CN115304394A - Preparation method of self-foaming sintering-swelling ceramsite - Google Patents
Preparation method of self-foaming sintering-swelling ceramsite Download PDFInfo
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Abstract
The invention provides a preparation method of self-foaming sintering-expanding ceramsite, which is prepared by mixing, stirring, balling and firing 50-70% of copper tailings, 15-35% of fly ash, 5-20% of high-iron phase solid waste foaming agent and 3-5% of fluxing agent in percentage by weight in an inert atmosphere. The method provided by the invention synergistically utilizes the + 3-valent Fe compound in the red mud to prepare the in-situ self-foaming light ceramsite through pyrolysis reaction, greatly reduces the preparation temperature and improves the sintering expansion efficiency by improving the sintering atmosphere, has the characteristics of reducing the cost and carbon emission, further improves the consumption rate of iron-rich wastes such as red mud and iron slag, and realizes high-quality utilization of the iron-rich wastes.
Description
Technical Field
The invention belongs to the technical field of solid waste treatment and resource utilization, and particularly relates to a preparation method of self-foaming sintering-swelling ceramsite.
Background
The sintered and expanded ceramsite is an artificial aggregate which is prepared at high temperature, has light weight and high strength, generally has a spherical shape, has a honeycomb-shaped porous structure inside, has excellent properties such as low density, high cylinder pressure strength, high softening coefficient, good frost resistance and the like, and is widely applied to the fields of building heat insulation, light structural members, wastewater treatment, sound insulation barriers and the like. The sintered and expanded ceramsite is used as the coarse aggregate and applied to the concrete, and has the advantages of greatly reducing the self weight of a concrete structure, reducing the section size and reducing the treatment cost of a foundation and a foundation.
The chemical composition of the raw material of the traditional ceramsite is mainly SiO 2 、Al 2 O 3 、Fe 2 O 3 And CaO, and the like, and natural minerals such as clay and shale are commonly used as main raw materials. Wherein SiO of the clay 2 High content and sufficient Al content 2 O 3 And fluxing agent, thereby becoming a more ideal raw material of the sintered ceramic particles. Currently, due to the restriction of environmental protection, shortage of natural resources, limited exploitation and other factors, the search for resources capable of replacing natural ceramsite raw materials is urgently needed.
The long-term development of the industry and mining industry in China accumulates that a large amount of tailing solid wastes are urgently needed to be treated, on the other hand, the tailings are potential renewable resources from the aspects of physical and chemical properties, and the development of tailing resource comprehensive utilization technology and related products is urgently needed at present to relieve the resource and environmental pressure. The ceramsite aggregate has large consumption in engineering application and has the potential of largely absorbing solid wastes. Therefore, the method for preparing the sintered ceramsite by partially or completely replacing the traditional natural minerals with the solid wastes such as the tailings and the like is an effective way for effectively solving the problems of tailing stockpiling and natural resource consumption.
Disclosure of Invention
The invention provides a preparation method of self-foaming sintering-expansion ceramsite for solving the technical problems. The method improves the consumption rate of red mud, solid waste and the like, and realizes high-quality utilization of iron-rich waste.
In order to achieve the purpose, the invention adopts the technical scheme that:
the self-foaming sintered ceramic grain is produced with copper tailings 50-70 wt%, flyash 15-35 wt%, high iron phase foaming agent 5-20 wt% and flux 3-5 wt%, and through mixing, pelletizing and sintering in inert atmosphere.
Preferably, the balling step specifically comprises: and putting the dry materials obtained by mixing and stirring into a disc granulator, spraying a proper amount of tap water, granulating into balls to obtain the material balls, wherein the particle size of the material balls is controlled to be 6-12 mm.
Preferably, the method further comprises the step of ageing and drying the pellets obtained in the pelletizing step before firing in an inert atmosphere.
Preferably, the specific steps of firing under an inert atmosphere are: placing the pellets in an atmosphere furnace, vacuumizing, introducing inert gas to control the pressure in the furnace to be 1 atmosphere, firstly raising the temperature from 25 ℃ to 900 ℃, preserving the heat for 10-15 min, then continuing raising the temperature to 1050-1100 ℃, preserving the heat for 30-60 min, and then cooling along with the furnace to obtain the sintering-expanding ceramsite.
Preferably, the rate of temperature rise is 8 to 12/min.
Preferably, the inert atmosphere is nitrogen or argon.
Preferably, the fluxing agent is one or a mixture of more than two of sodium silicate, sodium carbonate, albite or sodium hydroxide.
Preferably, the high-iron solid waste is red mud, fe 2 O 3 The content is not less than 30wt%, and the main iron-containing mineral is hematite.
