CN112552036A - Wollastonite tailing reinforcing and toughening low-temperature ceramic tile and preparation method thereof - Google Patents

Wollastonite tailing reinforcing and toughening low-temperature ceramic tile and preparation method thereof Download PDF

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CN112552036A
CN112552036A CN202011549344.XA CN202011549344A CN112552036A CN 112552036 A CN112552036 A CN 112552036A CN 202011549344 A CN202011549344 A CN 202011549344A CN 112552036 A CN112552036 A CN 112552036A
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wollastonite
parts
ceramic tile
low
tailings
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CN112552036B (en
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查越
黄弘
胡海泉
况慧芸
文园
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Jingdezhen Ceramic Institute
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Jingdezhen Ceramic Institute
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Abstract

The invention discloses a wollastonite tailing reinforcing and toughening low-temperature ceramic tile which comprises the following raw materials in parts by weight: 35-45 parts of wollastonite tailings, 18-32 parts of low-temperature sand, 2-7 parts of medium-temperature sand, 10-18 parts of quartz, 2-4 parts of talcum, 0-5 parts of magnesia clay, 2-5 parts of bentonite, 0.5-3 parts of bauxite, 0.5-2 parts of zircon sand and 0-3 parts of borocalcite; and sintering the ceramic at 1120-1150 deg.C. In addition, a preparation method of the wollastonite tailing reinforcing and toughening low-temperature ceramic tile is also disclosed. The invention takes wollastonite tailings as a main raw material, realizes low-temperature sintering through formula design, and obtains the ceramic tile with high strength and toughness. The invention realizes the resource utilization of the wollastonite tailings, applies the wollastonite tailings to the production of building ceramics in a large amount and improves the added value of the tailings. The invention effectively improves the mechanical strength and toughness of the ceramic building tile, and can be further expanded to the large-scale thin plate production technology in the ceramic building field.

