CN113860319A - Zircon sand production method - Google Patents
Zircon sand production method Download PDFInfo
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- CN113860319A CN113860319A CN202111118431.4A CN202111118431A CN113860319A CN 113860319 A CN113860319 A CN 113860319A CN 202111118431 A CN202111118431 A CN 202111118431A CN 113860319 A CN113860319 A CN 113860319A
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- 239000004576 sand Substances 0.000 title claims abstract description 163
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 229910052845 zircon Inorganic materials 0.000 title claims abstract description 151
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 34
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 80
- 239000007788 liquid Substances 0.000 claims abstract description 70
- 238000000926 separation method Methods 0.000 claims abstract description 46
- 239000000047 product Substances 0.000 claims abstract description 44
- 239000011265 semifinished product Substances 0.000 claims abstract description 39
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000000746 purification Methods 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000011010 flushing procedure Methods 0.000 claims description 47
- 238000005406 washing Methods 0.000 claims description 37
- 239000011343 solid material Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- 238000007885 magnetic separation Methods 0.000 claims description 14
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- 239000003546 flue gas Substances 0.000 claims description 9
- 239000002918 waste heat Substances 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000003556 assay Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000005484 gravity Effects 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 19
- 239000012530 fluid Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 238000005903 acid hydrolysis reaction Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000005188 flotation Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- 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
- C01B33/20—Silicates
-
- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a zircon sand production method, which comprises the following steps: carrying out physical purification on the zircon sand rough sand to obtain a zircon sand semi-finished product, wherein the mass percent of zirconium oxide is 60-70%, the mass percent of titanium oxide is 0.12-0.18%, the mass percent of iron oxide is 0.2-0.5%, and the whiteness of the zircon sand is 55-70%; carrying out acidolysis on the zircon sand semi-finished product, wherein the acidolysis comprises the step of placing the zircon sand semi-finished product in a dilute hydrochloric acid solution, stirring for 1-3 hours, wherein the mass percent of hydrochloric acid in the dilute hydrochloric acid solution is 5.1-10%, and heating the dilute hydrochloric acid solution to 70-80 ℃; and carrying out solid-liquid separation to obtain a zircon sand finished product. The method can firstly adopt physical purification to obtain a semi-finished zircon sand product, and purify the zircon sand to a higher grade; then the semi-finished zircon sand product is acidolyzed by dilute hydrochloric acid solution and at a lower heating temperature, so that the whiteness of the finally obtained zircon sand product is improved to over 80.
Description
Technical Field
The invention relates to the technical field of mineral separation, in particular to a production method of zircon sand.
Background
Zircon sand is mainly used in the ceramic industry, refractory industry, casting industry, zirconium metal and its chemicals, etc., wherein the ceramic industry is currently the most widely used field of zirconium worldwide. At present, zirconium resources are relatively lacked in China, and particularly, high-quality zirconium resources still mainly depend on imports.
Because of the mineralization of the zircon sand, the impurity components contained in the zircon sand all over the world are different, for the existing physical purification methods utilizing the physical properties of the zircon sand, such as gravity separation, flotation, magnetic separation, electric separation and the like, including the mineral separation method of a single or combined physical purification method, the quality of the finally produced finished zircon sand still needs to be improved, the zircon sand obtained by the physical purification method has poor effect when being used in the industries of zirconium silicate and chemical zirconium, so that the problems of poor whiteness and color development capability and the like of the zirconium silicate when being used in the ceramic industry occur; in addition, in the chemical zirconium industry, the problems of blockage, unsmooth production, large amount of waste residues and the like occur in the chemical process.
In recent years, some enterprises in China pay attention to the problem of high impurity content of zircon sand, and the quality requirements of products are still not satisfactory through a single or combined physical purification type ore dressing method such as gravity separation, flotation, magnetic separation, electric separation and the like; the method for removing iron by the acid hydrolysis of zircon sand in enterprises or colleges comprises the steps of putting the zircon sand into a reaction kettle and carrying out acid hydrolysis on the zircon sand and 15% -20% of concentrated hydrochloric acid, and carrying out external heating to realize that the temperature in the reaction kettle is 80-95 ℃ and heat preservation is carried out for 2-5 hours, so as to obtain a zircon sand finished product with low impurity content and high whiteness. The method has the advantages of high concentration of the needed hydrochloric acid, high reaction temperature and improved whiteness. Therefore, a method for producing zircon sand with higher efficiency, environmental protection, low cost and convenience for large-scale production is urgently needed to solve the technical problems.
