorphous particles, and grinding and screening the amorphous particles to obtain the decorative layer raw material with the particle size of 25 meshes.
The preparation method of the heat-insulating layer raw material in the step (2) comprises the following steps: mixing the mixture with water according to the proportion shown in example 4 in the table 2, feeding the mixture into a continuous ball mill for grinding and sieving to obtain slurry with the specific gravity of 1.64 passing through a 200-mesh screen; drying by a spray drying tower to obtain powder pellets with the diameter of 0.3mm and the water content of 2.5 percent; and ageing for 28 hours to obtain the raw material of the heat-insulating layer.
Wherein, in the layering and distributing process in the step (4): the thickness of the raw materials of the decoration layer is 3mm, and the thickness of the raw materials of the heat insulation layer is 80 mm.
Wherein the foaming crystallization heat treatment system in the step (4) is as follows:
preheating and dehydrating: heating to 590 ℃ at the heating rate of 12 ℃/min, and keeping the temperature for 2 h;
sintering shrinkage: heating to 710 ℃ at the heating rate of 8 ℃/min, and keeping the temperature for 2 h;
foaming and crystallizing: heating to 1035 ℃ at a heating rate of 4.5 ℃/min, and keeping the temperature for 4 h;
fast cooling and foam stabilizing: cooling to 890 ℃ at a cooling rate of 14.5 ℃/min, and keeping the temperature for 0.6 h;
stress relief annealing: cooling to 570 ℃ at the cooling rate of 5.5 ℃/min, and keeping the temperature for 1 h;
cooling and discharging: cooling to 80 ℃ at the cooling rate of 10.5 ℃/min, and leaving the shuttle kiln to obtain the sintered plate.
Wherein, the selection and the proportion of the components of the foaming agent, the foam stabilizer, the high-temperature fluxing agent and the strength modifier are shown in the example 4 in the table 4; the slurry modifier component selection and formulation is shown in example 4 of table 3.
The sample performance detection indexes of the finished microcrystalline heat-insulating decorative board are shown in Table 5, example 4.
Example five:
a process method for preparing a microcrystalline heat-insulating decorative board by using limestone powder comprises the following specific steps:
(1) preparing raw materials of the decorative layer: the raw material of the decorative layer is obtained by rough mixing of ingredients containing the Qingshi powder, melt water quenching and particle size screening;
(2) preparing raw materials of the heat-insulating layer: the insulation layer raw material is obtained by batching, grinding, water mixing and slurry mixing, spray granulation and ageing of the raw material containing the Qing mountain flour;
(3) layering and distributing: arranging the decorative layer raw material obtained in the step (1) and the heat insulation layer raw material obtained in the step (2) in a mould on a kiln car layer by layer through a material distributor;
(4) foaming crystallization heat treatment: the kiln car which finishes the material distribution in the step (3) enters a tunnel kiln to carry out high-temperature heat treatment, and a sintered plate is obtained through a preheating dehydration, sintering shrinkage, foaming crystallization, quick cooling and foam stabilization, stress relief annealing, cooling and discharging from the kiln, foaming crystallization and heat treatment system which are sequentially carried out;
(5) and (3) cold machining of the fired plate: and (5) performing thickness setting, polishing, cutting, packaging and packaging on the fired plate obtained in the step (4) to obtain the finished microcrystal heat-insulation decorative plate.
Wherein, the total addition amount of the limestone powder in the processes of preparing the raw material of the decorative layer and the raw material of the heat-insulating layer is 68 to 77 percent by mass.
Wherein the components of the limestone powder are shown in example 5 in table 6.
The preparation method of the raw materials of the decorative layer in the step (1) comprises the following steps: uniformly mixing the raw materials according to the proportion shown in the example 5 in the table 1, conveying the mixture into a melting furnace by a conveyor belt, melting the mixture at 1650 ℃ for 4 hours, then flowing into supercooled liquid to obtain amorphous particles, and grinding and screening the amorphous particles to obtain the decorative layer raw material with the granularity of 70 meshes.
The preparation method of the heat-insulating layer raw material in the step (2) comprises the following steps: : mixing the mixture with water according to the proportion shown in example 4 in the table 2, feeding the mixture into a continuous ball mill for grinding and sieving to obtain slurry with the specific gravity of 1.65 passing through a 200-mesh screen; drying by a spray drying tower to obtain powder pellets with the diameter of 0.5mm and the water content of 3 percent; and ageing for 32 hours to obtain the raw material of the heat-insulating layer.