Description

Wollastonite tailing reinforcing and toughening low-temperature ceramic tile and preparation method thereof
Technical Field
The invention relates to the technical field of building ceramic materials, in particular to a reinforcing and toughening low-temperature ceramic tile taking wollastonite tailings as a main raw material and a preparation method thereof.
Background
The ceramic industry belongs to the high-energy-consumption and high-pollution industry, taking the ceramic building tiles as an example, the annual output of the ceramic building tiles in China is about 40 hundred million square meters, and when the annual output is calculated according to 20-24 kg per square meter, 8000-9600-kiloton of mud materials and mineral materials are consumed every year; the fuel heavy oil consumption is 5.6 to 6.0 hundred million liters per year, calculated as 1.4 to 1.5 liters per square meter of fuel heavy oil consumption. The vitrified tile is one of main products of building ceramics, and accounts for about 1/6, namely, about 7.0 hundred million square meters is produced every year, about 1600 million tons of pug and mineral materials are consumed, about 1.0 hundred million liters of fuel oil is consumed every year, and a large amount of raw materials and fuel are consumed. It is imperative to reduce energy consumption and improve resource utilization. Therefore, the low-temperature fast burning technology in the field of building ceramics is produced. For example, the low-temperature quick-firing marble tile using the edge grinding waste residue of the marble tile as the raw material makes full use of the waste residue in ceramic building production, but the highest flexural strength of the product is only 45MPa, and the high requirement on the granularity of the waste residue is provided, so that more extra energy consumption can be still generated in the processing treatment. For another example, the ceramic tile prepared from the albite powder at 1150-1160 ℃ is difficult to realize large-scale production and practical application because a large amount of bentonite is used in the formula, the loss of green bodies is large, the tile shape is difficult to control, the price of the bentonite is high, and the cost of raw materials is increased due to the large amount of bentonite used. Therefore, the problems of low strength, poor toughness, high cost and the like of the low-temperature fast-fired brick in the prior art are still generally existed.
The wollastonite in China is abundant in reserves, a plurality of mineral deposits are found in Jilin, Liaoning, Heilongjiang, Hubei, Anhui, Jiangxi and the like, and the wollastonite reserves proven in 15 provinces (cities) in China are 13895.8 million tons at present. Wollastonite has a plurality of applications in the field of low-temperature fast-firing ceramics, but the prior art uses high-quality ceramic raw materials, and the adopted wollastonite is the preferred wollastonite fine powder, so that the production cost is higher.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a wollastonite tailing reinforcing and toughening low-temperature ceramic tile, which takes wollastonite tailing as a main raw material, realizes low-temperature sintering through formula design and obtains a ceramic tile with high strength and toughness. The invention also aims to provide a preparation method of the wollastonite tailing reinforced and toughened low-temperature ceramic tile.
The purpose of the invention is realized by the following technical scheme:
the invention provides a wollastonite tailing reinforcing and toughening low-temperature ceramic tile which comprises the following raw materials in parts by weight: 35-45 parts of wollastonite tailings, 18-32 parts of low-temperature sand, 2-7 parts of medium-temperature sand, 10-18 parts of quartz, 2-4 parts of talcum, 0-5 parts of magnesia clay, 2-5 parts of bentonite, 0.5-3 parts of bauxite, 0.5-2 parts of zircon sand and 0-3 parts of borocalcite; and sintering the ceramic at 1120-1150 deg.C.
Furthermore, the content of calcite in the wollastonite tailings is less than or equal to 24 wt%, and the content of quartz is less than or equal to 10 wt%. Specifically, the wollastonite tailing sand disclosed by the invention comprises the following mineral components: 50-65 wt% of wollastonite, 18-24 wt% of calcite, 4-10 wt% of quartz, 5-10 wt% of diopside and 3-8 wt% of amorphous phase.
With the change of the raw material composition, the main crystal phases of the ceramic tile are four or five combinations of wollastonite, anorthite, diopside, mullite and quartz.
In the scheme, the chemical composition of the ceramic tile is SiO2 60～68％、Al2O3 6.5～8.5％、TiO2+Fe2O3 0.3～0.6％、CaO 16～21％、MgO 3.4～4.2％、K2O 1.2～2.5％、Na2O 1.4～3.2％、B2O5 0～0.4％、ZrO2 0.3～1.5％。
The other purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of the wollastonite tailing reinforcing and toughening low-temperature ceramic tile, which comprises the following steps:
(1) ball-milling and mixing the materials except the wollastonite tailings in the raw materials by taking water as a medium to obtain slurry with the water content of 33.5-35.5%;
(2) adding wollastonite tailings, a ceramic dispergator and a forming agent, and continuously performing ball milling and mixing to obtain slurry with the particle fineness D50 of 18-25 mu m; the dosage of the ceramic debonder and the molding agent is 0.1-0.15 wt% and 0.2-0.4 wt% of the raw materials respectively;
(3) sieving the slurry to remove iron, drying and granulating to obtain powder;
(4) and (3) sieving the powder, ageing, carrying out compression molding to obtain a green brick, and firing at 1120-1150 ℃ to obtain the wollastonite tailing reinforcing and toughening low-temperature ceramic tile.
Further, the ceramic debonder prepared by the preparation method provided by the invention is one or two of sodium tripolyphosphate, sodium metasilicate pentahydrate, sodium hexametaphosphate and sodium humate; the forming agent is one or the combination of sodium carboxymethylcellulose, polyvinyl alcohol and chitosan.
Further, the ball milling time in the step (1) of the preparation method is 20-29 h; the ball milling time in the step (2) is 3-5 h.
The invention has the following beneficial effects:
(1) the wollastonite tailings are tailings of associated minerals containing more impurities such as calcite, wollastonite, quartz and the like after wollastonite raw ores are selected. The invention uses the wollastonite which is not selected from wollastonite tailings as a main body, and part of CaSiO is in the temperature range of 1120-1150 DEG C3The anorthite is formed with other components in the green body and forms eutectic with other components in the green body, the sintering temperature of the green body is obviously reduced, meanwhile, calcite and limestone are decomposed at about 800 ℃ to form active CaO, and the active CaO and other active fine silicate particles form low eutectic, which is beneficial to CaO-MgO-Al2O3-SiO2The formation of the liquid phase promotes sintering, is beneficial to the formation and development of anorthite crystal nucleus in the calcium ion-rich liquid phase, and further improves the strength of the porcelain blank; the molten anorthite and the potassium-sodalite are mutually permeated to accelerate the generation of mullite, and are filled in gaps among mullite grains, so that the mechanical strength of a blank body is improved; the unmelted wollastonite fibers are connected among the particles to form a compact skeleton structure together with mullite, so that internal crack propagation is hindered when a blank is stressed, and R is2O-RO2-SiO2-Al2O3The system plays a role in toughening and reinforcing.
