CN115304357A - Melilite/calcium aluminate two-phase material and preparation method thereof - Google Patents
Melilite/calcium aluminate two-phase material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a melilite/calcium aluminate two-phase material and a preparation method thereof, relating to the technical field of refractory materials, and the material comprises the following raw materials: 50-75 wt% of calcium aluminum slag, 0-8 wt% of limestone, 10-20 wt% of quartz sand, 2-5 wt% of industrial alumina, 1-10 wt% of clay and 1-10 wt% of additive, wherein the main crystal phase after high-temperature sintering is melilite Ca 2 Al 2 SiO 7 And calcium aluminate Ca 23.90 Al 27.88 O 65.58 . The traditional ceramic preparation process is improved, and compared with the calcium aluminate slag, the prepared porous material has the advantages of strong thermal stability, low expansion coefficient and the like, and can be used as an additive to be introduced into a refractory material to improve the sintering performance and the thermal shock stability of the refractory material.
Description
Technical Field
The invention relates to the technical field of refractory materials, in particular to a melilite/calcium aluminate two-phase material and a preparation method thereof.
Background
The refractory material is used as a homogeneous multiphase inorganic non-metallic material, has high refractoriness and excellent thermomechanical property, and is widely applied to high-temperature kilns and metallurgical industries. The production capacity of the refractory material in China is about 2477.49 ten thousand tons in 2020, and with the increase of the production cost and the environmental pollution caused by the excessive exploitation of mineral resources, the production process of the refractory material adopts industrial waste as a raw material to become a choice.
Melilite is a silicate mineral composed of aluminum, magnesium and iron silicate, and has a chemical formula of (Ca, na) 2 (Al,Mg,Fe)[(Al,Si)SiO 7 ]. Gehlenite (Ca) 2 Al(Al,Si)O 7 ) And akermanite (Ca) 2 MgSiO 7 ) Are two important compounds in melilite family. The melilite has the characteristics of low volume density, small thermal expansion coefficient and the like, although the melting point of the melilite is not high and can not be used as a main crystal phase of a refractory material, the melilite is introduced into the refractory material to be used as a second phase, so that the sintering property, the mechanical strength and the thermal shock stability of the material are improved.
The aluminum-calcium slag is mainly synthesized by aluminum ash and limestone at high temperature and is divided into sintering slag and melting slag. The aluminum ash is mainly derived from scrap generated in the production process of metallic aluminum, electrolytic aluminum smelting and aluminum alloy. In recent years, the aluminum industry in China is rapidly developed and becomes the main aluminum industry strong country in the world. The aluminum ash slag generated in the aluminum smelting process is industrial waste slag which has large yield and pollutes the environment. The industrial waste residues just discharged from the furnace contain high metallic aluminum, wherein only part of the metallic aluminum can be recovered, and the rest aluminum ash waste residues containing a small amount of metallic aluminum are accumulated in a factory or buried, so that not only is the resource waste caused, but also the environment is polluted.
Disclosure of Invention
Aiming at the technical problems, the invention overcomes the defects of the prior art and provides a melilite/calcium aluminate two-phase material, which comprises the following raw materials: 50-75 wt% of calcium aluminum slag, 0-8 wt% of limestone, 10-20 wt% of quartz sand, 2-5 wt% of industrial alumina, 1-10 wt% of clay and 1-10 wt% of additive, wherein the main crystal phase after high-temperature firing is melilite Ca 2 Al 2 SiO 7 And calcium aluminate Ca 23.90 Al 27.88 O 65.58 。
The technical scheme of the invention is further defined as follows:
the two-phase material of melilite/calcium aluminate has the grain size of the calcium aluminate slag of 3-1mm,1-0.5mm,0.5-0.088mm and less than 0.088mm.
The two-phase material of the melilite/calcium aluminate has evenly distributed pores, the apparent porosity is 25 to 32 percent, and the volume density is 1.5 to 2.0g/cm 3 。
The melilite/calcium aluminate two-phase material is prepared by adding at least one of a bonding agent and a release agent into an additive. .
The additive of the melilite/calcium aluminate two-phase material comprises a bonding agent and a release agent, wherein the bonding agent comprises at least one of polyvinyl alcohol and calcium lignosulfonate, and accounts for 3-8 wt% of the total weight of the raw materials; the release agent comprises at least one of paraffin and sodium stearate, and accounts for 0-1 wt% of the total weight of the raw materials.