Wherein, in the layering and distributing process in the step (4): the thickness of the raw materials of the decoration layer is 10mm, and the thickness of the raw materials of the heat insulation layer is 200 mm.
Wherein the foaming crystallization heat treatment system in the step (4) is as follows:
preheating and dehydrating: heating to 620 ℃ at the heating rate of 13 ℃/min, and keeping the temperature for 0.6 h;
sintering shrinkage: heating to 750 ℃ at the heating rate of 9 ℃/min, and keeping the temperature for 0.6 h;
foaming and crystallizing: heating to 1045 ℃ at the heating rate of 5.5 ℃/min, and keeping the temperature for 1 h;
fast cooling and foam stabilizing: cooling to 900 ℃ at a cooling rate of 15.5 ℃/min, and keeping the temperature for 0.6 h;
stress relief annealing: cooling to 630 ℃ at a cooling rate of 6.5 ℃/min, and keeping the temperature for 0.9 h;
cooling and discharging: cooling to 80 ℃ at the cooling rate of 11.5 ℃/min, and leaving the shuttle kiln to obtain the sintered plate.
Wherein, the selection and the proportion of the components of the foaming agent, the foam stabilizer, the high-temperature fluxing agent and the strength modifier are shown in the example 5 in the table 4; the slurry modifier component selection and formulation is shown in example 5 of table 3.
The sample performance detection indexes of the finished microcrystalline heat-insulating decorative board are shown in Table 5 in example 5.
In conclusion, the invention provides a direct foaming sintering technology for the Qing mountain flour by analyzing the physicochemical properties and the component structure of the Qing mountain flour with low calcium content, the Qing mountain flour is modified by selecting and regulating the content of additives such as a foaming agent, a stabilizing agent, a blank reinforcing agent, a high-temperature fluxing agent, a strength modifying agent and the like, so that the modified Qing mountain flour has good high-temperature foaming property and sintering property with a microcrystal decorative surface, and then the heat-insulating decorative plate with low cost, excellent physical property and high additional value is produced by a specific temperature system of the invention, so that the utilization rate of the Qing mountain flour is up to 77 percent, and the problem of environmental destruction of the low-calcium Qing mountain flour is effectively solved.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A process method for preparing a microcrystal heat-insulation decorative plate by using limestone powder is characterized by comprising the steps of preparing a decorative layer raw material, preparing a heat-insulation layer raw material, distributing materials in a layering manner, carrying out foaming crystallization heat treatment, and carrying out cold machining on a sintered plate to finally form, wherein the mass percent of the total addition amount of the limestone powder in the processes of preparing the decorative layer raw material and preparing the heat-insulation layer raw material is 68-77%.
2. The process method for preparing the microcrystal heat-insulation decorative plate by using the limestone powder as claimed in claim 1, wherein the limestone powder comprises the following components: 63-71% of silicon dioxide, 17-20% of aluminum oxide, 0-1% of calcium oxide, 2-6% of magnesium oxide, 1-7% of ferric oxide, 1-3% of potassium oxide, 2-7% of sodium oxide and the balance less than 5%.
3. The process method for preparing the microcrystalline heat-insulating decorative board by using the limestone powder as claimed in claim 1, wherein the process method specifically comprises the following steps:
(1) preparing raw materials of the decorative layer: the raw material of the decorative layer is obtained by rough mixing of ingredients containing the Qingshi powder, melt water quenching and particle size screening;
(2) preparing raw materials of the heat-insulating layer: the insulation layer raw material is obtained by batching, grinding, water mixing and slurry mixing, spray granulation and ageing of the raw material containing the Qing mountain flour;
(3) layering and distributing: arranging the decorative layer raw material obtained in the step (1) and the heat insulation layer raw material obtained in the step (2) in a mould on a kiln car layer by layer through a material distributor;
(4) foaming crystallization heat treatment: the kiln car which finishes the material distribution in the step (3) enters a tunnel kiln to carry out high-temperature heat treatment, and a sintered plate is obtained through a preheating dehydration, sintering shrinkage, foaming crystallization, quick cooling and foam stabilization, stress relief annealing, cooling and discharging from the kiln, foaming crystallization and heat treatment system which are sequentially carried out;
(5) and (3) cold machining of the fired plate: and (5) performing thickness setting, polishing, cutting, packaging and packaging on the fired plate obtained in the step (4) to obtain the finished microcrystal heat-insulation decorative plate.