Disclosure of Invention
The invention mainly aims to provide a production method of zircon sand, aiming at improving the whiteness of zircon sand finished products.
The researcher of this application discovers, and the existence of iron oxide impurities such as ferric oxide in the zircon sand hinders the promotion of zircon sand whiteness degree, on the off-the-shelf basis of the concentrated hydrochloric acid method of generally adopting preparation zircon sand, and the content of adding big concentrated hydrochloric acid is not obvious to the whiteness degree continuation promotion of zircon sand off-the-shelf.
In order to achieve the purpose, the production method of the zircon sand provided by the invention comprises the following steps: carrying out physical purification on zircon sand rough sand to obtain a zircon sand semi-finished product, wherein the zircon sand semi-finished product comprises 60-70% by mass of zirconium oxide, 0.12-0.18% by mass of titanium oxide and 0.2-0.5% by mass of iron oxide, and the whiteness of the zircon sand is 55-70%; carrying out acidolysis on the zircon sand semi-finished product, wherein the acidolysis step comprises the step of placing the zircon sand semi-finished product in a dilute hydrochloric acid solution, stirring for 1-3 hours, wherein the mass percent of hydrochloric acid in the dilute hydrochloric acid solution is 5.1-10%, and heating the dilute hydrochloric acid solution to 70-80 ℃; and carrying out solid-liquid separation to obtain a zircon sand finished product.
Optionally, the step of performing solid-liquid separation to obtain a zircon sand finished product includes the following steps: recovering the recovered liquid obtained by solid-liquid separation for subsequent acidolysis of the zircon sand semi-finished product, wherein the mass percent of hydrochloric acid in the recovered liquid is 5.3-10.5%; and washing the solid material obtained by solid-liquid separation to obtain a zircon sand finished product. The zircon sand semi-finished product after physical purification has higher grade and less metal oxides, so that the whiteness of the zircon sand finished product is improved to over 80 by using the zircon sand production method, and simultaneously, the reduction degree of the hydrochloric acid concentration can be reduced, so that the dilute hydrochloric acid solution after acidolysis still has stronger acidolysis capability and can be used for the subsequent acidolysis process of the zircon sand semi-finished product.
Optionally, the step of washing the solid material obtained through solid-liquid separation to obtain the zircon sand finished product includes the following steps: and (3) washing the solid material obtained through solid-liquid separation at least twice, wherein the pH value of the washing liquid washed at least twice is gradually increased. The pH value of the flushing liquid flushed at least twice successively gradually rises, so that the flushing liquid can better adapt to solid materials with the gradually rising pH value, and the flushing effect is improved.
Optionally, the step of sequentially washing the solid material obtained through solid-liquid separation at least twice includes the following steps: washing the solid material by a washing device, wherein the washing device comprises at least two washing areas which are sequentially connected along the material conveying direction; when cleaning is carried out, the flushing liquid flushed in the latter flushing area is used as the flushing liquid in the former flushing area; and recovering the flushing liquid after flushing the flushing area which is positioned at the foremost end of the material conveying direction, and using the recovered flushing liquid to produce the artificial rutile. Through setting up the washing unit who includes at least two flushing areas that connect gradually along material direction of delivery, the flush fluid after the washing of back flushing area can be retrieved and be used for the washing of preceding flushing area, makes the flush fluid can recycle in the production of many batches of zircon sand, has improved the utilization ratio of flush fluid, makes the ferric chloride more enrichment in the flush fluid after the flushing area that is located the most front end of material direction of delivery simultaneously, more is favorable to collecting remaining chloride.
Optionally, the flushing device comprises vacuum belt filters connected in sequence along the material conveying direction, and a water outlet pipe is arranged above the vacuum belt filters.
Optionally, after the step of sequentially washing at least two times the solid material obtained through solid-liquid separation, the method further comprises the following steps: and drying and cooling the washed solid materials in sequence to obtain a zircon sand finished product.
Optionally, the mass percentage of zirconium oxide in the zircon sand semi-finished product is 60-67%; heating the dilute hydrochloric acid solution to 75-80 ℃; and (3) placing the semi-finished zircon sand product in dilute hydrochloric acid solution, and stirring for 1.5-2.5 hours, thereby further improving the whiteness of the zircon sand product.