(2) The invention realizes the resource utilization of the wollastonite tailings, applies the wollastonite tailings to the production of building ceramics in a large amount and improves the added value of the tailings.
(3) The invention provides a production process of wollastonite tailing low-temperature ceramic tile, which is characterized in that the low-temperature ceramic tile is prepared at 1120-1150 ℃ on the basis of ensuring that the microstructure of residual wollastonite fibers is not damaged, and the mechanical strength and toughness (the breaking strength is more than 80MPa, and the fracture toughness is more than 3 MPa/m) of the ceramic tile are improved1/2) The method can be further expanded to the production technology of large-scale thin plates.
The present invention will be described in further detail with reference to examples.
Detailed Description
The first embodiment is as follows:
1. the embodiment provides a wollastonite tailing reinforcing and toughening low-temperature ceramic tile, which comprises the following raw materials: 3600g of wollastonite tailing sand, 2900g of low-temperature sand, 400g of medium-temperature sand, 1400g of quartz, 400g of calcined talc, 500g of magnesia clay, 500g of bentonite, 100g of bauxite and 100g of zircon sand.
Wherein, the mineral composition of the wollastonite tailings is as follows: 55 wt% of wollastonite, 23 wt% of calcite, 9 wt% of quartz, 6 wt% of diopside and 7 wt% of amorphous phase.
2. The preparation method of the wollastonite tailing reinforcing and toughening low-temperature porcelain comprises the following steps:
(1) adding 5150ml of water into the raw materials except for the wollastonite tailings, ball-milling and mixing for 25h to obtain slurry with the water content of 34.2%;
(2) adding wollastonite tailings, 15g of sodium tripolyphosphate and 30g of sodium carboxymethylcellulose, and continuously ball-milling and mixing for 3h to obtain slurry with the particle fineness D50 of 21.3 mu m;
(3) sieving the slurry to remove iron, drying and granulating to obtain powder;
(4) sieving the above powder, aging, compression molding to obtain green brick, and sintering in roller kiln at 1130 deg.CThe period is 70min, thus obtaining the wollastonite tailing reinforcing and toughening low-temperature ceramic tile, wherein the main crystalline phases of the wollastonite tailing reinforcing and toughening low-temperature ceramic tile are quartz, anorthite, mullite and wollastonite, and the chemical composition of the wollastonite tailing reinforcing and toughening low-temperature ceramic tile is SiO2 67.47％、Al2O3 7.44％、TiO2+Fe2O3 0.38％、CaO 17.05％、MgO 3.55％、K2O 1.25％、Na2O 2.1％、ZrO20.76％。
The wollastonite tailing reinforcing and toughening low-temperature ceramic tile prepared in the embodiment has the water absorption of 0.32 percent, the breaking strength of 83.5MPa, the firing shrinkage of 11.45 percent and the fracture toughness of 3.2MPa/m1/2。
Example two:
1. the embodiment provides a wollastonite tailing reinforcing and toughening low-temperature ceramic tile, which comprises the following raw materials: 4200g of wollastonite tailings, 2600g of low-temperature sand, 700 g of medium-temperature sand, 1000g of quartz, 400g of calcined talc, 250g of magnesia clay, 200g of bentonite, 200g of bauxite and 200g of zircon sand.
Wherein, the mineral composition of the wollastonite tailings is as follows: 59 wt% of wollastonite, 18 wt% of calcite, 8 wt% of quartz, 10 wt% of diopside and 5 wt% of amorphous phase.
2. The preparation method of the wollastonite tailing reinforcing and toughening low-temperature porcelain comprises the following steps:
(1) adding 5380ml of water into the raw materials except for the wollastonite tailings, ball-milling and mixing for 28h to obtain slurry with the water content of 35.5%;
(2) adding wollastonite tailings, 5g of sodium hexametaphosphate, 5g of sodium humate, 10g of sodium carboxymethylcellulose and 9.5g of polyvinyl alcohol, and continuously performing ball milling and mixing for 4 hours to obtain slurry with the particle fineness D50 of 19 microns;
(3) sieving the slurry to remove iron, drying and granulating to obtain powder;
(4) the powder is sieved, and then the brick blank obtained by ageing and compression molding is sent into a roller kiln to be sintered at the temperature of 1150 ℃ for 60min to obtain the wollastonite tailing reinforced and toughened low-temperature ceramic tile, the main crystalline phases of which are quartz, wollastonite, anorthite, diopside and mullite, and the chemical composition of which is SiO2 63.8％、Al2O3 7.85％、TiO2+Fe2O3 0.5％、CaO 19.78％、MgO 3.61％、K2O 1.2％、Na2O 1.90％、ZrO2 1.36％。
The wollastonite tailing reinforcing and toughening low-temperature ceramic tile prepared in the embodiment has the water absorption rate of 0.22 percent, the breaking strength of 80.3MPa, the firing shrinkage of 12.05 percent and the fracture toughness of 3.1MPa/m1/2。
Example three:
1. the embodiment provides a wollastonite tailing reinforcing and toughening low-temperature ceramic tile, which comprises the following raw materials: 4200g of wollastonite tailing sand, 3100g of low-temperature sand, 700 g of medium-temperature sand, 1000g of quartz, 400g of calcined talc, 500g of magnesia clay, 200g of bentonite, 200g of bauxite, 50g of zircon sand and 150g of borocalcite.
Wherein, the mineral composition of the wollastonite tailings is as follows: 63 wt% of wollastonite, 19 wt% of calcite, 4 wt% of quartz, 9 wt% of diopside and 4 wt% of amorphous phase.
2. The preparation method of the wollastonite tailing reinforcing and toughening low-temperature porcelain comprises the following steps:
(1) adding 5555ml of water into the raw materials except the wollastonite tailings, ball-milling and mixing for 28 hours to obtain slurry with the water content of 34.6%;
(2) adding wollastonite tailings, 5.3g of sodium metaphosphate pentahydrate, 6.2g of sodium humate and 31.5g of polyvinyl alcohol, and continuously performing ball milling and mixing for 5 hours to obtain slurry with the particle fineness D50 of 24 mu m;
(3) sieving the slurry to remove iron, drying and granulating to obtain powder;
(4) sieving the above powder, aging, compression molding to obtain green brick, and sintering in roller kiln at 1140 deg.C for 55min to obtain wollastonite tailing reinforced toughened low-temperature ceramic tile with main crystal phases of quartz, wollastonite, anorthite, diopside and SiO2 64.38％、Al2O3 8.3％、TiO2+Fe2O3 0.5％、CaO19.35％、MgO 3.49％、K2O 1.21％、Na2O 2.14％、B2O5 0.29％、ZrO2 0.34％。
The wollastonite tailing reinforcing and toughening low-temperature ceramic tile prepared in the embodiment has the water absorption of 0.25 percent, the breaking strength of 84.5MPa, the firing shrinkage of 12.9 percent and the fracture toughness of 3.2MPa/m1/2。

