CN110436468A - A kind of improved method of pickling high-purity quartz sand purifying technique - Google Patents
A kind of improved method of pickling high-purity quartz sand purifying technique Download PDFInfo
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- CN110436468A CN110436468A CN201910802543.8A CN201910802543A CN110436468A CN 110436468 A CN110436468 A CN 110436468A CN 201910802543 A CN201910802543 A CN 201910802543A CN 110436468 A CN110436468 A CN 110436468A
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- quartz sand
- reaction kettle
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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
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention relates to a kind of improved methods of pickling high-purity quartz sand purifying technique, belong to electron-optical quartz glass field.The present invention is by being improved to polytetrafluoroethylene material by polyethylene for the inner-wall material of bipyramid reaction kettle, can also allow while acid-fast alkali-proof acid cleaning process of the invention 100 DEG C or more at a temperature of carry out, fully open the lattice system of quartz sand, gasify the technical hydrochloric acid of use to form HCl gas in combination with high temperature, metal salt is generated into reacting in the lattice of quartz sand with impurity component, it can further be dissolved in the water of cleaning, to improve the purity of quartz sand after pickling for the impurity phased soln inside quartz sand；Simultaneously because having only with technical hydrochloric acid and saving raw material, reduce with sour amount, pollution abatement, improve pickling effect, the purpose that waste water control is recycled.
Description
Technical field
The invention belongs to electron-optical quartz glass fields, and in particular to a kind of pickling high-purity quartz sand purifying technique changes
Into method.
Background technique
Quartz glass is new and high technology material, the quartz glass crucibles as used in semi-conductor industry, Novel electric light source glass
Glass shell, communication silicon fiber etc.；Quartz glass has become modern science technology and present chemical industry is indispensable heavy
Want material.The development of quartz glass technology, it has also become a new disciplines field of new and high technology material, and original used in quartz glass
Material is glass sand, and chemical analysis is very pure SiO2, and the technology for extracting glass sand is passed through by raw ore
Cross hand picking, high-temperature water quenching, sand processed, magnetic separation, flotation, pickling, chlorination processing, superconducting magnetic separation, electric separation, high-temperature vacuum processing,
New and high technology means, the purposes such as ultrasonication, doping purification, rectification and purification are all sought in every way to and are removed contained by quartz
Impurity and gas liquid inclusion, and the acid cleaning process in the prior art of quartz sand purifying is a kind of essential work of impurity elimination purification
Process, i.e. pickling are one of the essential important procedures of quartz glass sandy plain material purifying technique, and main function is
Except some metal chlorides and part silicate mineral for being dissolved in acid.Acid cleaning process is divided to static pickling and dynamic pickling two kinds of sides
Method: static pickling is put into quartz sand in acidproof plastic containers, with HCL, HNO3, HF composition mixed liquid dipping, according to
Weather conditions determine soaking time, are at least also required to 5-7 days；And dynamic pickling is that quartz sand is put into dynamic acid-resistant reacting kettle
It is interior, HCL, HNO is added3, HF three acid proportions after saturated solution in carry out pickling, quartz sand per ton about need 600-800 kilograms it is mixed
Acid solution is closed, reaction kettle passes through 55-60 DEG C of heating, operates (interior band stirring or biconial) using two kinds of modes, makes entire anti-
Quartz sand dynamically rolls in reaction kettle when answering kettle spinning motion, to reach the uniform purpose of acidification.
With the progress of science and technology, reaction kettle heating dynamic process is changed by original cabinet natural temperature leaching method
Technology can substantially reduce the pickling reaction time, to achieve the purpose that quality is stable；But reaction kettle inner wall is acidproof at present
Material is vinyon, can be adhered to reaction kettle inner wall by heating rotational moulding, and due to the temperature tolerance of vinyon by
Certain limitation causes the temperature during heating acid-washed quartz sand can only be between 50-60 DEG C, and quartz sand is in above-mentioned temperature
When spending in boundary, lattice system is also completely in closed state, so the acid cleaning process of kind mode can only remove quartz
The impurity on sand surface, and a large amount of harmful elements remaining in lattice system not can be removed still；In addition it is saturated pickling technology
Recovered liquid contain a large amount of harmful substances, reusing 1-2 time can also be such that pickling effect substantially reduces later, will ultimately result in nothing
The generation of a large amount of tails acid, waste liquid that method uses, needs to discharge using neutralisation treatment, but this tail acid waste liquid is that three acid-mixeds are closed
Body, CL-、F-、NO3 -Equal compositions are considerably complicated, are extremely difficult to discharge standard, will cause serious environmental pollution.