The invention also aims to provide a preparation method of the melilite/calcium aluminate two-phase material, which comprises the following steps:
(1) Respectively weighing the raw materials of the calcium aluminum slag, the limestone, the quartz sand, the industrial alumina and the clay according to the mass percentage;
(2) Premixing the fine powder part in a ball mill for 2-6 hours to ensure that the granularity of the premixed powder is less than 350 meshes and the ratio is less than 20%;
(3) Stirring the coarse particles and the premixed powder in a powerful stirrer for 5-10 minutes, and then adding an additive to continuously mix for 10-60 minutes;
(4) Pressing and molding the uniformly mixed blank in a hydraulic press in a hydraulic molding mode;
(5) Drying the pressed and formed blank in a vacuum drying oven at the vacuum degree of less than 0.08Mpa at the drying temperature of 80-110 ℃ for 15-24 hours;
(6) And (3) placing the dried blank in an electric furnace, heating at 1200-1400 ℃ by adopting temperature gradient, keeping the temperature for 3-10 hours, and cooling along with the furnace to obtain the low-expansion porous melilite/calcium aluminate two-phase material.
The preparation method of the melilite/calcium aluminate two-phase material comprises the steps of (2) to (4), adding the additive, uniformly mixing, and forming the powder into a green body, wherein the addition amount of water is 1.5-10 wt%.
In the preparation method of the melilite/calcium aluminate two-phase material, in the step (4), the blank is kept under the pressure of 150-200 MPa for 10-100 s, and is pressed and formed to obtain a blank body with the size of 1363multiplied by 50mm H50 mm.
In the above-mentioned method for preparing melilite/calcium aluminate two-phase material, in the step (6), the temperature control system of the heat treatment is as follows: (1) the room temperature is between 1000 ℃, and the heating rate is between 5 and 10 ℃/min; (2) 1000 ℃ to the target temperature, the heating rate is 3 ℃/min, and the temperature is kept.
The invention has the beneficial effects that:
(1) The method for preparing the melilite/calcium aluminate composite material by taking the waste aluminum ash waste residues and the limestone as main raw materials can not only avoid the pollution of industrial waste materials to the ecological environment, but also reduce the production cost, change waste into valuable, recycle industrial raw materials and have important social significance and economic benefit;
(2) The invention has simple equipment, low cost and no special limitation on the molding of materials, and can make corresponding adjustment according to the specific equipment process;
(3) The invention adopts vacuum drying in the drying process of the green body formed by pressing, the vacuum degree is less than 0.08MPa, and the cracking of the material containing the aluminum-calcium slag due to the hydration of calcium oxide in the drying and curing processes is avoided;
(4) The main raw materials of the invention adopt industrial waste materials generated in the processes of smelting metallic aluminum and electrolytic aluminum and producing aluminum alloy, the traditional ceramic preparation process is improved, and the prepared porous material has the advantages of stronger thermal stability, low expansion coefficient and the like compared with the aluminum-calcium slag, and can also be used as an additive to be introduced into a refractory material to improve the sintering property and the thermal shock stability of the refractory material.
Drawings
Fig. 1 and 2 are XRD diffraction patterns of the melilite/calcium aluminate two-phase material.
Detailed Description
Example 1
The melilite/calcium aluminate two-phase material provided by the embodiment comprises the following raw materials: 68wt% of calcium aluminum slag (less than 0.088 mm), 2wt% of limestone, 19wt% of quartz sand, 1wt% of industrial alumina, 10wt% of clay and 5% of calcium lignosulfonate solution in total mass as a binding agent, and weighing according to the mass.
Premixing the fine powder part in a planetary ball mill for 3 hours;
stirring the coarse particles and the premixed powder in a powerful stirrer for 10 minutes, and then adding a binding agent calcium lignosulfonate for mixing for 1 hour;
pressing and molding the uniformly mixed blank in a hydraulic press in a hydraulic molding mode;
drying the pressed and formed blank in a vacuum drying oven at the vacuum degree of less than 0.08MPa and the drying temperature of 110 ℃ for 20 hours;
and (3) placing the dried blank in an electric furnace, heating by adopting temperature gradient, wherein the heat treatment temperature is 1200 ℃, 1300 ℃ and 1400 ℃, and the heat preservation time is 5 hours, and cooling along with the furnace to obtain the low-expansion porous ceramic.
By comparing the phase compositions at different firing temperatures, the phase compositions at 1200 ℃ are melilite, calcium aluminate and anorthite, and the phase compositions are melilite and calcium aluminate when the firing temperature is higher than 1300 ℃, and the mechanical properties of the material are improved along with the rise of the firing temperature.
Example 2
The two-phase melilite/calcium aluminate material provided by the embodiment comprises the following raw materials: 70wt% of calcium aluminum slag (< 0.088 mm), 2wt% of limestone, 17wt% of quartz sand, 1wt% of industrial alumina, 10wt% of clay, 3wt% of calcium lignosulfonate solution serving as a bonding agent and 1wt% of sodium stearate serving as a release agent, and weighing according to the mass.
