CN114229891B - Device for preparing crystals through pyrolysis and magnetic separation and method for preparing zirconium oxide by using device - Google Patents
Device for preparing crystals through pyrolysis and magnetic separation and method for preparing zirconium oxide by using device Download PDFInfo
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- CN114229891B CN114229891B CN202111560213.6A CN202111560213A CN114229891B CN 114229891 B CN114229891 B CN 114229891B CN 202111560213 A CN202111560213 A CN 202111560213A CN 114229891 B CN114229891 B CN 114229891B
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- 238000000197 pyrolysis Methods 0.000 title claims abstract description 151
- 238000000034 method Methods 0.000 title claims abstract description 58
- 238000007885 magnetic separation Methods 0.000 title claims abstract description 45
- 239000013078 crystal Substances 0.000 title claims abstract description 26
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title description 27
- 229910001928 zirconium oxide Inorganic materials 0.000 title description 5
- 230000005484 gravity Effects 0.000 claims abstract description 134
- 238000000926 separation method Methods 0.000 claims abstract description 94
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000498 cooling water Substances 0.000 claims abstract description 42
- 238000007599 discharging Methods 0.000 claims abstract description 33
- 230000008569 process Effects 0.000 claims abstract description 27
- 239000000654 additive Substances 0.000 claims abstract description 21
- 230000000996 additive effect Effects 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000012141 concentrate Substances 0.000 claims description 98
- 230000005291 magnetic effect Effects 0.000 claims description 73
- 238000001816 cooling Methods 0.000 claims description 33
- 238000003860 storage Methods 0.000 claims description 27
- 239000004576 sand Substances 0.000 claims description 24
- 229910052845 zircon Inorganic materials 0.000 claims description 23
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 21
- 239000006148 magnetic separator Substances 0.000 claims description 20
- 239000007921 spray Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 239000011819 refractory material Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 103
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 38
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 8
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 8
- 238000005469 granulation Methods 0.000 description 7
- 230000003179 granulation Effects 0.000 description 7
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 239000000292 calcium oxide Substances 0.000 description 6
- 238000003723 Smelting Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000010891 electric arc Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000002006 petroleum coke Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 241001584775 Tunga penetrans Species 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
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- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
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- 230000007704 transition Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a device for preparing crystals by pyrolysis and magnetic separation, which comprises a pyrolysis furnace, a discharging system, a gravity separation system and a magnetic separation system. Wherein, the discharging system comprises a cooling water tower, a cooling water circulating pump, a granulating tank and a scraper discharging machine. The granulating tank is provided with circulating cooling water, so that the granulating temperature can be ensured to be stable within a reasonable range, and the water consumption of the process is reduced. The scraper blade discharging machine comprises a horizontal section and an inclined section, wherein the horizontal section is embedded in the granulating groove, has a good stirring effect on granulated products, can improve granulating efficiency, and improves the granularity range width of the products. The invention also provides a method for preparing crystals by using the device, taking zirconia as an example, pyrolysis additive is added into a pyrolysis furnace in the pyrolysis process, so that pyrolysis can be performed at a lower temperature, such as 1300-1900 ℃, the selection range of refractory materials of the pyrolysis furnace is widened, the service life of the pyrolysis furnace is prolonged, and the energy consumption in the pyrolysis process is reduced.
Description
Technical Field
The invention relates to the technical field of crystal preparation, in particular to a device for preparing crystals by pyrolysis and magnetic separation and a method for preparing zirconium oxide by using the device.
Background
Zirconium dioxide is a main oxide of zirconium, has the excellent characteristics of high wear resistance, high melting point, corrosion resistance, non-conduction, non-magnetic conduction and the like, has low thermal expansion coefficient, high refractive index and good thermal shock resistance, and is an important and emerging material in the fields of high temperature resistant materials, structural ceramics, functional ceramics and the like. The existing preparation methods of zirconia mainly comprise a chemical method and an electric melting method, wherein the high-purity zirconia produced by the chemical method has excellent performance, but the production process is difficult to treat in an environment-friendly way due to long process flow and large reagent consumption, and the production cost is high.
The electrofused zirconia is prepared by using the principle of reducing silicon dioxide in zircon sand by carbon, and removing silicon from the zircon sand by controlling the reduction carbon amount and the catalyst amount under the high temperature condition of 2500-3000 ℃ by means of an electric arc furnace. The characteristics of the zirconium dioxide products obtained by production are different, and can be classified into desilication zirconium dioxide and stable zirconium dioxide. The process for preparing the stable zirconium dioxide by the electric melting method can be divided into a primary electric melting method and a secondary electric melting method according to different raw materials, and the process for producing the stable zirconium dioxide by adopting zircon sand as the raw material is the primary electric melting method; the process for producing stable zirconium dioxide by adopting desilication zirconium dioxide as a raw material is a secondary electrofusion method.
