CN113860319A - Zircon sand production method - Google Patents

Zircon sand production method Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
zircon sand
finished product
hydrochloric acid
solid
semi
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202111118431.4A
Other languages
Chinese (zh)
Inventor
李吕华
谭健锋
王祥丁
黄翔
刘永雄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangxi Yueqiao New Material Technology Co ltd
Guangdong Yueqiao New Material Technology Co ltd
Original Assignee
Guangxi Yueqiao New Material Technology Co ltd
Guangdong Yueqiao New Material Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangxi Yueqiao New Material Technology Co ltd, Guangdong Yueqiao New Material Technology Co ltd filed Critical Guangxi Yueqiao New Material Technology Co ltd
Priority to CN202111118431.4A priority Critical patent/CN113860319A/en
Publication of CN113860319A publication Critical patent/CN113860319A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/129Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Landscapes

  • 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

Zircon sand production method
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
Figure BDA0003274638280000061
Figure BDA0003274638280000071
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%.
CN202111118431.4A 2021-09-23 2021-09-23 Zircon sand production method Pending CN113860319A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111118431.4A CN113860319A (en) 2021-09-23 2021-09-23 Zircon sand production method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111118431.4A CN113860319A (en) 2021-09-23 2021-09-23 Zircon sand production method

Publications (1)

Publication Number Publication Date
CN113860319A true CN113860319A (en) 2021-12-31

Family

ID=78993729

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111118431.4A Pending CN113860319A (en) 2021-09-23 2021-09-23 Zircon sand production method

Country Status (1)

Country Link
CN (1) CN113860319A (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1070625A (en) * 1991-11-05 1993-04-07 徐振江 The method of purifying zirconium (hafnium) silicate zirconium (hafnium)
US20070148066A1 (en) * 2003-10-28 2007-06-28 Horta Ronaldo D M Process to obtain titanium concentrates with high contents of tio2 and low contents of radionuclide elements from anatase mechanical concentrates
CN101717260A (en) * 2009-12-07 2010-06-02 浙江工业大学 Method for pickling and whitening feldspar powder
CN105502423A (en) * 2016-01-28 2016-04-20 郭志斌 Method for producing high-grade zircon sand
US20160326009A1 (en) * 2014-01-16 2016-11-10 Daiichi Kigenso Kagaku Kogyo Co., Ltd. Method for producing aqueous zirconium chloride solution
CN109336116A (en) * 2018-10-31 2019-02-15 黄冈师范学院 A method of photovoltaic high purity quartz emery dust is prepared containing feldspar ore type quartzite

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1070625A (en) * 1991-11-05 1993-04-07 徐振江 The method of purifying zirconium (hafnium) silicate zirconium (hafnium)
US20070148066A1 (en) * 2003-10-28 2007-06-28 Horta Ronaldo D M Process to obtain titanium concentrates with high contents of tio2 and low contents of radionuclide elements from anatase mechanical concentrates
CN101717260A (en) * 2009-12-07 2010-06-02 浙江工业大学 Method for pickling and whitening feldspar powder
US20160326009A1 (en) * 2014-01-16 2016-11-10 Daiichi Kigenso Kagaku Kogyo Co., Ltd. Method for producing aqueous zirconium chloride solution
CN105502423A (en) * 2016-01-28 2016-04-20 郭志斌 Method for producing high-grade zircon sand
CN109336116A (en) * 2018-10-31 2019-02-15 黄冈师范学院 A method of photovoltaic high purity quartz emery dust is prepared containing feldspar ore type quartzite

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
邝国春等: "锆英石精矿制取高纯度锆英石微粉过程中的净化除铁研究", 《江西有色金属》 *

Similar Documents

Publication Publication Date Title
CN100500893C (en) Copper cobalt alloy separation and recovery method
CN103030175B (en) Device and method applied to metatitanic acid washing room
CN103043714B (en) Tubular membrane device applicable to titanium dioxide washing and washing method
CN101475172A (en) Recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder
CN1244498C (en) Manufacture of high grade artificial rutile from low grade primary greporite
CN112708786A (en) Method for recycling scandium from aluminum-scandium alloy target material waste
CN109467123A (en) A kind of artificial rutile mether liquor comprehensive resource utilizes method
CN102424418A (en) Method for continuous filtration washing of hydrated titanium dioxide
CN107022681A (en) A kind of comprehensive recovering process of aluminium scrap silicon middle rare earth, aluminium and silicon
CN86108511A (en) Produce the method for titanium dioxide with the titaniferous iron-smelting blast-furnace slag
CN106011466A (en) Method for improving copper slag level in zinc hydrometallurgy process
CN101457301A (en) Technique for extracting cobalt from alpha-nitroso beta-naphthyl hydroxide cobalt slag
CN101328542B (en) Method for directly preparing copper sulfate and cathode copper from copper ore concentrate
CN201250267Y (en) Purification system for gold ore concentrate cinder acid leaching solution
CN106542506A (en) A kind of method that selenium is reclaimed from heavy tellurium waste liquid
CN104876362B (en) Acid purification recycling system
CN214864341U (en) Wet preparation production line of high-purity quartz sand
CN105385853B (en) A kind of cupric gives up the processing method of magnesia brick
CN103194621A (en) Method for treating sulfur slag
CN106893859B (en) A method of processing nickel cobalt waste material
CN113860319A (en) Zircon sand production method
CN105483378B (en) A kind of method for making fluorine in white residue removing solution of zinc sulfate by oneself
CN101683998A (en) One-step production method for cerium poor rare earth fluoride and cerium fluoride
CN85104036A (en) Directly produce the production method of sodium stannate from the tin concentrate
CN211570321U (en) Copper separation system of high acidity copper-containing waste liquid of strong oxidation

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination