CN114804129A - Method for purifying high-purity quartz sand - Google Patents

Method for purifying high-purity quartz sand Download PDF

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Publication number
CN114804129A
CN114804129A CN202210496202.4A CN202210496202A CN114804129A CN 114804129 A CN114804129 A CN 114804129A CN 202210496202 A CN202210496202 A CN 202210496202A CN 114804129 A CN114804129 A CN 114804129A
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China
Prior art keywords
quartz sand
reaction kettle
acid
water
stirring
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CN202210496202.4A
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Chinese (zh)
Inventor
任其广
肖华
刘宝
孙国峰
何君君
张思旗
钟媛
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Jiangsu Hengxin Quartz Technology Co ltd
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Jiangsu Hengxin Quartz Technology Co ltd
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Priority to CN202210496202.4A priority Critical patent/CN114804129A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof

Abstract

The invention relates to a method for purifying high-purity quartz sand, which comprises the following steps: s1, scrubbing, namely putting quartz sand and pure water into the reaction kettle in proportion, stirring, scrubbing for many times, and discharging sewage until the water is clear; s2, performing flotation, namely adding warm water, a flotation reagent and a foaming agent into quartz sand to form ore pulp, stirring, continuously introducing compressed air into the quartz sand to form foam on the surface of the ore pulp, and removing the foam; s3, cleaning, namely adding hot pure water into the quartz sand subjected to flotation, and discharging the cleaned quartz sand; s4, acid washing, namely adding mixed acid to immerse the quartz sand, sealing the reaction kettle, introducing high-temperature steam into the quartz sand, keeping stirring continuously, and discharging waste liquid after acid washing; and S5, acid washing, namely adding pure water into the reaction kettle for acid washing, washing for many times until the detection is qualified, and discharging the quartz sand. According to the invention, the purification of the quartz sand is completed in the same reaction kettle, so that secondary pollution caused by multiple purification processes in material transfer is avoided, and the purity of the quartz sand is improved.