Optionally, the dilute hydrochloric acid solution is heated by using the waste heat of the flue gas, and/or the step of physically purifying the zircon sand rough sand comprises the steps of reselecting the zircon sand rough sand, carrying out first magnetic separation, carrying out electric separation and carrying out second magnetic separation in sequence, wherein the magnetic field intensity of the second magnetic separation is greater than that of the first magnetic separation, so that the requirement of the acidolysis step is met by the zircon sand semi-finished product obtained by physical purification, and the whiteness of the zircon sand finished product is further improved by matching with the acidolysis step. The dilute hydrochloric acid liquid is heated by using the waste heat of the flue gas, so that the waste heat of the flue gas with a low heat value can be used for heating to the required temperature, and the waste heat of the waste flue gas is fully utilized.
Optionally, before the step of performing solid-liquid separation, the method further comprises the following steps: sampling and testing after the acidolysis reaction is carried out for a preset time; and when the sampling assay meets a preset index, ending the acidolysis reaction.
Optionally, the preset index comprises that the content of iron oxide is less than 0.15%, so that the acidolysis reaction can be monitored, the abnormal condition can be avoided, and the production success rate of the zircon sand product can be improved.
The technical scheme includes that the zircon sand rough sand is physically purified, and the zircon sand semi-finished product is subjected to acidolysis, wherein the acidolysis step comprises the steps of placing the zircon sand semi-finished product in a dilute hydrochloric acid solution, stirring for 1-3 hours, wherein the mass percent of hydrochloric acid in the dilute hydrochloric acid solution is 5.1-10%, and heating the dilute hydrochloric acid solution to 70-80 ℃; carrying out solid-liquid separation to obtain a zircon sand finished product, wherein a zircon sand semi-finished product can be obtained by physical purification, and the zircon sand is purified to a higher grade; then the semi-finished zircon sand product is acidolyzed by dilute hydrochloric acid solution and at a lower heating temperature, so that the whiteness of the finally obtained zircon sand product is improved to over 80. And dilute hydrochloric acid solution is adopted, so that the corrosion to reaction equipment is reduced, and the service life of the reaction equipment is prolonged.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a schematic view showing the steps of one embodiment of the zircon sand production method of the present invention.
FIG. 2 is a schematic flow chart of another embodiment of the zircon sand production method of the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that if directional indications (such as up, down, left, right, front, and back … …) are involved in the embodiment of the present invention, the directional indications are only used to explain the relative positional relationship between the components, the movement situation, and the like in a specific posture, and if the specific posture is changed, the directional indications are changed accordingly.
In addition, if there is a description of "first", "second", etc. in an embodiment of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, if the meaning of "and/or" and/or "appears throughout, the meaning includes three parallel schemes, for example," A and/or B "includes scheme A, or scheme B, or a scheme satisfying both schemes A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The researcher of this application discovers, and the existence of iron oxide impurities such as ferric oxide in the zircon sand hinders the promotion of zircon sand whiteness degree, on the off-the-shelf basis of the concentrated hydrochloric acid method of generally adopting preparation zircon sand, and the content of adding big concentrated hydrochloric acid is not obvious to the whiteness degree continuation promotion of zircon sand off-the-shelf. Further research by researchers of the application finds that the use of the zircon sand is seriously influenced due to the existence of the main impurity component Fe in the zircon sand. The zirconium silicate of the subsequent product has the problems of poor whiteness and color development capability and the like when used in the ceramic industry due to the high content of Fe impurities. In this case, the concentration of hydrochloric acid is increased in the acidolysis process using concentrated hydrochloric acid, which is usually used, and thus the removal of Fe as an impurity is not greatly facilitated. Therefore, the invention provides a production method of zircon sand.
Referring to fig. 1, in an embodiment of the present invention, the zircon sand production method includes the following steps: carrying out physical purification on the zircon sand rough sand to obtain a zircon sand semi-finished product, wherein the zircon sand semi-finished product comprises 60 to 70 mass percent of zirconium oxide, 0.12 to 0.18 mass percent of titanium oxide, 0.2 to 0.5 mass percent of iron oxide, and the whiteness of the zircon sand is 55 to 70; carrying out acidolysis on the zircon sand semi-finished product, wherein the acidolysis step comprises the steps of placing the zircon sand semi-finished product in a dilute hydrochloric acid solution, stirring for 1-3 hours, wherein the mass percent of hydrochloric acid in the dilute hydrochloric acid solution is 5.1-10%, and heating the dilute hydrochloric acid solution to 70-80 ℃; and carrying out solid-liquid separation to obtain a zircon sand finished product.