In view of above-mentioned technical method, tradition saturation acid cleaning process will saturation pickling tail acid discharge after the completion of quartz sand acid is washed
Storage, and still remaining has a large amount of tail acid that cannot be discharged in quartz sand, the tail acid remained in quartz sand is up to 2 percent
15 to 30, at this moment can only using plus water filtering clean repeatedly, a large amount of tail acid waste water enter in treatment tank need into
Row neutralisation treatment.
Therefore traditional saturation pickling processing compound contains a large amount of HF, and HF is exactly SiO2Jinx, the two meets
SiO2It will dissolve, dissolved substance is H2SiF6If quartz sand will be generated when pure water cleaning is not exclusively thorough
Micro H2SiF6Superfine powder will generate a large amount of microbubble when producing silica crucible, quartzy heavy stone used as an anchor, gas and refining quartzy trombone slide,
Keep the decline of its quality or quality technology unqualified, this is also glass sand generated gas-liquid package in process
One of the reason of body.
It can be seen that needing to improve existing quartz sand acid cleaning process, the purity of quartz sand after raising processing, together
When reduce tail acid waste water generation, avoid serious environmental pollution.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of improved methods of pickling high-purity quartz sand purifying technique.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, a kind of improved method of pickling high-purity quartz sand purifying technique, described method includes following steps:
(1) the bipyramid reaction kettle that polytetrafluoroethylene material is inner-wall material is chosen, is added according to the weight ratio of 100:7~10
Quartz sand and technical hydrochloric acid；
(2) the bipyramid reaction kettle is warming up to 100~120 DEG C, the reaction kettle internal temperature is protected at 100 DEG C or more
Temperature 4~6 hours, while the reaction kettle being kept to be in operating mixing；
(3) water that temperature is 65 DEG C or more, operating cleaning stone is added after heat preservation terminates in step (2) into the reaction kettle
Sand 30min stops heating after cleaning, exclude cleaning waste liquid, repeat to clean, glass sand can be obtained.
Preferably, the drain tap for heating up described in step (2) and opening the reaction kettle in the insulating process, makes to produce
Raw exhaust gas is neutralized by waste gas recovery tower.
Preferably, the revolving speed when operating is 18~22 turns/mim.
Preferably, the volume mass ratio of water described in step (3) and quartz sand described in step (1) is 2:1.
Preferably, cleaning waste liquid described in step (3) uses high-pressure pump intensifier discharge in exclusion process.
Preferably, the time cleaned every time in step (3) is 30min.
Preferably, the processing method of waste liquid is cleaned described in step (3) are as follows: CaO is added into the cleaning waste liquid and carries out
Neutralisation treatment settles CaCl2After filter, the water that can be recycled.
The beneficial effects of the present invention are: the invention discloses a kind of improved pickling high-purity quartz sand method of purification, phases
Than for existing acid cleaning process, having the advantage that inner-wall material is polytetrafluoroethylene (PTFE) in the bipyramid reaction kettle 1. used
Material, this material not only resistance to various strong acid, and operating temperature can be up to 120 DEG C, this is conducive to improve quartz sand in acid cleaning process
In temperature, so that the lattice system of quartz sand is completely in open state, be conducive in acid cleaning process acid solution and immerse quartz crystal lattice
Inside system, by internal impurity phased soln, the purity of quartz sand after pickling is improved；2. only with technical hydrochloric acid in acid cleaning process
As pickled material, almost SiO can be removed with all2Outer impurity reacts, and ensures stone while can do purifying quartz sand
Sand crystal is not damaged；3. reaction kettle is warming up to 100~120 DEG C in acid cleaning process, it is greater than the actual temperature of reaction kettle
100 DEG C, quartz sand is in soft fluffy state in reaction kettle at this time, and lattice system will generate expansion, and quartz sand, which will generate, to be split
Line, and the HCl in reaction kettle is become HCl gas from liquid by high temperature action, can enter quartz sand intracell and be followed
Vigorous reaction occurs for ring, the impurity trace element Al included with quartz sand, Ca, Cu, Fe, K, Li, Na, Cr, Mn, Ti etc., thus
The a large amount of impurity element contained in solid quartz sand inclusion enclave can be removed, i.e., method of the invention utilizes differential expansion coefficient
Variation, so that the impurity in quartz sand is sufficiently exposed, be sufficiently submerged in HCl gas inside quartz crystal lattice system and harmful element
It reacts, achievees the purpose that purifying quartz sand；4. the present invention is only with technical hydrochloric acid as in pickled material, with quartz sand
Almost all generates metal chloride after impurity element reaction, on the basis of carrying out the quartz sand after cleaning pickling using pure water
It can be dissolved in aqueous solution, be excluded in the form of waste water, be easy to be neutralized, environmental pollution caused by reducing.