Description

Method for purifying high-purity quartz sand
Technical Field
The invention relates to the technical field related to quartz sand production, in particular to a high-purity quartz sand purification method.
Background
Quartz is a non-metallic mineral and has the characteristics of hardness, wear resistance, stable chemical properties and the like. The quartz sand is quartz particles formed by crushing and processing quartz stone, is an important industrial mineral raw material, and is widely used in the industrial fields of glass, casting, ceramics and fireproof materials, ferrosilicon smelting, metallurgical fusing agents, metallurgy, building, chemical industry, plastics, rubber, grinding materials, filter materials and the like.
In order to improve the purity of the quartz sand, a purification process is required. In the purification process of high-purity quartz, flotation is mainly used for removing mica and feldspar minerals which are symbiotic with the quartz, and also can be used for floating minerals containing phosphorus and iron, and acid washing can effectively remove metal impurities such as Fe, Al, Mg and the like. The flotation and acid washing are key processes in the whole purification process, the requirements on equipment are extremely strict, and materials have the advantages of corrosion resistance, wear resistance, resistance to the temperature of about 100 ℃, no pollution and safety in work.
In the prior art, flotation and pickling equipment are mutually independent, certain requirements are set for space requirements and material turnover of a factory building, pollution can be caused to materials per se in the material turnover process, and certain loss exists, so that the quality of quartz produced by flotation and pickling is reduced, and the production efficiency is influenced.
Disclosure of Invention
Therefore, the invention aims to solve the technical problem of overcoming the defect that the flotation and acid washing process of quartz sand in the prior art generates secondary pollution to materials in the material turnover process; the method for purifying the high-purity quartz sand is designed, the flotation and acid washing processes of the quartz sand can be completed in the same device, the purification cost is reduced, and the purity of the quartz sand is improved.
In order to solve the technical problem, the invention provides a method for purifying high-purity quartz sand, which comprises the following steps:
s1, scrubbing, namely putting quartz sand and pure water into the reaction kettle in proportion, stirring, scrubbing for many times, and discharging sewage until the water is clear;
s2, performing flotation, namely adding warm water, a flotation reagent and a foaming agent into quartz sand to form ore pulp, stirring, continuously introducing compressed air into the quartz sand to form foam on the surface of the ore pulp, and removing the foam;
s3, cleaning, namely adding hot pure water into the quartz sand subjected to flotation, and discharging the cleaned quartz sand;
s4, acid washing, namely adding mixed acid to immerse the quartz sand, sealing the reaction kettle, introducing high-temperature steam into the quartz sand, keeping stirring continuously, and discharging waste liquid after acid washing;
and S5, acid washing, namely adding pure water into the reaction kettle for acid washing, washing for many times until the detection is qualified, and discharging the quartz sand.
In one embodiment of the present invention, in step S1, the mass ratio of the silica sand to the water is 35 to 45%.
In one embodiment of the present invention, in step S2, the specific operation steps of the flotation are as follows;
s21, adding warm water of 40-50 degrees into the reaction kettle, adding a flotation reagent and a foaming agent, and stirring at a high speed for 10 minutes to enable the flotation reagent and the foaming agent to fully react with the quartz sand;
s22, introducing compressed air to the bottom of the reaction kettle, stirring at a high speed to break up the compressed air into small bubbles, and forming a large amount of foam under the action of a foaming agent;
and S23, scraping the foam suspended on the surface of the ore pulp out of the reaction kettle.
In one embodiment of the invention, the flotation reagent is cationic collector diamine and anionic collector sulfonate, the concentration ratio of the cationic collector diamine is 100g/t-220g/t, the concentration ratio of the anionic collector sulfonate is 250g/t-350g/t, and the concentration ratio of the foaming agent is 10g/t-70 g/t.
In an embodiment of the present invention, in step S4, the specific steps of acid washing are as follows:
s41, adding the mixed acid into the reaction kettle according to the set concentration ratio, and sealing the feeding port;
s42, introducing steam into the bottom of the reaction kettle, and stirring at a medium speed to ensure that the high-temperature steam is completely contacted with the quartz sand;
s43, controlling the pickling time to be 2-3h, then stopping stirring, closing high-temperature steam, simultaneously opening a pressure release valve, and discharging the acid water after reaction until the quartz sand is completely precipitated.
In one embodiment of the invention, the mixed acid is a mixture comprising hydrofluoric acid with a mass concentration of 7% -10%, sulfuric acid with a mass concentration of 15% -20%, hydrochloric acid with a mass concentration of 10% -15% and nitric acid with a mass concentration of 5% -8%.