Performing physical purification on zircon sand rough sand, and performing acidolysis on the zircon sand semi-finished product, wherein the acidolysis step comprises the steps of placing the zircon sand semi-finished product in a dilute hydrochloric acid solution, stirring for 1-3 hours, wherein the mass percent of hydrochloric acid in the dilute hydrochloric acid solution is 5.1-10%, and heating the dilute hydrochloric acid solution to 70-80 ℃; carrying out solid-liquid separation to obtain a zircon sand finished product, wherein a zircon sand semi-finished product can be obtained by physical purification, and the zircon sand is purified to a higher grade; then the semi-finished zircon sand product is acidolyzed by dilute hydrochloric acid solution and at a lower heating temperature, so that the whiteness of the finally obtained zircon sand product is improved to over 80. And dilute hydrochloric acid solution is adopted, so that the corrosion to reaction equipment is reduced, and the service life of the reaction equipment is prolonged.
As an alternative embodiment, the mass percentage of zirconium oxide in the zircon sand semi-finished product is 60 to 67 percent; heating the dilute hydrochloric acid solution to 75-80 ℃; the semi-finished zircon sand product is placed in dilute hydrochloric acid solution and stirred for 1.5 to 2.5 hours, so that the whiteness of the zircon sand product is further improved.
Referring to fig. 2, in another embodiment of the present invention, the zircon sand production method comprises the following steps:
the zircon sand rough sand is physically purified to obtain a zircon sand semi-finished product, and zirconium oxide (zirconium dioxide ZrO in the embodiment) in the zircon sand semi-finished product2As an index), 60 to 70% by mass of titanium oxide (in this example, titanium dioxide, TiO)2As an index) of 0.12 to 0.18 percent and iron oxide (ferric oxide Fe in the embodiment)2O3As an index) of 0.2 to 0.5 percent by mass, and the whiteness of the zircon sand is between 55 and 70; the step of carrying out physical purification on the zircon sand rough sand comprises the steps of reselecting, carrying out first magnetic separation, carrying out electric separation and carrying out second magnetic separation on the zircon sand rough sand in sequence, wherein the magnetic field intensity of the second magnetic separation is greater than that of the first magnetic separation, so that the zircon sand semi-finished product obtained by the physical purification can meet the requirement of the acid hydrolysis step, and the whiteness of the zircon sand finished product is further improved by matching with the acid hydrolysis step.
Carrying out acidolysis on the zircon sand semi-finished product, wherein the acidolysis step comprises the steps of placing the zircon sand semi-finished product in a dilute hydrochloric acid solution, stirring for 1-3 hours, wherein the mass percent of hydrochloric acid in the dilute hydrochloric acid solution is 5.1-10%, and heating the dilute hydrochloric acid solution to 70-80 ℃; before the step of carrying out solid-liquid separation, the method also comprises the following steps: sampling and testing after the acidolysis reaction is carried out for a preset time; and when the sampling assay meets the preset index, ending the acidolysis reaction. The preset indexes comprise that the content of iron oxide is less than 0.15%, which is beneficial to monitoring acidolysis reaction, avoiding abnormal conditions and improving the production success rate of zircon sand products. And carrying out solid-liquid separation to obtain a zircon sand finished product. In the acidolysis step, the dilute hydrochloric acid solution is heated by the waste heat of the flue gas. The dilute hydrochloric acid liquid is heated by using the waste heat of the flue gas, so that the waste heat of the flue gas with a low heat value can be used for heating to the required temperature, and the waste heat of the waste flue gas is fully utilized.
Specifically, the step of performing solid-liquid separation to obtain the zircon sand finished product comprises the following steps of: and recovering the recovered liquid obtained by solid-liquid separation for subsequent acidolysis of the zircon sand semi-finished product, wherein the mass percent of hydrochloric acid in the recovered liquid is 5.3-10.5%. Specifically, the acid hydrolysis is finished, then the acid hydrolysis is carried out, the material discharged from the tank is pumped to a first-stage vacuum belt filter for solid-liquid separation, and the separated liquid is recycled for the next acid hydrolysis because of small change of the acid concentration. And then washing the solid material obtained by solid-liquid separation (explained in more detail later) to obtain the zircon sand finished product. The zircon sand semi-finished product after physical purification has higher grade and less metal oxides, so that the whiteness of the zircon sand finished product is improved to over 80 by using the zircon sand production method, and simultaneously, the reduction degree of the hydrochloric acid concentration can be reduced, so that the dilute hydrochloric acid solution after acidolysis still has stronger acidolysis capability and can be used for the subsequent acidolysis process of the zircon sand semi-finished product.