Preferably, the copper tailings are bulk solid waste generated by copper ore beneficiation, and SiO in the copper tailings 2 More than 60wt% and less than 80wt%, al 2 O 3 The content is more than 10wt%.
Preferably, the raw material of the self-foaming sintered and expanded ceramsite comprises the following oxides in percentage by mass: siO 2 2 ：45～65％，Al 2 O 3 ：18～28％，K 2 O+Na 2 O+CaO+MgO：9～15％，Fe 2 O 3 ：5～12％。
The foaming principle of the invention is as follows: the invention adopts the red mud as the high-temperature in-situ foaming agent, and the compound of the Fe with the valence of 3 in the red mud can be decomposed to generate gas at the temperature far lower than the theoretical decomposition temperature in the inert atmosphere in the high-temperature process, so that the sintering temperature is greatly reduced. The copper tailings have high content of silicon oxide, and react with a fluxing agent at high temperature to generate a liquid phase with appropriate viscosity, the liquid phase can seal gas released under the high-temperature reaction in a melt, and the generated gas forms a plurality of independent spaces in the liquid phase to finally generate a uniform pore structure, so that the ceramsite can expand. The fly ash of the invention contains almost no carbon, and mainly provides alumina, thereby providing support for the strength of ceramsite.
The reaction equation of the red mud as the foaming agent is as follows:
Fe 2 O 3 (hematlte)→FeO n +O 2 ↑
6Fe 2 O 3 (s)＝4Fe 3 O 4 (s)+O 2 ↑
2Fe 3 O 4 (s)＝6FeO(l)+O 2 ↑
compared with the prior art, the invention has the beneficial effects that:
1) The method provided by the invention synergistically utilizes the pyrolysis reaction of the + 3-valent Fe compound in the red mud to prepare the in-situ self-foaming light ceramsite, greatly reduces the preparation temperature and improves the sintering expansion efficiency by improving the sintering atmosphere, has the characteristics of reducing the cost and carbon emission, further improves the consumption rate of iron-rich wastes such as red mud and iron slag, and realizes the high-quality utilization of the iron-rich wastes;
2) The invention utilizes the large-dosage copper tailings to prepare the light ceramsite, searches for the proper raw material proportion of the copper tailing ceramsite, optimizes the firing process, greatly improves the copper tailing absorption rate, reduces the exploitation of natural high-quality resources, enlarges the usable raw material range for the ceramsite production industry, and fully excavates the potential social, economic and environmental benefits of the copper tailings;
3) The preparation method of the invention synergistically utilizes solid waste, and the utilization rate can reach more than 95%;
4) The invention has low cost, simple preparation process, mature production equipment, suitability for large-scale popularization and application and good application prospect;
5) The sintered and expanded ceramsite prepared by the method has the bulk density of 0.47-0.73 g/cm 3 And the apparent density is 0.84-1.40 g/cm 3 The single particle strength is 4.28-13.15 MPa, the cylinder pressure strength is 2.69-6.32MPa, the water absorption rate in 1 hour is 0.89-1.54%, the water absorption rate in 24 hours is 2.05-2.96%, and the physical properties meet GB/T17431.1 2010 lightweight aggregate and test method part 1 thereof: the stipulation of light aggregate in light aggregate can be used for preparing light aggregate concrete with excellent performances in various aspects such as light weight, high strength and the like. The sintered and expanded ceramsite provides a certain technical reference for the further development of the building material industry towards light weight and high reinforcement, and provides a feasible route for the green development of the building engineering, the industrial metallurgical engineering and the material industry under the double-carbon strategy.
Drawings
FIG. 1 is a diagram of the calcination process of ceramsite. The firing process adopts a two-step firing method, and the firing process stays for 10 minutes at 900 ℃, so that the full reaction of some minerals in the ceramsite is facilitated.
FIG. 2 is an XRD pattern of the ceramsite under different sintering atmospheres. After sintering in inert atmosphere, the hematite phase in the red mud is completely converted into a spinel phase and a pyroxene phase, namely, the + 3-valent iron is completely converted into + 2-valent iron, which indicates that the decomposition reaction of the + 3-valent iron is fully carried out, and more gas is generated. After air sintering, most of the hematite in red mud still exists as hematite phase, and the +3 iron is not completely decomposed.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the following examples, the inert gas used in the sintering process was high purity nitrogen gas with a purity of 99.999% and an oxygen content of less than 3ppm.
In the following examples, the copper tailings used were bulk solid waste from copper ore beneficiation. In the invention, siO in the copper tailings 2 72.1wt% of Al 2 O 3 The content was 10.5wt%.