In an embodiment of the present invention, in step S5, the specific steps of acid washing are as follows:
s51, adding pure water into the reaction kettle, stirring at a low speed for 10 minutes, and discharging the water;
s52, repeating the steps, and detecting the pH value and the conductivity of the discharged water while discharging water until the pH value is 6.5-7 and the conductivity is less than or equal to 5 mu S/cm;
and S53, flushing the quartz sand out of the discharge hole by pure water, and sampling and detecting.
In one embodiment of the invention, the inner wall of the reaction kettle is provided with a protective layer, and the material of the protective layer is PP or PE.
A quartz sand purification device adopts the high-purity quartz sand purification method.
Compared with the prior art, the technical scheme of the invention has the following advantages:
the invention discloses a high-purity quartz sand purification method, which comprises the steps of scrubbing, flotation, cleaning, acid washing and acid washing, wherein the steps are all finished in the same reaction kettle, and the quartz sand with high purity is obtained. The invention can complete the purification process without material transportation, thereby avoiding secondary pollution caused by material transportation in the purification process of quartz sand, reducing loss, improving the purity and yield of quartz sand and improving production efficiency.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the embodiments of the present disclosure taken in conjunction with the accompanying drawings, in which
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a process flow diagram of flotation in FIG. 1;
FIG. 3 is a process flow diagram of the acid wash of FIG. 1;
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Referring to fig. 1, the invention discloses a method for purifying high-purity quartz sand, which comprises the following steps:
s1, scrubbing, namely putting quartz sand and pure water into a reaction kettle according to a certain proportion, stirring, scrubbing for many times, and discharging sewage until the water is clear;
mineral impurities and dust exist on the surface of the quartz sand which just enters the reaction kettle, the quartz sand particles are rubbed with each other by adding water and stirring, the dust on the surface is scrubbed out, and the quartz sand is stirred for a plurality of times until the water is clear, so that the surface of the quartz sand is scrubbed clean. Specifically, in order to ensure the scrubbing effect, the mass ratio of the quartz sand to the water is 35-45%, ore pulp with a certain concentration is formed, and the surface of the quartz sand is fully contacted with the water, so that the scrubbing effect is facilitated.
S2, performing flotation, namely adding warm water, a flotation reagent and a foaming agent into quartz sand to form ore pulp, starting stirring, continuously introducing compressed air into the quartz sand, forming foams on the surface of the quartz sand, and removing the foams;
the purpose of the warm water added here is to provide a gentle environment for the flotation and frother agents and to increase the reaction rate between the flotation and frother agents and the silica sand. The flotation reagent, the foaming agent and the quartz sand are fully stirred to react with mineral impurities such as iron, feldspar, mica and the like in the quartz sand, at the moment, compressed air is introduced into the quartz sand, a large number of bubbles are generated in the stirring process, the bubbles can adsorb the reacted mineral impurities, and finally the bubbles can form foams at the top of ore pulp, and the foams are removed in time, so that the mineral impurities can be effectively removed; it is noted that the entire flotation process is carried out in an open environment.
S3, cleaning, namely adding hot pure water into the quartz sand after flotation, wherein the hot water is high in temperature, the water molecules are faster in movement speed and more hydrophilic, and can be easily diffused into the oil stain to be melted, the hot water is high in temperature and can dissolve solid oil stain, the hot water increases hydrophilic groups in the oil stain and can not be attached to the quartz sand, oily substances attached to the surface of the quartz sand can be effectively washed away, clean quartz sand is obtained, and meanwhile, clear water is discharged;
s4, acid washing, namely adding mixed acid to immerse the quartz sand, sealing the reaction kettle, introducing high-temperature steam into the quartz sand, keeping stirring continuously, and discharging waste liquid after acid washing;
the step is the key of quartz sand purification, and iron oxide, other oxides and acid-soluble mineral impurities in the quartz sand are removed through a plurality of mixed acids. The quartz products have different requirements for the mineral impurity content of the quartz sand, such as iron, aluminum, titanium, lithium and the like. In particular, the requirement on the content of iron is particularly strict for quartz sand for glass; high-temperature steam is introduced into the reaction kettle to provide a high-temperature and high-pressure environment, so that the pickling process can be accelerated, and the reaction rate can be increased. It should be noted that the reaction kettle needs to be sealed in the actual pickling process.
And S5, acid washing, namely adding pure water into the reaction kettle for acid washing in order to remove acid remained in the reaction kettle until the detection data reach the standard, and finally discharging the quartz sand.