Premixing the fine powder part in a planetary ball mill for 3 hours;
stirring the coarse particles and the premixed powder in a powerful stirrer for 10 minutes, then adding a binding agent calcium lignosulfonate and a release agent sodium stearate, and continuously mixing for 1 hour;
pressing and molding the uniformly mixed blank in a hydraulic press in a hydraulic molding mode;
drying the pressed and formed blank in a vacuum drying oven at the vacuum degree of less than 0.08Mpa and the drying temperature of 110 ℃ for 15 hours;
and (3) placing the dried blank in an electric furnace, heating by adopting temperature gradient, wherein the heat treatment temperature is 1200 ℃, 1300 ℃ and 1400 ℃, and the heat preservation time is 5 hours, and cooling along with the furnace to obtain the low-expansion porous ceramic.
FIG. 1 shows the X-ray diffraction patterns of low-expansion, porous ceramics after firing at different temperatures. The composition of the phase at the firing temperature of 1200 ℃ is melilite, calcium aluminate and calcium silicate, the composition of the phase at the firing temperature of 1300 ℃ and 1400 ℃ is melilite and calcium aluminate, the content of melilite after firing at 1300 ℃ is 59.5%, and the content of melilite after firing at 1400 ℃ is 76.6%. In consideration of the excellent thermal shock stability of melilite, 1400 ℃ is more suitable for the preparation of low-expansion, porous melilite/calcium aluminate materials.
Example 3
The melilite/calcium aluminate two-phase material provided by the embodiment comprises the following raw materials: 72 percent of calcium aluminum slag (less than 0.088 mm), 5 percent of limestone, 10 percent of quartz sand, 3 percent of industrial alumina, 10 percent of clay and 3 percent of calcium lignosulfonate in the total mass as a bonding agent are weighed according to the mass.
Premixing the fine powder part in a ball mill for 3 hours;
stirring the coarse particles and the premixed powder in a powerful stirrer for 10 minutes, and then adding a binding agent calcium lignosulfonate for mixing for 1 hour;
pressing and molding the uniformly mixed blank in a hydraulic press in a hydraulic molding mode;
drying the pressed and formed blank in a vacuum drying oven at the vacuum degree of less than 0.08MPa and the drying temperature of 110 ℃ for 18 hours;
induction heating the dried blank body, the heat treatment temperature is about 1400 ℃, and furnace cooling is carried out to obtain the low-expansion porous melilite/calcium aluminate composite material, wherein the melilite content is higher than 80%, and the volume density is 1.8g/cm 3 The apparent porosity was 30%.
Example 4
The melilite/calcium aluminate two-phase material provided by the embodiment comprises the following raw materials: 70wt% of calcium aluminum slag (less than 0.088 mm), 5wt% of limestone, 10wt% of quartz sand, 5wt% of industrial alumina, 10wt% of clay and 3wt% of calcium lignosulfonate in total mass as a binding agent, and weighing according to the mass.
Premixing the fine powder part in a ball mill for 3 hours;
stirring the coarse particles and the premixed powder in a powerful stirrer for 10 minutes, and then adding a binding agent calcium lignosulfonate for mixing for 1 hour;
pressing and molding the uniformly mixed blank in a hydraulic press in a hydraulic molding mode;
drying the pressed and formed blank in a vacuum drying oven at the vacuum degree of less than 0.08MPa and the drying temperature of 110 ℃ for 20 hours;
and (3) carrying out induction heating on the dried blank at the heat treatment temperature of about 1400 ℃, and cooling the blank along with the furnace to obtain the low-expansion porous melilite/calcium aluminate two-phase material, wherein the melilite content is higher than 92.5%. FIG. 2 is an X-ray diffraction pattern thereof, and the bulk density of the melilite/calcium aluminate two-phase material is 2.1g/cm 3 The apparent porosity was 26%.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (9)
1. Melilite/aluminic acidA calcium two-phase material characterized by: the raw materials comprise: 50-75 wt% of calcium aluminum slag, 0-8 wt% of limestone, 10-20 wt% of quartz sand, 2-5 wt% of industrial alumina, 1-10 wt% of clay and 1-10 wt% of additive, wherein the main crystal phase after high-temperature firing is melilite Ca 2 Al 2 SiO 7 And calcium aluminate Ca 23.90 Al 27.88 O 65.58 。
2. The melilite/calcium aluminate two-phase material as claimed in claim 1, wherein: the grain diameter of the aluminum-calcium slag comprises 3-1mm,1-0.5mm,0.5-0.088mm and less than 0.088mm.