In the following examples, the fly ash used was grade I low carbon fly ash provided by Steheng Water purification Material works, and the specific surface area was 2036m 2 /kg，SiO 2 Content 52.4wt%, al 2 O 3 The content was 35.6wt%, the CaO content was 2.1wt%, and the loss on ignition was 2.18% and contains very little unburned carbon.
In the following examples, red mud is an effluent product of alumina extraction industry, wherein Fe 2 O 3 The content is 42.7wt%, and the main iron-containing mineral is hematite.
In the following examples, the flux used was anhydrous sodium metasilicate, which is produced by chemical reagents of the national drug group, llc.
In the following examples, the particle sizes of the copper tailings, the fly ash and the red mud are all below 80 meshes, and the chemical components are shown in table 1.
It is to be understood that the particular raw material compositions described herein are illustrative only and are not limiting upon the invention, as various changes (including raw material origin) can be made within the scope of the invention as defined in the appended claims.
Table 1 main chemical composition (wt.%) of copper tailings, fly ash and red mud
| SiO 2 | Al 2 O 3 | Fe 2 O 3 | CaO | MgO | K 2 O | Na 2 O | TiO2 | LOI | Others | |
| Copper tailings | 72.07 | 10.46 | 3.45 | 2.93 | 0.87 | 5.33 | 0.27 | 0.27 | 1.64 | 2.71 |
| Red mud | 9.93 | 21.75 | 42.67 | 1.44 | 0.14 | 0.08 | 6.63 | 5.84 | 10.39 | 1.13 |
| Fly ash | 52.37 | 35.55 | 2.79 | 2.13 | 0.64 | 1.27 | 0.66 | 1.32 | 2.18 | 1.09 |
Example 1
The embodiment provides a preparation method of self-foaming sintering-swelling ceramsite, which comprises the following steps:
(1) Mixing copper tailings, fly ash, red mud and fluxing agent according to the weight ratio of 50:30:15:5, then putting the mixture into a mixer to be stirred for 10 to 15 minutes to obtain dry materials which are uniformly mixed; the chemical composition of the raw material is as follows: siO 2 2 ：57.44％，Al 2 O 3 ：19.76，Fe 2 O 3 ：9.24，CaO：2.39，MgO：0.67，K 2 O：3.15，Na 2 O:3.99, others: 3.36.
(2) Putting the uniformly mixed dry materials into a disc granulator (the rotating speed is 45 r/min), spraying a proper amount of tap water to granulate into balls, and controlling the particle size to be 6-12 mm;
(3) Naturally stacking the material balls at room temperature for 24 hours for aging;
(4) Drying the pellets in a drying oven at 105 ℃ for 8h;
(5) And placing the dried pellets in an atmosphere furnace, vacuumizing, introducing inert gas to control the pressure in the furnace to be 1 atmosphere, raising the temperature from 25 ℃ to 900 ℃ at the speed of 10 ℃/min, preserving the heat for 10min, continuing raising the temperature to 1080 ℃ at the speed of 10 ℃/min, preserving the heat for 60min, and cooling along with the furnace to obtain the self-foaming sintering-swelling ceramsite.
The bulk density of the obtained self-foaming sintered and expanded ceramsite is 0.51g/cm 3 Apparent density of 0.89g/cm 3 The water absorption rate is 0.94% for 1 hour, the water absorption rate is 2.17% for 24 hours, the single-particle strength of the ceramsite is 6.14-9.62 MPa, and the cylinder pressure strength is 4.47MPa.
Example 2
This example is substantially the same as example 1 except for the difference in step (1):
(1) Mixing copper tailings, fly ash, red mud and fluxing agent according to the weight ratio of 50:35:10:5, then putting the mixture into a mixer to be stirred for 10 to 15 minutes to obtain dry materials which are uniformly mixed; the chemical composition of the raw material is as follows: siO 2 2 ：59.37％，Al 2 O 3 ：20.38，Fe 2 O 3 ：7.16，CaO：2.42，MgO：0.69，K 2 O：3.20，Na 2 O:3.67, others: 3.11.
the bulk density of the obtained self-foaming sintered and expanded ceramsite is 0.62g/cm 3 Apparent density of 1.08g/cm 3 1.22 percent of water absorption rate after 1 hour, 2.43 percent of water absorption rate after 24 hours, 7.43 to 11.45MPa of single-particle strength of the ceramsite, and 5.52MPa of cylinder pressure strength. Compared with the embodiment 1, the red mud mixing amount is reduced, the expansion effect of the ceramsite is slightly poor, and the strength is improved. The strength is slightly higher because the foaming effect is poor and the pores formed inside the ceramsite are not large.