Further, the specific operation of step S2 is as follows:
in order to ensure the maximum reaction rate of the flotation reagent and the foaming agent, in step S21, adding warm water of 40-50 ℃ into a reaction kettle; stirring at high speed, controlling the time to be 10 minutes, fully reacting the flotation reagent and the foaming agent with the quartz sand, and screening out mineral impurities.
In order to ensure that the quartz sand can fully react with the flotation reagent and the foaming agent, in step S22, compressed air is introduced to the bottom of the reaction kettle, and is stirred at a high speed to scatter the compressed air into small bubbles, so that the compressed air exists between the quartz sand and the quartz sand in the form of bubbles, and simultaneously a large amount of foams are formed under the action of the foaming agent, and the bubbles adsorb the floated mineral impurities.
Finally, in step S23, the foam brings the floated mineral impurities to the surface of the quartz sand, and the foam suspended on the surface of the ore slurry is scraped out of the reaction kettle by the scraper at the feed inlet, so as to remove the floated mineral impurities in time.
According to the preferable scheme, the flotation reagent is cationic collector diamine and anionic collector sulfonate, the concentration ratio of the cationic collector diamine is 100g/t-220g/t, the concentration ratio of the anionic collector sulfonate is 250g/t-350g/t, and the concentration ratio of the foaming agent is 10g/t-70 g/t.
Further, the specific operation steps of step S4 are as follows:
in step S41, first, a mixed acid solution is prepared according to a set concentration ratio, and the mixed acid is added into a reaction kettle, wherein it is noted that after the mixed acid is added, a feeding port needs to be sealed;
in order to ensure the pickling effect, in step S42, steam is introduced into the bottom of the reaction kettle to provide a high-temperature and high-pressure reaction environment for pickling, so as to increase the reaction rate; simultaneously, stirring the quartz sand at a medium speed to ensure that the introduced high-temperature steam is in complete contact with the quartz sand;
and finally, controlling the pickling time to be 2-3h by step S43, so that the mixed acid in the reaction kettle and the quartz sand fully react. And then stopping stirring, closing steam, simultaneously opening a pressure relief valve, recovering the pressure in the reaction kettle, and discharging the acid water after the reaction after the quartz sand is completely precipitated. It should be noted that the acid liquid is collected and processed uniformly.
Further, the mixed acid is a mixture comprising 7-10% of hydrofluoric acid, 15-20% of sulfuric acid, 10-15% of hydrochloric acid and 5-8% of nitric acid by mass concentration. One or more acids may be selected for pickling, as desired.
Further, in step S5, the specific steps of acid washing are as follows:
the purpose of acid washing is to remove acid liquor remained in the reaction kettle and discharge other ions in the acid liquor so as to improve the purity of the quartz sand. Firstly, adding pure water into a reaction kettle, stirring at a low speed for 10 minutes, discharging water to dilute the residual acid liquid by the pure water, and discharging the acid liquid out of the reaction kettle along with the water.
Repeating the above steps, and detecting pH value and conductivity of the discharged water while discharging water, wherein the pH value is detected to be 6.5-7 and is close to neutral as a standard for acid washing completion. Secondly, the conductivity is high due to the large ion concentration in the acid solution, and therefore, the conductivity is also a standard for completing acid washing, and in the invention, the conductivity is less than or equal to 5 muS/cm.
Finally, continuously let in the pure water in the reation kettle, wash out the quartz sand from the discharge gate through the pure water to sample detection, the detection index should be in the purity requirement scope, promptly: total impurity element content: less than 50ppm, the purity is more than 99.99 percent, the final purity is more than or equal to 99.998 percent after the high-temperature chlorination purification process, and the design purpose and the requirement of a high-efficiency purification device of the high-purity quartz sand are achieved.
Furthermore, in order to ensure the purity of the quartz sand, a protective layer is arranged on the inner wall of the whole reaction kettle, so that the influence of other factors on the purity of the quartz sand is prevented. As a preferred scheme, the material of the protective layer is PP or PE, has good corrosion resistance, and cannot react with various reagents in the purification process.
A quartz sand purification device adopts the high-purity quartz sand purification method.
In conclusion, the invention discloses a purification method of quartz sand, which can realize the steps of scrubbing, flotation, cleaning, acid washing and acid washing in the same reaction kettle and can obtain the quartz sand with higher purity. The method solves the problem of secondary pollution caused by the need of transferring a plurality of operation steps in the purification process of the quartz sand. And simultaneously, the production efficiency of purification can be improved.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (9)