As a further alternative embodiment, the implementation is specifically carried out according to the examples of specific values in table 1 below. As can be seen from the following further optional examples, the method for producing zircon sand of the present application can perform acidolysis on the zircon sand semi-finished product with a relatively dilute hydrochloric acid solution (concentration 5.4% to 9.31%) and at a relatively low heating temperature (70 ℃ to 80 ℃), so that the whiteness of the finally obtained zircon sand finished product is increased to over 80, and the whiteness of most zircon sand finished products can reach about 90.
TABLE 1 further alternative examples
Specifically, the step of washing the solid material obtained by solid-liquid separation to obtain the zircon sand finished product comprises the following steps: and (3) washing the solid material obtained by solid-liquid separation at least twice, wherein the pH value of the washing liquid washed at least twice is gradually increased. The pH value of the flushing liquid flushed at least twice successively gradually rises, so that the flushing liquid can better adapt to solid materials with the gradually rising pH value, and the flushing effect is improved.
More specifically, the step of washing the solid material obtained by solid-liquid separation at least twice sequentially comprises the following steps: the solid material is washed by the washing device, the washing device comprises vacuum belt filters which are sequentially connected along the material conveying direction, namely, the multistage vacuum belt filters are arranged, and a water outlet pipe is arranged above the vacuum belt filters. The vacuum belt filter is a device which uses vacuum negative pressure as driving force to realize solid-liquid separation. Under the action of vacuum negative pressure (about 0.04-0.07MPa), liquid in suspension is pumped out through the filtering medium (filter cloth), and solid particles are intercepted by the filtering medium, so that the separation of liquid and solid is realized. The filtering sections are arranged along the horizontal length direction in the structure, and can continuously complete the operations of filtering, washing, sucking, filter cloth regeneration and the like. The vacuum belt filter has the advantages of high filtering efficiency, large production capacity, good washing effect, low water content of filter cakes, flexible operation, low maintenance cost and the like. The vacuum belt filter is widely applied to the fields of metallurgy, mines, chemical industry, papermaking, food, pharmacy, environmental protection and the like. The flushing device comprises at least two flushing areas which are sequentially connected along the material conveying direction; when cleaning is carried out, the flushing liquid flushed in the latter flushing area is used as the flushing liquid in the former flushing area; and recovering the flushing liquid after flushing the flushing area which is positioned at the foremost end of the material conveying direction, and using the recovered flushing liquid to produce the artificial rutile. The wet material obtained by the solid-liquid separation is subjected to back flushing by a lower two-stage vacuum belt filter, the back flushing is divided into A, B, C three areas, flushing pipes (namely water outlet pipes) and circulating liquid pools are respectively arranged in the vacuum belt filter, a discharge end (area A) at the rearmost end is flushed by tap water, liquid filtered out from the area A is recycled by a corresponding circulating pool below and is used for flushing a previous area (area B), and by analogy, liquid recycled from the area B is used for flushing an area C of the previous area, and the like.
Through setting up the washing unit who includes at least two flushing areas that connect gradually along material direction of delivery, the flush fluid after the washing of back flushing area can be retrieved and be used for the washing of preceding flushing area, makes the flush fluid can recycle in the production of many batches of zircon sand, has improved the utilization ratio of flush fluid, makes the ferric chloride more enrichment in the flush fluid after the flushing area that is located the most front end of material direction of delivery simultaneously, more is favorable to collecting remaining chloride. Specifically, iron chloride (FeCl) is contained in the rinse liquid after rinsing in the rinse zone located at the forefront in the material conveying direction3) More rich, FeCl3The reaction is carried out in the corrosion process to generate hydrated iron oxide which is finally used for producing iron oxide red, thereby realizing FeCl3And (5) resource utilization of waste residues. The process not only realizes chloride washing, but also realizes solid-liquid separation and dehydration.