Example 3
This example is substantially the same as example 1 except for the difference in step (5):
(5) And placing the dried material balls in an atmosphere furnace, vacuumizing, introducing inert gas to control the pressure in the furnace to be 1 atmosphere, raising the temperature from 25 ℃ to 900 ℃ at the speed of 10 ℃/min, preserving the heat for 10min, continuing raising the temperature to 1050 ℃ at the speed of 10 ℃/min, preserving the heat for 60min, and cooling along with the furnace.
The bulk density of the obtained self-foaming sintered and expanded ceramsite is 0.73g/cm 3 Apparent density of 1.40g/cm 3 1.54 percent of water absorption rate after 1 hour, 2.96 percent of water absorption rate after 24 hours, 8.21-13.15 MPa of single-particle strength of the ceramsite, and 6.32MPa of cylinder pressure strength. Compared with the embodiment 1, the sintering temperature is low, the expansion effect of the ceramsite is relatively poor, and the strength is higher.
Example 4
This example is substantially the same as example 1 except for the difference in step (5):
(5) And (3) placing the dried material balls in an atmosphere furnace, vacuumizing, introducing inert gas to control the pressure in the furnace to be 1 atmospheric pressure, heating to 900 ℃ from 25 ℃ at the speed of 10 ℃/min, preserving the heat for 10min, then continuously heating to 1100 ℃ at the speed of 10 ℃/min, preserving the heat for 60min, and cooling along with the furnace.
The bulk density of the obtained self-foaming sintered and expanded ceramsite is 0.47g/cm 3 Apparent density of 0.84g/cm 3 The water absorption rate of the sintered ceramsite is 0.89% in 1 hour, the water absorption rate of the sintered ceramsite is 2.05% in 24 hours, the single-particle strength of the sintered ceramsite is 4.28-7.16 MPa, and the cylinder pressure strength of the sintered ceramsite is 2.69 MPa. Compared with the embodiment 1, the sintering temperature is higher, the ceramsite expansion effect is good, and the strength is low.
Comparative example 1
This comparative example is substantially the same as example 1 except for the difference in step (1):
(1) Mixing copper tailings, fly ash, red mud and fluxing agent according to the weight ratio of 50:45:0:5 (excluding red mud), and then putting the mixture into a mixer to be stirred for 10 to 15 minutes to obtain a dry material which is uniformly mixed.
The bulk density of the obtained sintered and expanded ceramsite is 1.03g/cm 3 Apparent density 2.09g/cm 3 The water absorption rate for 1 hour is 1.74 percent, the water absorption rate for 24 hours is 3.66 percent, the single-particle strength of the ceramsite is 10.77-18.61 MPa, and the cylinder pressure strength is 7.43MPa. Compared with the ceramsite prepared in the embodiment 1 without the red mud as a foaming agent, the ceramsite has no expansion effect and is in a sintering shrinkage state.
Comparative example 2
This comparative example is substantially the same as example 1 except for the difference in step (1):
(1) Mixing copper tailings, fly ash, pyrite and fluxing agent according to the weight ratio of 50:30:15:5, and then putting the mixture into a mixer to be stirred for 10 to 15 minutes to obtain a dry material which is uniformly mixed.
Pyrite (FeS) containing predominantly +2 valent iron compared to that used in example 1 2 97.4 wt%) as foaming agent, the ceramsite has no expansion effect and is in a sintered state.
Comparative example 3
This comparative example is substantially the same as example 1 except for the difference in step (5):
(5) And (3) placing the dried material balls in an atmosphere furnace, not introducing nitrogen, heating to 900 ℃ from 25 ℃ at the temperature of 10 ℃ for min under the atmosphere of/air, preserving the heat for 10min, then continuously heating to 1200 ℃ at the temperature of 10 ℃/min, preserving the heat for 60min, and cooling along with the furnace to obtain the material balls.
The obtained sintered and expanded ceramsite has the bulk density of 0.58g/cm 3 Apparent density of 0.97g/cm 3 The water absorption rate for 1 hour is 1.76 percent, the water absorption rate for 24 hours is 3.13 percent, the single-particle strength of the ceramsite is 7.05-11.05 MPa, and the cylinder pressure strength is 5.16MPa. It can be seen that the ceramsite in this comparative example was fired in an air atmosphere, the expansion effect was slightly inferior to that of the ceramsite in example 1, and the sintering temperature required for the preparation was higher.