1. The method for purifying the high-purity quartz sand is characterized by comprising the following steps of:
s1, scrubbing, namely putting quartz sand and pure water into the reaction kettle in proportion, stirring, scrubbing for many times, and discharging sewage until the water is clear;
s2, performing flotation, namely adding warm water, a flotation reagent and a foaming agent into quartz sand to form ore pulp, stirring, continuously introducing compressed air into the quartz sand to form foam on the surface of the ore pulp, and removing the foam;
s3, cleaning, namely adding hot pure water into the quartz sand subjected to flotation, and discharging the cleaned quartz sand;
s4, acid washing, namely adding mixed acid to immerse the quartz sand, sealing the reaction kettle, introducing high-temperature steam into the quartz sand, keeping stirring continuously, and discharging waste liquid after acid washing;
and S5, acid washing, namely adding pure water into the reaction kettle for acid washing, washing for many times until the detection is qualified, and discharging the quartz sand.
2. The method for purifying high-purity quartz sand according to claim 1, wherein: in step S1, the mass ratio of the silica sand to the water is 35 to 45%.
3. The method for purifying high-purity quartz sand according to claim 1, wherein: in step S2, the specific operation steps of the flotation are as follows;
s21, adding warm water of 40-50 degrees into the reaction kettle, adding a flotation reagent and a foaming agent, and stirring at a high speed for 10 minutes to enable the flotation reagent and the foaming agent to fully react with the quartz sand;
s22, introducing compressed air to the bottom of the reaction kettle, stirring at a high speed to break up the compressed air into small bubbles, and forming a large amount of foam under the action of a foaming agent;
and S23, scraping the foam suspended on the surface of the ore pulp out of the reaction kettle.
4. The method of purifying high purity quartz sand according to claim 3, wherein: the flotation reagent is composed of cationic collector diamine and anionic collector sulfonate, the concentration ratio of the cationic collector diamine is 100g/t-220g/t, the concentration ratio of the anionic collector sulfonate is 250g/t-350g/t, and the concentration ratio of the foaming agent is 10g/t-70 g/t.
5. The method for purifying high-purity quartz sand according to claim 1, wherein: in step S4, the pickling specifically includes the following steps:
s41, adding the mixed acid into the reaction kettle according to the set concentration ratio, and sealing the feeding port;
s42, introducing steam into the bottom of the reaction kettle, and stirring at a medium speed to ensure that the high-temperature steam is completely contacted with the quartz sand;
s43, controlling the pickling time to be 2-3h, then stopping stirring, closing high-temperature steam, simultaneously opening a pressure release valve, and discharging the reacted acid water after the quartz sand is completely precipitated.
6. The method for purifying high-purity quartz sand according to claim 5, wherein: the mixed acid is a mixture comprising 7-10% of hydrofluoric acid, 15-20% of sulfuric acid, 10-15% of hydrochloric acid and 5-8% of nitric acid by mass concentration.
7. The method for purifying high-purity quartz sand according to claim 1, wherein: in step S5, the acid washing specifically includes the following steps:
s51, adding pure water into the reaction kettle, stirring at a low speed for 10 minutes, and discharging the water;
s52, repeating the steps, and detecting the pH value and the conductivity of the discharged water while discharging water until the pH value is 6.5-7 and the conductivity is less than or equal to 5 mu S/cm;
and S53, flushing the quartz sand out of the discharge hole by pure water, and sampling and detecting.
8. The method for purifying high-purity quartz sand according to claim 1, wherein: the inner wall of the reaction kettle is provided with a protective layer, and the protective layer is made of PP or PE.
9. A purification apparatus of silica sand, which adopts the purification method of high purity silica sand according to any one of claims 1 to 8.
CN202210496202.4A 2022-04-29 2022-04-29 Method for purifying high-purity quartz sand Pending CN114804129A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116119676A (en) * 2023-04-17 2023-05-16 力丰硅科技(天津)有限公司 Integrated process method and device for series three-phase flow pickling high-purity quartz sand

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104340981A (en) * 2013-08-09 2015-02-11 新沂市中大石英科技有限公司 Preparation method for high-purity quartz sand
CN110127708A (en) * 2019-05-01 2019-08-16 黄冈师范学院 A kind of SiO2Purity >=99.99% glass sand method of purification
CN114392836A (en) * 2021-12-16 2022-04-26 江苏中腾石英材料科技股份有限公司 Processing technology of high-purity quartz sand

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104340981A (en) * 2013-08-09 2015-02-11 新沂市中大石英科技有限公司 Preparation method for high-purity quartz sand
CN110127708A (en) * 2019-05-01 2019-08-16 黄冈师范学院 A kind of SiO2Purity >=99.99% glass sand method of purification
CN114392836A (en) * 2021-12-16 2022-04-26 江苏中腾石英材料科技股份有限公司 Processing technology of high-purity quartz sand

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116119676A (en) * 2023-04-17 2023-05-16 力丰硅科技(天津)有限公司 Integrated process method and device for series three-phase flow pickling high-purity quartz sand
CN116119676B (en) * 2023-04-17 2023-06-23 力丰硅科技(天津)有限公司 Integrated process method and device for series three-phase flow pickling high-purity quartz sand

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