4. The process method for preparing a microcrystalline heat-insulating decorative board by using the limestone powder as claimed in claim 3, wherein the preparation steps of the raw materials of the decorative layer in the step (1) are as follows: 36-54 parts of green stone powder, 3-5 parts of potassium feldspar, 3-5 parts of albite, 12-18 parts of calcite, 8-16 parts of quartz sand, 1-3 parts of titanium dioxide, 2-4 parts of zinc oxide, 1-3 parts of borax, 2-4 parts of spodumene, 4-7 parts of barium carbonate, 4-7 parts of sodium nitrate and 1-2 parts of glass clarifier are uniformly mixed according to a proportion, then the mixture is conveyed into a melting furnace by a conveyor belt, melted at 1650 ℃ for 4 hours and then flows into a supercooling liquid to obtain amorphous particles, and the amorphous particles are ground and screened to obtain a decorative layer raw material with the particle size of 12-80 meshes.
5. The process method for preparing the microcrystal heat-insulation decorative plate by using the limestone powder as claimed in claim 3, wherein the heat-insulation layer raw material in the step (2) is prepared by the following steps: mixing 71-89 parts of green stone powder, 1-3 parts of foaming agent, 0.5-2 parts of stabilizing agent, 0.5-1 part of embryo reinforcing agent, 7-25 parts of high-temperature fluxing agent, 1-3 parts of strength modifier, 2-5 parts of slurry modifier and water, feeding the mixture into a continuous ball mill, grinding and sieving to obtain slurry with the specific gravity of 1.63-1.68 passing through a 200-mesh screen; drying in a spray drying tower to obtain powder balls with diameter of 0.2-0.6mm and water content of 2-4%; and ageing for 24-36 hours to obtain the raw material of the heat-insulating layer.
6. The process method for preparing microcrystal heat-insulation decorative plate by using limestone powder as claimed in claim 3, wherein in the layered material distribution process of step (4): the thickness of the raw material of the decorative layer is 1-12mm, and the thickness of the raw material of the heat-insulating layer is 15-270 mm.
7. The process method for preparing a microcrystalline heat-insulating decorative board by using the limestone powder as claimed in claim 3, wherein the foaming crystallization heat treatment system in the step (4) is as follows:
preheating and dehydrating: heating to 580-640 ℃ at the heating rate of 11-14 ℃/min, and keeping the temperature for 0.1-3 h;
sintering shrinkage: heating to 690 and 770 ℃ at the heating rate of 7-10 ℃/min, and keeping the temperature for 0.1-3 h;
foaming and crystallizing: heating to 1030-1050 ℃ at the heating rate of 4-6 ℃/min, and keeping the temperature for 0.5-5 h;
fast cooling and foam stabilizing: cooling to 880-910 ℃ at a cooling rate of 14-16 ℃/min, and keeping the temperature for 0.5-1 h;
stress relief annealing: cooling to 550 ℃ and 680 ℃ at the cooling rate of 5-7 ℃/min, and preserving heat for 0.5-2 h;
cooling and discharging: cooling to 80 ℃ at the cooling rate of 10-12 ℃/min, and leaving the shuttle kiln to obtain the sintered plate.
8. The process method for preparing the microcrystalline heat-preservation decorative board by using the limestone powder as claimed in claim 4 or 5, wherein the foaming agent is one or more of silicon carbide, light calcium powder, heavy calcium powder, titanium hydride, magnesium carbonate, sodium carbonate, manganese dioxide, sodium nitrate, ammonium nitrate, potassium nitrate and calcium sulfate; the stabilizer is one or more of sodium hexametaphosphate, boric acid, borax, phosphorus pentoxide and chromium oxide; the high-temperature fluxing agent is one or more of silicon tetrafluoride, spodumene, calcium fluoride and potash feldspar; the strength modifier is one or more of zirconia, nickel oxide and zirconium silicate; the slurry modifier is one or more of dehydrating agent, sodium methyl cellulose, ammonium chloride, kaolin and clay.
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