Adding appropriate amount of reducer petroleum coke into electric furnace, and decomposing zircon sand into ZrO under the action of arc heat 2 And SiO 2 ，SiO 2 React with carbon in petroleum coke to generate gaseous SiO, the gaseous SiO is discharged along with flue gas under the action of the pumping force of a fan, and the gaseous SiO is oxidized into amorphous SiO after being discharged from a furnace by air 2 . SiO in the furnace 2 And pouring the zirconia melt in a molten state out of the furnace after the zirconia melt is removed, and performing blowing granulation. There are two main methods for granulating fused zirconia: one is a jet method, i.e., a high pressure gas is used to spray zirconia melt into particles; the other is a water spraying method, which utilizes the principle that the high-temperature fused zirconia can burst when being quenched by water, and the high-temperature fused zirconia is cooled and granulated by directly contacting the high-temperature fused zirconia with water flow, thus obtaining the desilication fused zirconia balls.
When the electric arc furnace is adopted to produce desilication zirconia according to the main chemical reaction, the main components of the electric arc furnace smoke are carbon dioxide and gaseous SiO, and CO is discharged to the atmosphere every 1t of desilication zirconia is produced 2 About 250kg. The smelting reaction is carried out at the high temperature of 2500-3000 ℃, the heat loss of the furnace shell is large, the comprehensive power consumption of 1t of zirconia is about 6500-9000 kw.h, and the production energy consumption is high.
It is therefore desirable to optimize the zirconia production apparatus and production process, such as to reduce pyrolysis temperatures, control carbon emissions during production, and increase the specific gravity of the silica fines in the product.
In view of this, the present invention has been made.
Disclosure of Invention
The first object of the invention is to provide a device for preparing crystals by pyrolysis and magnetic separation, which can realize pyrolysis of raw zircon sand and granulation of pyrolysis melt, and then sequentially perform reselection and magnetic separation on pyrolysis products to obtain monoclinic desilication zirconium dioxide products with higher purity and silicon dioxide products with larger volume weight.
A second object of the present invention is to provide a method for preparing zirconia, in particular monoclinic zirconia, using the apparatus.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the invention relates to a device for preparing crystals by pyrolysis and magnetic separation, which comprises a pyrolysis furnace, a discharging system, a gravity separation system and a magnetic separation system, wherein,
the pyrolysis furnace is used for heating and decomposing the raw materials to obtain pyrolysis products;
the discharging system is used for outputting and cooling the pyrolysis product to obtain a cooled product, and inputting the cooled product into the reselection system;
the gravity separation system is used for carrying out gravity separation on the cooling product to obtain gravity separation tailings and gravity separation concentrate;
the magnetic separation system is used for removing magnetic matters in the gravity concentrate to obtain magnetic concentrate, namely a single crystal target product.
Preferably, the discharging system comprises a cooling water tower, a cooling water circulating pump, a granulating tank and a scraper discharging machine, wherein,
the granulating tank is used for cooling pyrolysis products output from the pyrolysis furnace to obtain cooling products, a spray water pipe is arranged in the granulating tank, a water outlet of the cooling water tower is connected with a water inlet of the spray water pipe through a pipeline, water is sprayed into the granulating tank by the spray water pipe, a water outlet is arranged on the side face of the granulating tank, a water outlet of the granulating tank is connected with a water inlet of the cooling water tower through a pipeline, and the cooling water circulating pump is positioned on a connecting pipeline of the spray water pipe and the cooling water tower;
the scraper discharging machine is used for outputting the cooling product from the granulating tank, stirring the cooling product to uniformly mix the cooling product, the scraper discharging machine comprises a horizontal section and an inclined section which are integrally formed, the horizontal section is embedded in the granulating tank, the inclined section extends to a direction away from the granulating tank, and the material output end of the inclined section is connected with a feed inlet of the gravity separation system.
Preferably, the gravity separation system comprises a gravity separation device, a gravity separation tailings reservoir, a gravity separation concentrate reservoir and a gravity separation concentrate delivery pump, wherein,
the gravity separation equipment is used for carrying out gravity separation on the cooled product to obtain gravity separation tailings and gravity separation concentrate, the gravity separation equipment is provided with a gravity separation tailings discharge port and a gravity separation concentrate discharge port, the gravity separation tailings discharge port is connected with the feed inlet of the gravity separation tailings storage tank, the gravity separation concentrate discharge port is connected with the feed inlet of the gravity separation concentrate storage tank,
the discharge gate of gravity concentrate storage tank with the feed inlet of magnetic separation system is connected, gravity concentrate delivery pump is located gravity concentrate storage tank with the connecting line of magnetic separation system.