After the step of washing the solid material obtained by solid-liquid separation at least twice, the method also comprises the following steps: and drying and cooling the washed solid materials in sequence, feeding and lifting the cooled zircon sand into a finished product bin, and packaging to obtain a high-quality zircon sand finished product. The production method of the zircon sand is connected in the whole flow, can realize continuous large-scale production, and has the advantages of high efficiency, environmental protection and low treatment cost. The whole process is high in continuity and short in time when the qualified product is finally produced, automatic control is favorably realized, acid liquor in the production process is recycled step by step, and meanwhile, waste residues are timely recycled, so that resource utilization is realized, benefits are increased, and the environment-friendly treatment cost is reduced. Because the concentration of the used acid liquid is lower, the equipment only needs simple antiseptic treatment, the whole investment cost is lower, and enterprises can develop the production of the zircon sand more favorably.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. The production method of zircon sand is characterized by comprising the following steps:
carrying out physical purification on zircon sand rough sand to obtain a zircon sand semi-finished product, wherein the zircon sand semi-finished product comprises 60-70% by mass of zirconium oxide, 0.12-0.18% by mass of titanium oxide and 0.2-0.5% by mass of iron oxide, and the whiteness of the zircon sand is 55-70%;
carrying out acidolysis on the zircon sand semi-finished product, wherein the acidolysis step comprises the step of placing the zircon sand semi-finished product in a dilute hydrochloric acid solution, stirring for 1-3 hours, wherein the mass percent of hydrochloric acid in the dilute hydrochloric acid solution is 5.1-10%, and heating the dilute hydrochloric acid solution to 70-80 ℃;
and carrying out solid-liquid separation to obtain a zircon sand finished product.
2. The zircon sand production method according to claim 1, wherein the step of performing solid-liquid separation to obtain a zircon sand finished product comprises the steps of:
recovering the recovered liquid obtained by solid-liquid separation for subsequent acidolysis of the zircon sand semi-finished product, wherein the mass percent of hydrochloric acid in the recovered liquid is 5.3-10.5%;
and washing the solid material obtained by solid-liquid separation to obtain a zircon sand finished product.
3. The zircon sand production method according to claim 2, wherein the step of washing the solid material obtained by the solid-liquid separation to obtain the final zircon sand product comprises the steps of:
and (3) washing the solid material obtained through solid-liquid separation at least twice, wherein the pH value of the washing liquid washed at least twice is gradually increased.
4. The zircon sand production method according to claim 3, wherein the step of washing the solid material obtained by the solid-liquid separation at least twice in sequence comprises the following steps:
washing the solid material by a washing device, wherein the washing device comprises at least two washing areas which are sequentially connected along the material conveying direction; when cleaning is carried out, the flushing liquid flushed in the latter flushing area is used as the flushing liquid in the former flushing area;
and recovering the flushing liquid after flushing the flushing area which is positioned at the foremost end of the material conveying direction, and using the recovered flushing liquid to produce the artificial rutile.
5. The zircon sand production method according to claim 4, wherein the flushing device comprises a vacuum belt filter connected in sequence along the material conveying direction, and a water outlet pipe is arranged above the vacuum belt filter.
6. The zircon sand production method according to claim 3, wherein the step of washing the solid material obtained by the solid-liquid separation at least twice in sequence further comprises the following steps:
and drying and cooling the washed solid materials in sequence to obtain a zircon sand finished product.
7. The method for producing zircon sand according to claim 1, wherein the zircon oxide content in the zircon sand semifinished product is 60 to 67% by mass; heating the dilute hydrochloric acid solution to 75-80 ℃; and (3) placing the zircon sand semi-finished product in dilute hydrochloric acid solution, and stirring for 1.5-2.5 hours.
8. The zircon sand production method according to claim 1, wherein the dilute hydrochloric acid solution is heated by using waste heat of flue gas, and/or the step of physically purifying the zircon sand rough sand comprises the steps of gravity separation, first magnetic separation, electric separation and second magnetic separation of the zircon sand rough sand in sequence, wherein the magnetic field strength of the second magnetic separation is greater than that of the first magnetic separation.
9. The zircon sand production method according to claim 1, further comprising, before the step of performing solid-liquid separation, the steps of:
sampling and testing after the acidolysis reaction is carried out for a preset time;
and when the sampling assay meets a preset index, ending the acidolysis reaction.
10. The zircon sand production method according to claim 9, wherein the predetermined criteria includes an iron oxide content of less than 0.15%.
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