Comparative example 4
This comparative example is substantially the same as example 1 except for the difference in step (5):
(5) Placing the dried material balls in an atmosphere furnace, heating from 25 ℃ to 900 ℃ at 10 ℃ for min under the air atmosphere without introducing nitrogen, preserving heat for 10min, then continuously heating to 1080 ℃ at 10 ℃/min, preserving heat for 60min, and cooling along with the furnace. The ceramsite in this comparative example was fired in an air atmosphere at a temperature at which red mud could not decompose gas, and the ceramsite was sintered at the same temperature as the ceramsite in example 1, without expansion effect, and in a sintering shrinkage state.
The above embodiments are merely examples for clearly illustrating the present invention and do not limit the present invention. Other variants and modifications of the invention, which are obvious to those skilled in the art and can be made on the basis of the above description, are not necessary or exhaustive for all embodiments, and are therefore within the scope of the invention.
Claims (10)
1. The self-foaming sintered and expanded ceramsite is characterized by being prepared by mixing, stirring, balling and firing 50-70 wt% of copper tailings, 15-35 wt% of fly ash, 5-20 wt% of high-iron phase solid waste foaming agent and 3-5 wt% of fluxing agent.
2. The method of claim 1, wherein the balling step specifically comprises: and putting the dry materials obtained by mixing and stirring into a disc granulator, spraying a proper amount of tap water, granulating into balls to obtain the material balls, wherein the particle size of the material balls is controlled to be 6-12 mm.
3. The method of claim 1, further comprising the step of aging and drying the pellets obtained in the pelletizing step before firing in an inert atmosphere.
4. The method of claim 1, wherein the firing under an inert atmosphere comprises the following specific steps: placing the pellets in an atmosphere furnace, vacuumizing, introducing inert gas to control the pressure in the furnace to be 1 atmosphere, raising the temperature from 25 ℃ to 900 ℃, preserving the heat for 10-15 min, then continuing raising the temperature to 1050-1100 ℃, preserving the heat for 30-60 min, and then cooling along with the furnace to obtain the sintering expansion ceramsite.
5. The method according to claim 4, wherein the rate of temperature rise is 8 to 12/min.
6. The method of claim 1, wherein the inert atmosphere is nitrogen or argon.
7. The method according to claim 1, wherein the flux is one or a mixture of two or more of sodium silicate, sodium carbonate, albite, and sodium hydroxide.
8. The preparation method according to claim 1, wherein the high-iron solid waste is red mud, fe 2 O 3 The content is not less than 30wt%, and the main iron-containing mineral is hematite.
9. The preparation method according to claim 1, wherein the copper tailings are bulk solid waste generated by copper ore beneficiation, and SiO in the copper tailings 2 More than 60wt% and less than 80wt%, al 2 O 3 The content is more than 10wt%.
10. The method of claim 1, wherein the self-foaming sintered ceramic is a ceramicThe mass percentage of each oxide in the raw material of the particles is as follows: siO 2 2 ：45～65％，Al 2 O 3 ：18～28％，K 2 O+Na 2 O+CaO+MgO：9～15％，Fe 2 O 3 ：5～12％。
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| CN101538131A (en) * | 2009-04-14 | 2009-09-23 | 桂林工学院 | Method for preparing sintering-expanded haydite by taking red mud of Bayer process as main raw material |
| CN105669157A (en) * | 2016-03-05 | 2016-06-15 | 成都育芽科技有限公司 | Preparation method of copper mine tailing haydite for landscaping |
| CN107324774A (en) * | 2017-08-18 | 2017-11-07 | 江苏省冶金设计院有限公司 | It is a kind of to improve the apparatus system that red mud porcelain granule burns swollen rate |
| CN115093242A (en) * | 2022-07-01 | 2022-09-23 | 陈松靖 | High-strength copper tailing ceramsite and preparation method thereof |
| CN115141034A (en) * | 2021-03-31 | 2022-10-04 | 广东清大同科环保技术有限公司 | Red mud sintered aggregate |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538131A (en) * | 2009-04-14 | 2009-09-23 | 桂林工学院 | Method for preparing sintering-expanded haydite by taking red mud of Bayer process as main raw material |
| CN105669157A (en) * | 2016-03-05 | 2016-06-15 | 成都育芽科技有限公司 | Preparation method of copper mine tailing haydite for landscaping |
| CN107324774A (en) * | 2017-08-18 | 2017-11-07 | 江苏省冶金设计院有限公司 | It is a kind of to improve the apparatus system that red mud porcelain granule burns swollen rate |
| CN115141034A (en) * | 2021-03-31 | 2022-10-04 | 广东清大同科环保技术有限公司 | Red mud sintered aggregate |
| CN115093242A (en) * | 2022-07-01 | 2022-09-23 | 陈松靖 | High-strength copper tailing ceramsite and preparation method thereof |
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