Preferably, the magnetic separation system comprises a magnetic separator, a magnetic concentrate product bin and a magnetic product bin, wherein,
the magnetic separator is used for carrying out magnetic separation on the gravity concentrate to obtain magnetic concentrate and magnetic matters, a magnetic concentrate discharge port and a magnetic matter discharge port are arranged on the magnetic separator, the magnetic concentrate discharge port is connected with a feed port of a magnetic concentrate product bin, and the magnetic matter discharge port is connected with a feed port of the magnetic matter product bin.
The invention also relates to a method for preparing crystals by using the device, taking zirconium oxide as an example, comprising the following steps:
step one, adding raw materials and pyrolysis additives into a pyrolysis furnace, and heating and decomposing to obtain pyrolysis products;
preferably, the feedstock is zircon sand, wherein ZrO 2 The mass percentage of the water content is 55.0-66.0%, and the water content is less than or equal to 1%.
Preferably, the pyrolysis additive is alkaline earth metal oxide, and is at least one selected from CaO and MgO. The addition amount of the pyrolysis additive is 5-15% of the mass of the zircon sand raw material by taking the mass of the zircon sand as 100%.
Preferably, the pyrolysis temperature is 1300-1900 ℃, the pyrolysis time is 45-120 minutes, and the pyrolysis process is carried out in a natural furnace gas atmosphere.
Step two, starting a cooling water circulating pump after pyrolysis is finished, pouring pyrolysis products in the pyrolysis furnace into a granulating tank, and cooling the pyrolysis products to obtain cooled products;
preferably, the flow rate of the cooling water output by the cooling water circulating pump is 40-100 times of the mass flow rate of the pyrolysis product. The mass flow of the pyrolysis product is 30-500 kg/min, and the flow rate of cooling water is 5-10 m/s. The temperature of circulating water provided by the cooling water tower is less than or equal to 45 ℃.
Step three, starting a scraper discharging machine, and inputting cooling products in the granulating tank into the reselection equipment;
preferably, the motor operating frequency of the scraper discharging machine is 20-50 Hz.
The gravity separation equipment performs gravity separation on the cooled product to obtain gravity separation tailings and gravity separation concentrate, wherein the gravity separation tailings enter a gravity separation tailings storage tank, and the gravity separation concentrate enters a gravity separation concentrate storage tank;
preferably, the working stroke frequency of the reselection equipment is 280-320 times/min, and the stroke is 10-16 mm. Wherein the gravity concentrate contains zirconium dioxide and ZrO as main components 2 The mass percentage content in the gravity concentrate is 88.0-99.0%. The main component of the tailings is SiO 2 。
And fifthly, delivering the gravity concentrate in the gravity concentrate storage tank into the magnetic separator for magnetic separation to obtain magnetic concentrate and magnetic substances, wherein the magnetic concentrate is a single crystal target product.
Preferably, the magnetic field intensity of the magnetic separator is 80-400 KA/m, and the rotating speed of the rotary drum is 10-25 rpm.
The invention has the beneficial effects that:
the invention provides a device for preparing crystals by pyrolysis and magnetic separation, which comprises a pyrolysis furnace, a discharging system, a gravity separation system and a magnetic separation system. Wherein, the discharging system comprises a cooling water tower, a cooling water circulating pump, a granulating tank and a scraper discharging machine. The granulating tank is provided with circulating cooling water, so that the granulating temperature can be ensured to be stable within a reasonable range, and the water consumption of the process is reduced. The scraper blade discharging machine comprises a horizontal section and an inclined section, wherein the horizontal section is embedded in the granulating groove, has a good stirring effect on granulated products, can improve granulating efficiency, and improves the granularity range width of the products. The equipment is universal equipment, easy to purchase and manufacture, simple and convenient to install, reliable in operation, low in energy consumption and small in occupied area, and the equipment can be arranged in a centralized way or installed in a segmented way according to the actual situation of a place.
The invention also provides a method for preparing crystals by using the device, taking zirconia as an example, in the pyrolysis process: 1) According to the invention, the pyrolysis additive is added into the pyrolysis furnace, so that pyrolysis can be performed at a lower temperature, such as 1300-1900 ℃, the selection range of refractory materials of the pyrolysis furnace is widened, the service life of the pyrolysis furnace is prolonged, and the energy consumption in the pyrolysis process is reduced. Compared with the traditional electric smelting desilication zirconia production process, the pyrolysis power consumption of only 5600 kw.h/t for producing 1 ton of desilication zirconia by adopting the method provided by the invention is reduced by 417.86kgce/tZrO 2 . 2) Compared with the traditional production process of the electric smelting desilication zirconia, the pyrolysis process of the invention has no direct carbon emission. By adopting the method provided by the invention, each 1 ton of desilication zirconia is produced, and the emission of 250kg of carbon dioxide to the atmosphere is reduced. 3) Compared with the production process of producing the desilication zirconia lump by cooling in the original furnace, the zirconia obtained by the pyrolysis melting product by adopting the quenching granulating method has uniform granularity and high qualification rate, and creates more superior conditions for subsequent processing refinement. Solves the problems of high hardness and difficult crushing of the desilication zirconia lump, and greatly improves the production efficiency of zirconia product crushing equipment.