Claims (8)

1. The wollastonite tailing reinforcing and toughening low-temperature ceramic tile is characterized by comprising the following raw materials in parts by weight: 35-45 parts of wollastonite tailings, 18-32 parts of low-temperature sand, 2-7 parts of medium-temperature sand, 10-18 parts of quartz, 2-4 parts of talcum, 0-5 parts of magnesia clay, 2-5 parts of bentonite, 0.5-3 parts of bauxite, 0.5-2 parts of zircon sand and 0-3 parts of borocalcite; and sintering the ceramic at 1120-1150 deg.C.
2. The wollastonite tailings reinforced and toughened low-temperature ceramic tile as claimed in claim 1, wherein: the content of calcite in the wollastonite tailings is less than or equal to 24 wt%, and the content of quartz is less than or equal to 10 wt%.
3. The wollastonite tailings reinforced and toughened low-temperature ceramic tile as claimed in claim 2, wherein: the wollastonite tailing comprises the following minerals: 50-65 wt% of wollastonite, 18-24 wt% of calcite, 4-10 wt% of quartz, 5-10 wt% of diopside and 3-8 wt% of amorphous phase.
4. The wollastonite tailings reinforced and toughened low-temperature ceramic tile as claimed in claim 1, wherein: the main crystalline phases of the ceramic tile are four or five combinations of wollastonite, anorthite, diopside, mullite and quartz.
5. The wollastonite tailings reinforced and toughened low-temperature ceramic tile as claimed in claim 1, wherein: the chemical composition of the ceramic tile is SiO2 60～68％、Al2O3 6.5～8.5％、TiO2+Fe2O3 0.3～0.6％、CaO 16～21％、MgO 3.4～4.2％、K2O 1.2～2.5％、Na2O 1.4～3.2％、B2O5 0～0.4％、ZrO2 0.3～1.5％。
6. A preparation method of the wollastonite tailing reinforcing and toughening low-temperature ceramic tile as described in one of the claims 1 to 5 is characterized by comprising the following steps:
(1) ball-milling and mixing the materials except the wollastonite tailings in the raw materials by taking water as a medium to obtain slurry with the water content of 33.5-35.5%;
(2) adding wollastonite tailings, a ceramic dispergator and a forming agent, and continuously performing ball milling and mixing to obtain slurry with the particle fineness D50 of 18-25 mu m; the dosage of the ceramic debonder and the molding agent is 0.1-0.15 wt% and 0.2-0.4 wt% of the raw materials respectively;
(3) sieving the slurry to remove iron, drying and granulating to obtain powder;
(4) and (3) sieving the powder, ageing, carrying out compression molding to obtain a green brick, and firing at 1120-1150 ℃ to obtain the wollastonite tailing reinforcing and toughening low-temperature ceramic tile.
7. The preparation method of the wollastonite tailing reinforcing and toughening low-temperature ceramic tile according to claim 6, which is characterized in that: the ceramic debonder is one or two of sodium tripolyphosphate, sodium metasilicate pentahydrate, sodium hexametaphosphate and sodium humate; the forming agent is one or the combination of sodium carboxymethylcellulose, polyvinyl alcohol and chitosan.
8. The preparation method of the wollastonite tailing reinforcing and toughening low-temperature ceramic tile according to claim 6, which is characterized in that: the ball milling time in the step (1) is 20-29 h; the ball milling time in the step (2) is 3-5 h.
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