3. The melilite/calcium aluminate two-phase material of claim 1, wherein: the two-phase material has evenly distributed pores, the apparent porosity is 25 to 32 percent, and the volume density is 1.5 to 2.0g/cm 3 。
4. The melilite/calcium aluminate two-phase material of claim 1, wherein: the additive is at least one of a bonding agent and a release agent.
5. The melilite/calcium aluminate two-phase material of claim 4, wherein: the additive comprises a bonding agent and a release agent, wherein the bonding agent comprises at least one of polyvinyl alcohol and calcium lignosulphonate, and accounts for 3-8 wt% of the total weight of the raw materials; the release agent comprises at least one of paraffin and sodium stearate, and accounts for 0-1 wt% of the total weight of the raw materials.
6. A preparation method of melilite/calcium aluminate two-phase material is characterized in that: application to any of claims 1-5, comprising the steps of:
(1) Respectively weighing raw materials of calcium aluminum slag, limestone, quartz sand, industrial alumina and clay according to mass percentage;
(2) Premixing the fine powder part in a ball mill for 2-6 hours to ensure that the granularity of the premixed powder is less than 350 meshes and the proportion is less than 20 percent;
(3) Stirring the coarse particles and the premixed powder in a powerful stirrer for 5-10 minutes, and then adding an additive to continuously mix for 10-60 minutes;
(4) Pressing and molding the uniformly mixed blank in a hydraulic press in a hydraulic molding mode;
(5) Drying the pressed and formed blank in a vacuum drying oven at the vacuum degree of less than 0.08Mpa at the drying temperature of 80-110 ℃ for 15-24 hours;
(6) And (3) placing the dried blank in an electric furnace, heating at 1200-1400 ℃ by adopting temperature gradient, keeping the temperature for 3-10 hours, and cooling along with the furnace to obtain the low-expansion porous melilite/calcium aluminate two-phase material.
7. The method for preparing melilite/calcium aluminate biphasic material according to claim 6, wherein: and (5) adding an additive between the steps (2) to (4), and uniformly mixing to form the powder into a green body, wherein the addition amount of water is 1.5-10 wt%.
8. The method for preparing melilite/calcium aluminate two-phase material as claimed in claim 6, wherein: in the step (4), the blank is kept under the pressure of 150-200 MPa for 10-100 s, and a blank body with the size of 50mm x H50mm is obtained through compression molding.
9. The method for preparing melilite/calcium aluminate two-phase material as claimed in claim 6, wherein: in the step (6), the temperature control system of the heat treatment is as follows: (1) the room temperature is between 1000 ℃, and the heating rate is between 5 and 10 ℃/min; (2) 1000 ℃ to the target temperature, the heating rate is 3 ℃/min, and the temperature is preserved.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141892A (en) * | 1995-02-15 | 1997-02-05 | 郭建华 | Formular of artificial kalzium slugs and technology thereof |
| CN1408886A (en) * | 2002-09-23 | 2003-04-09 | 郭建华 | Aluminum-calcium slag and its preparing method |
| CN103351166A (en) * | 2012-07-25 | 2013-10-16 | 田玉明 | Calcium hexaluminate/gehlenite diphase heat-insulation refractory material and preparation method thereof |
| US20180186651A1 (en) * | 2015-07-15 | 2018-07-05 | Kerneos | Process for manufacturing calcium aluminates |
| CN108950141A (en) * | 2018-07-10 | 2018-12-07 | 屯留县彬烨钙合金工贸有限公司 | A kind of steel-making preparation method of pro-molten refining slag |
| CN112607758A (en) * | 2020-12-18 | 2021-04-06 | 中南大学 | Method for preparing calcium aluminate by synergistic treatment of high-magnesium aluminum ash and fly ash |
-
2022
- 2022-08-18 CN CN202210990731.XA patent/CN115304357B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141892A (en) * | 1995-02-15 | 1997-02-05 | 郭建华 | Formular of artificial kalzium slugs and technology thereof |
| CN1408886A (en) * | 2002-09-23 | 2003-04-09 | 郭建华 | Aluminum-calcium slag and its preparing method |
| CN103351166A (en) * | 2012-07-25 | 2013-10-16 | 田玉明 | Calcium hexaluminate/gehlenite diphase heat-insulation refractory material and preparation method thereof |
| US20180186651A1 (en) * | 2015-07-15 | 2018-07-05 | Kerneos | Process for manufacturing calcium aluminates |
| CN108950141A (en) * | 2018-07-10 | 2018-12-07 | 屯留县彬烨钙合金工贸有限公司 | A kind of steel-making preparation method of pro-molten refining slag |
| CN112607758A (en) * | 2020-12-18 | 2021-04-06 | 中南大学 | Method for preparing calcium aluminate by synergistic treatment of high-magnesium aluminum ash and fly ash |
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