In the product separation process, the pyrolysis product is subjected to reselection and magnetic separation in sequence. Wherein: 1) The energy consumption in the reselection process is low, no new impurity element is introduced, the purity of the reselected product is high, and the three wastes are not discharged, so that the method is environment-friendly. In addition, siO as a byproduct can be obtained through reselection 2 The volume weight of the catalyst can reach 1200kg/m 3 The above method is superior to the conventional electric smelting zirconia process in that 200kg/m of silica fume is obtained 3 Improves the transportation characteristics by 6 times and greatly enhances the transportation characteristics. 2) The gravity concentrate (gravity density) product is subjected to the magnetic separation again, so that the magnetic substances introduced in the whole production process can be removed, and the content of the magnetic substances in the zirconium dioxide product is ensured to meet the requirements.
Drawings
Fig. 1 is a schematic structural view of an apparatus according to the present invention for preparing crystals by pyrolysis and magnetic separation.
Wherein, the liquid crystal display device comprises a liquid crystal display device,
1-a pyrolysis furnace;
2-a discharging system;
21-a cooling tower; 22-a cooling water circulating pump; 23-granulating tank; 24-scraper discharging machine;
3-reselection systems;
31-a reselection device; 32-a gravity tailings storage tank; 33-gravity concentrate storage tank; 34-gravity concentrate feed pump;
4-magnetic separation system;
41-a magnetic separator; 42-magnetically separating concentrate product bin; 43-magnetic product bin.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, based on the examples herein, which are within the scope of the invention as defined by the claims, will be within the scope of the invention as defined by the claims.
The embodiment of the invention relates to a device for preparing crystals by pyrolysis and magnetic separation, which comprises a pyrolysis furnace 1, a discharging system 2, a gravity separation system 3 and a magnetic separation system 4, as shown in figure 1. Wherein the pyrolysis furnace 1 is used for heating and decomposing the raw materials to obtain pyrolysis products; the discharging system 2 is used for outputting and cooling pyrolysis products to obtain cooled products, and inputting the cooled products into the reselection system 3; the gravity separation system 3 is used for carrying out gravity separation on the cooled product to obtain gravity separation tailings and gravity separation concentrate; the magnetic separation system 4 is used for removing magnetic matters in the gravity concentrate to obtain magnetic concentrate, namely a single crystal target product.
Further, the discharging system 2 includes a cooling water tower 21, a cooling water circulation pump 22, a granulating tank 23, and a scraper discharging machine 24. Wherein the granulating tank 23 is for cooling the pyrolysis product outputted from the pyrolysis furnace 1 to obtain a cooled product. The granulating tank 23 is internally provided with a spray water pipe, the water outlet of the cooling tower 21 is connected with the water inlet of the spray water pipe through a pipeline, the spray water pipe sprays water into the granulating tank 23, and the pyrolysis products output by the pyrolysis furnace 1 are quenched to be granulated. The side of the granulating tank 23 is provided with a water outlet, the water outlet of the granulating tank 23 is connected with the water inlet of the cooling tower 21 through a pipeline, and the cooling water circulating pump 22 is positioned on the connecting pipeline of the spray water pipe and the cooling tower 21 and provides power for the circulation of cooling water in the pipeline.
In one embodiment of the invention, the granulation tank is a rectangular tank. Cooling water is sent into a nozzle of a spray header at a pressure of 0.35-0.65 MPa, pyrolysis products (in this case, pyrolysis molten fluid) output from the pyrolysis furnace 1 are quenched and solidified, and glassy SiO in the pyrolysis molten fluid is decomposed 2 Granulating into fine particles. The granulating tank may be constructed as disclosed in 205133641U.
The scraper discharger 24 is for discharging the cooled product from the granulating tank 23 while stirring the cooled product to uniformly mix it. As shown in fig. 1, the scraper discharging machine 24 comprises a horizontal section and an inclined section which are integrally formed, wherein the horizontal section is embedded in the granulating tank 23, a cylindrical roller (not shown) is arranged at the end of the horizontal section, and a chain and a scraper which are arranged on the roller stir the accumulated cooling products and continuously collect and convey materials; the inclined section extends away from the granulating tank 23, the material output end of the inclined section is connected with the feed inlet of the reselection system 3, and the tail end of the inclined section is higher than the position of the granulating tank 23. The output cooling product is continuously rolled and ground in the conveying process under the action of gravity in the inclined section, and further disintegrated. The function of the horizontal section is to collect the cooled product from the granulation tank 23 and to extend the cooling time. The inclined section acts to effect solid-liquid separation of the cooled product.
The gravity separation system 3 comprises a gravity separation device 31, a gravity separation tailings reservoir 32, a gravity separation concentrate reservoir 33 and a gravity separation concentrate feed pump 34. Wherein the re-separation device 31 is used for re-separating the cooled product to obtain re-separated tailings and re-separated concentrate. The gravity separation equipment 31 is provided with a gravity separation tailing discharge port and a gravity separation concentrate discharge port, the gravity separation tailing discharge port is connected with a feed port of the gravity separation tailing storage tank 32, and the gravity separation concentrate discharge port is connected with a feed port of the gravity separation concentrate storage tank 22. The gravity concentrate output from the gravity separation device 3 enters the gravity concentrate storage tank 22 and the gravity tailings enter the gravity tailings storage tank 32.
The discharge port of the gravity concentrate storage tank 33 is connected with the feed port of the magnetic separation system 4, and the gravity concentrate conveying pump 34 is positioned on the connecting pipeline of the gravity concentrate storage tank 33 and the magnetic separation system 4 and provides power for conveying gravity concentrate in the pipeline.
The magnetic separation system 4 comprises a magnetic separator 41, a magnetic concentrate product bin 42 and a magnetic product bin 43. Wherein, the magnetic separator 41 is used for carrying out magnetic separation on the gravity concentrate to obtain magnetic concentrate and magnetic matters. The magnetic separator 41 is provided with a magnetic concentrate discharge port and a magnetic substance discharge port, the magnetic concentrate discharge port is connected with a feed port of a magnetic concentrate product bin 42, and the magnetic substance discharge port is connected with a feed port of a magnetic substance product bin 43. The non-magnetic concentrate output from the magnetic separator 41 enters a magnetic concentrate product bin 42, and the magnetic substance enters a magnetic substance product bin 43.
From the process point of view, the same product can be obtained by magnetic separation and then reselection. However, if magnetic separation is performed before gravity separation, the material quantity treated by the two procedures is the same as the material quality (weight); if the gravity separation is carried out before the magnetic separation, the material quantity treated by the magnetic separation process is only 60-66% of the material mass. Therefore, from the aspects of fixed asset investment and production and operation costs, magnetic separation followed by reselection is not reasonable.
The embodiment of the invention also relates to a method for preparing crystals by using the device, taking the crystals as zirconium oxide as an example, comprising the following steps of:
step one, adding raw materials and pyrolysis additives into a pyrolysis furnace 1, and performing heating decomposition to obtain pyrolysis products;
in one embodiment of the invention, the feedstock is zircon sand, the major component of which is a silicate of zirconium, wherein ZrO 2 The mass percentage of the water content is 55.0-66.0%, and the water content is less than or equal to 1%.
In one embodiment of the invention, the pyrolysis additive is an alkaline earth metal oxide selected from at least one of CaO, mgO, all of which are technical grade. The addition amount of the pyrolysis additive is 5-15% of the mass of the zircon sand raw material by taking the mass of the zircon sand as 100%. The pyrolysis additive is reasonably used, so that the pyrolysis temperature can be reduced, for example, the addition amount of the pyrolysis additive is too small, the pyrolysis temperature is increased, and the pyrolysis energy consumption is increased; if the addition amount is too high, cubic crystal form products may appear in the pyrolysis products, and the production cost is increased.
In one embodiment of the invention, the pyrolysis furnace is a three-phase arc furnace, a direct current arc furnace, a rotary kiln, or a plasma furnace. The pyrolysis temperature is 1300-1900 ℃, the pyrolysis time is 45-120 minutes, and the pyrolysis process is carried out in the natural furnace gas atmosphere.
Step two, starting a cooling water circulating pump 22 after pyrolysis is finished, pouring pyrolysis products in the pyrolysis furnace 1 into a granulating tank 23, and cooling the pyrolysis products to obtain cooled products;
in one embodiment of the invention, the flow of cooling water output by the cooling water circulation pump 22 is 40 to 100 times the mass flow of pyrolysis products. The flow rate is formulated according to the cooling granulating effect of the pyrolysis products in a molten state output from the pyrolysis furnace 1 and the heating rate of the cooling water, and the reasonable flow rate is controlled to avoid production accidents such as vaporization or explosion of the cooling water. The mass flow of the pyrolysis product is 30-500 kg/min, and the flow rate of the cooling water is 5-10 m/s. The cooling tower 21 is provided with a forced ventilation motor, and the temperature of circulating water is kept to be less than or equal to 45 ℃.
In one embodiment of the present invention, the furnace tilting device of the pyrolysis furnace 1 is started, and the pyrolysis products in the pyrolysis furnace 1 are slowly poured into the granulating tank 13, and the pyrolysis products are granulated into balls. After the pyrolysis products in the pyrolysis furnace 1 are poured, the pyrolysis furnace 1 is adjusted to a pyrolysis operation position, and the step one is repeated. I.e. the raw materials and pyrolysis additives are continuously added to the pyrolysis furnace 1, and the pyrolysis furnace 1 enters the next working cycle. If the pyrolysis furnace 1 is another type of pyrolysis furnace other than an arc furnace, the granulation process of the pyrolysis products may be continuously performed, and the furnace tilting process of this step may be omitted.
Step three, starting a scraper discharging machine 24, and inputting the cooling products in the granulating tank 23 into a reselection device 31;
in one embodiment of the invention, the motor of the blade discharge machine 24 operates at a frequency of 20 to 50Hz which maintains the capacity of the conveyed material to match that of the reselection device 31.
The cooled product is subjected to gravity separation by gravity separation equipment 31 to obtain gravity separation tailings and gravity separation concentrate, wherein the gravity separation tailings enter a gravity separation tailings storage tank 32, and the gravity separation concentrate enters a gravity separation concentrate storage tank 33;
in one embodiment of the invention, the reselection device 31 is a shaker, jigger or spiral chute. The working stroke frequency of the reselection equipment 31 is 280-320 times/min, and the stroke is 10-16 mm. Wherein the gravity concentrate contains zirconium dioxide and ZrO as main components 2 The mass percentage content in the gravity concentrate is 88.0% -99.0%, siO 2 The mass percentage content in the gravity concentrate is 0.6-5.0%. The main component of the gravity tailings is SiO 2 Dehydrating and drying to obtain glassy SiO 2 And (5) a product. For the same reselection equipment 31, the operating parameters and the size range of the granulated material determine the throughput of the reselection equipment 31. If the grain size of the gravity concentrate is finer, the capacity of the gravity device 31 is smaller and the granulation grain size is related to the amount of water used for granulation. Unreasonable equipment parameters can affect the recovery rate and grade of the gravity concentrate.
And fifthly, delivering the gravity concentrate in the gravity concentrate storage tank 33 into the magnetic separator 41 for magnetic separation to obtain magnetic concentrate and magnetic substances, wherein the magnetic concentrate is a single crystal target product.
In one embodiment of the invention, the gravity concentrate delivery pump 34 is started to deliver gravity concentrate to the feed inlet of the magnetic separator 41, and the magnetic field strength and the rotating speed of the rotating drum of the magnetic separator 41 are set to obtain magnetic concentrate and magnetic substances. The magnetic concentrate enters a magnetic concentrate product bin 42 and the magnetic substance enters a magnetic substance product bin 43.
In one embodiment of the present invention, the magnetic field strength of the magnetic separator 41 is 80-400 KA/m, and the drum rotation speed is 10-25 rpm. The magnetic separation process is to remove the magnetic impurities in the zirconium dioxide product, and the main product zirconium dioxide is a non-magnetic substance, so that the increase of the magnetic field strength in a certain range has no influence on the production process and the product quality. However, the magnetic field strength deviates from the normal value, so that weak magnetic impurities in the product cannot be selected, and the quality of the product is affected.
Because the main component of the magnetic substance is a ferromagnetic substance, impurities which are not strictly introduced in the production process due to equipment abrasion and production control are produced. The magnetic substance is an externally introduced impurity, so that the content of the magnetic substance is uncertain, and the magnetic substance has certain contingency. The zirconia content in the magnetic concentrate is less than 1.0%.
Example 1
Zircon sand of a certain concentrating plant of Indonesia is used as raw material, and the main technical index is ZrO 2 ：65.5％、SiO 2 ：32.8％、Fe 2 O 3 ：0.2％、Al 2 O 3 :1.0% and 1.98% of 100 mesh oversize material.
The pyrolysis additive used in the test is industrial pure calcium oxide containing CaO:90.2% of zircon sand, and the addition amount is 6.0% of the mass of the raw zircon sand.
Preparing materials: the raw materials zircon sand and the pyrolysis additive are stirred and mixed uniformly, and the uniformly mixed powder is pressed into 35 multiplied by 25 multiplied by 15 cold-set balls by using the pressure of 35 MPa.
Pyrolysis reaction: the pyrolysis process is carried out in a direct current arc furnace, and the furnace lining is a self-baking furnace lining formed after zircon sand is preheated, baked and cooled. The liquid level diameter of the molten pool is 800mm, the volume of the molten pool is 60L, the electrode diameter phi is 250mm, the average current is 6500A, the average electrode voltage is 135V, the pyrolysis temperature is 1650 ℃, and the smelting time is 50min. And adding 318kg of cold solid balls into each furnace, and adopting submerged arc pyrolysis.
Cooling and granulating: the circulating water pressure of the spray pipe nozzle is 0.5MPa, the flow rate is 1500kg/min, and the cooling water flow rate is 7.15m/s. The scraper running speed of the scraper discharging machine is 0.05m/s. And after pyrolysis is finished, starting a cooling water circulating pump, lifting an electric furnace electrode, deflecting the electrode to leave the electric furnace, tilting the furnace body, controlling pyrolysis melt to slowly flow into the granulating tank, and discharging for 10min.
And (3) reselection: the gravity separation adopts a cloud tin type fine sand shaking table, the size of the bed surface is 4310 multiplied by 1100 multiplied by 500, the stroke is 15mm, the stroke frequency is 220 times per minute, the gradient of the bed surface is 2 degrees, the ore feeding concentration is 10 percent, and the water washing quantity is 35L/min.
Magnetic separation: the magnetic separation equipment is a semi-countercurrent permanent magnet wet magnetic separator, the diameter phi of the roller is 400mm, the length of the roller is 600mm, the induction intensity of the magnetic field of the roller is 3800Gs, the rotating speed is 20rpm, the ore feeding concentration is 20%, and the concentrate flushing water pressure is 0.25MPa.
The product quality and process economic index are shown in Table 1:
TABLE 1
In table 1, other losses are mainly the volatilization losses of silicon oxide caused by the oxidation-reduction reaction of silicon dioxide and graphite electrodes after pyrolysis of the raw materials. The pyrolysis power consumption of ton of product (desilicated zirconium dioxide) was 5425.31kw.h calculated from the pyrolysis average current and voltage. The consumption of the graphite electrode is 13.28Kg, the unit consumption is 67.33Kg/t after the conversion according to the zirconium dioxide product amount, and the pyrolysis rate of the raw material is 98.5 percent.
Comparative example 1
Zircon sand feedstock was the same as in example 1.
The procedure of example 1 was followed without the use of a pyrolysis additive. The product quality and process economic index are shown in Table 2:
TABLE 2
The pyrolysis power consumption of ton products (desilicated zirconium dioxide) was 4055.52kw.h calculated from the pyrolysis average current and voltage. The consumption of the graphite electrode is 13.95Kg, and the unit consumption is 52.85Kg/t after being converted according to the zirconium dioxide product quantity.
Under the same technological parameters, the pyrolysis is carried out without adding a pyrolysis additive, and the pyrolysis rate of the raw material is only 36.0 percent calculated according to the yield of the silicon dioxide product (the silicon dioxide content with volatilization loss).
Comparative example 2
Zircon sand feedstock was the same as in example 1.
The addition amount of the pyrolysis additive in the test is 20.0% of the mass of the zircon sand serving as the raw material. Other procedure was as in example 1. The product quality and process economic index are shown in Table 3:
TABLE 3 Table 3
The pyrolysis power consumption of ton of product (desilicated zirconium dioxide) was 5387.66kw.h calculated from the pyrolysis average current and voltage. The consumption of the graphite electrode is 13.18Kg, and the unit consumption is 66.33Kg/t after being converted according to the zirconium dioxide product quantity.
Under the condition of the same process parameters, excessive pyrolysis additive is added for pyrolysis, and the pyrolysis rate of the raw material reaches 99.0 percent according to the yield of the silicon dioxide product (the silicon dioxide content with volatilization loss). Comparing the data in tables 3 and 1, the calcium oxide content of the zirconia product was increased by 148.07%. The zirconia product was observed by means of scanning electron microscopy (SEM pictures) to find small amounts of Zr 4+ Ca with similar radius 2+ Ion-substituted Zr 4+ Is a part of the zirconia to form semi-stable zirconia (t-ZrO 2 ) Because the pyrolysis process is carried out at a lower temperature (1650 ℃ C.), the zirconium dioxide cube (c-ZrO) 2 ) The transition temperature of the crystal (2370 ℃ C.) the zirconium dioxide product is also in monoclinic (m-ZrO) 2 ) The crystal form is mainly. Residual pyrolysis additive CaO and SiO after zircon sand pyrolysis 2 And (3) introducing the compound production silicate into the gravity tailings.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. An apparatus for preparing crystals by pyrolysis and magnetic separation, characterized in that the apparatus comprises a pyrolysis furnace, a discharge system, a gravity separation system and a magnetic separation system, wherein,
the pyrolysis furnace is used for heating and decomposing the raw materials to obtain pyrolysis products;
the discharging system is used for outputting and cooling the pyrolysis product to obtain a cooled product, and inputting the cooled product into the reselection system;
the gravity separation system is used for carrying out gravity separation on the cooling product to obtain gravity separation tailings and gravity separation concentrate;
the magnetic separation system is used for removing magnetic matters in the gravity concentrate to obtain magnetic concentrate, namely a single crystal target product;
the discharging system comprises a cooling water tower, a cooling water circulating pump, a granulating tank and a scraper discharging machine, wherein,
the granulating tank is used for cooling pyrolysis products output from the pyrolysis furnace to obtain cooling products, a spray water pipe is arranged in the granulating tank, a water outlet of the cooling water tower is connected with a water inlet of the spray water pipe through a pipeline, water is sprayed into the granulating tank by the spray water pipe, a water outlet is arranged on the side face of the granulating tank, a water outlet of the granulating tank is connected with a water inlet of the cooling water tower through a pipeline, and the cooling water circulating pump is positioned on a connecting pipeline of the spray water pipe and the cooling water tower;
the scraper discharging machine is used for outputting the cooling product from the granulating tank and stirring the cooling product to uniformly mix the cooling product, the scraper discharging machine comprises a horizontal section and an inclined section which are integrally formed, the horizontal section is embedded in the granulating tank, the inclined section extends to a direction far away from the granulating tank, and the material output end of the inclined section is connected with a feed inlet of the gravity separation system;
the gravity separation system comprises gravity separation equipment, a gravity separation tailing storage tank, a gravity separation concentrate storage tank and a gravity separation concentrate delivery pump, wherein,
the gravity separation equipment is used for carrying out gravity separation on the cooled product to obtain gravity separation tailings and gravity separation concentrate, the gravity separation equipment is provided with a gravity separation tailings discharge port and a gravity separation concentrate discharge port, the gravity separation tailings discharge port is connected with the feed inlet of the gravity separation tailings storage tank, the gravity separation concentrate discharge port is connected with the feed inlet of the gravity separation concentrate storage tank,
the discharge port of the gravity concentrate storage tank is connected with the feed port of the magnetic separation system, and the gravity concentrate conveying pump is positioned on a connecting pipeline of the gravity concentrate storage tank and the magnetic separation system;
the magnetic separation system comprises a magnetic separator, a magnetic concentrate product bin and a magnetic product bin, wherein,
the magnetic separator is used for carrying out magnetic separation on the gravity concentrate to obtain magnetic concentrate and magnetic matters, a magnetic concentrate discharge port and a magnetic matter discharge port are arranged on the magnetic separator, the magnetic concentrate discharge port is connected with a feed port of a magnetic concentrate product bin, and the magnetic matter discharge port is connected with a feed port of the magnetic matter product bin.
2. A method for producing zirconia crystals using the apparatus of claim 1, comprising the steps of:
step one, adding raw materials and pyrolysis additives into a pyrolysis furnace, and heating and decomposing to obtain pyrolysis products;
step two, starting a cooling water circulating pump after pyrolysis is finished, pouring pyrolysis products in the pyrolysis furnace into a granulating tank, and cooling the pyrolysis products to obtain cooled products;
step three, starting a scraper discharging machine, and inputting cooling products in the granulating tank into the reselection equipment;
the gravity separation equipment performs gravity separation on the cooled product to obtain gravity separation tailings and gravity separation concentrate, wherein the gravity separation tailings enter a gravity separation tailings storage tank, and the gravity separation concentrate enters a gravity separation concentrate storage tank;
and fifthly, delivering the gravity concentrate in the gravity concentrate storage tank into the magnetic separator for magnetic separation to obtain magnetic concentrate and magnetic substances, wherein the magnetic concentrate is a single crystal target product.
3. The method according to claim 2, wherein in the first step, the raw material is zircon sand, the pyrolysis additive is alkaline earth metal oxide, and at least one of CaO and MgO is selected from the group consisting of;
and/or, the addition amount of the pyrolysis additive is 5% -15% of the mass of the zircon sand raw material by taking the mass of the zircon sand as 100%.
4. The method according to claim 2, wherein in the first step, the pyrolysis temperature is 1300-1900 ℃, the pyrolysis time is 45-120 minutes, and the pyrolysis process is performed in a natural furnace gas atmosphere.
5. The method according to claim 2, wherein in the second step, the flow rate of the cooling water outputted by the cooling water circulation pump is 40 to 100 times the mass flow rate of the pyrolysis product;
and/or the mass flow rate of the pyrolysis product is 30-500 kg/min, and the flow rate of cooling water is 5-10 m/s;
and/or the temperature of the circulating water provided by the cooling water tower is less than or equal to 45 ℃.
6. The method according to claim 2, wherein in the fourth step, the working stroke frequency of the reselection equipment is 280-320 times/min, and the stroke is 10-16 mm.
7. The method according to claim 2, wherein in the fifth step, the magnetic field strength of the magnetic separator is 80-400 ka/m, and the rotating speed of the drum is 10-25 rpm.
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