Other advantages, target and feature of the invention will be illustrated in the following description to a certain extent, and
And to a certain extent, based on will be apparent to those skilled in the art to investigating hereafter, Huo Zheke
To be instructed from the practice of the present invention.Target of the invention and other advantages can be realized by following specification and
It obtains.
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Purification processes are carried out according to different methods to the preferable suprasil mine of In A Certain Place of Xinjiang quality:
Embodiment 1
(1) the bipyramid reaction kettle that polytetrafluoroethylene material is inner-wall material is chosen, is added according to the weight ratio of 100:10 former
Pit wood material and technical hydrochloric acid；
(2) bipyramid reaction kettle is warming up to 120 DEG C according to natural rate, reaction kettle internal temperature is made to reach 100 DEG C or more
Shi Jinhang keeps the temperature 4 hours, keeps the reaction kettle to be in operating condition during reaction kettle heats up and keeps the temperature, revolving speed is
18-22 turns/mim. is sufficiently mixed the HCl of reaction kettle class with quartz sand, opens simultaneously the drain tap of reaction kettle, makes to process
The exhaust gas generated in journey enters waste gas recovery tower after excluding, then is neutralized；
(3) 65 DEG C or more of pure water is added after heat preservation terminates into reaction kettle (to add in the water being wherein added and step (1)
The volume mass ratio of the quartz sand entered is water sand 2:1, ml:g), with the rotation speed operation reaction kettle of 18~22 turns/mim, cleaning reaction
Quartz sand 30min in kettle stops heating after cleaning, excluded cleaning waste liquid by the way of high-pressure pump intensifier discharge
It loses no time, repeats cleaning 2 times, glass sand can be obtained；
(4) CaO is added into the cleaning waste liquid of exclusion, can settles to form CaCl2, obtained after filtering more pure
Water is applied to the cleaning process after pickling again, achievees the purpose that recycle.
Embodiment 2
(1) the bipyramid reaction kettle that polytetrafluoroethylene material is inner-wall material is chosen, raw ore is added according to the weight ratio of 100:7
Material and technical hydrochloric acid；
(2) bipyramid reaction kettle is warming up to 120 DEG C according to natural rate, make reaction kettle internal temperature reach 100 DEG C with
Heat preservation 6 hours was carried out when upper, kept the reaction kettle to be in operating condition, revolving speed during reaction kettle heats up and keeps the temperature
It for 18~22 turns/mim, is sufficiently mixed the HCl of reaction kettle class with quartz sand, opens simultaneously the drain tap of reaction kettle, make to locate
The exhaust gas generated during reason enters waste gas recovery tower after excluding, then is neutralized；
(3) 65 DEG C or more of pure water is added after heat preservation terminates into reaction kettle (to add in the water being wherein added and step (1)
The volume mass ratio of the quartz sand entered is water sand 2:1, ml:g), with the rotation speed operation reaction kettle of 18~22 turns/mim, cleaning reaction
Quartz sand 30min in kettle stops heating after cleaning, excluded cleaning waste liquid by the way of high-pressure pump intensifier discharge
It loses no time, repeats cleaning 3 times, glass sand can be obtained；
(4) CaO is added into the cleaning waste liquid of exclusion, can settles to form CaCl2, obtained after filtering more pure
Water is applied to the cleaning process after pickling again, achievees the purpose that recycle.
Embodiment 3
(1) the bipyramid reaction kettle that polytetrafluoroethylene material is inner-wall material is chosen, raw ore is added according to the weight ratio of 100:8
Material and technical hydrochloric acid；
(2) bipyramid reaction kettle is warming up to 120 DEG C according to natural rate, make reaction kettle internal temperature reach 100 DEG C with
Heat preservation 5 hours was carried out when upper, kept the reaction kettle to be in operating condition, revolving speed during reaction kettle heats up and keeps the temperature
It for 18~22 turns/mim, is sufficiently mixed the HCl of reaction kettle class with quartz sand, opens simultaneously the drain tap of reaction kettle, make to locate
The exhaust gas generated during reason enters waste gas recovery tower after excluding, then is neutralized；
(3) 65 DEG C or more of pure water is added after heat preservation terminates into reaction kettle (to add in the water being wherein added and step (1)
The volume mass ratio of the quartz sand entered is water constituents 2:1, ml:g), with the rotation speed operation reaction kettle of 18~22 turns/mim, cleaning is anti-
The quartz sand 30min in kettle is answered, stops heating after cleaning, it will cleaning waste liquid row by the way of high-pressure pump intensifier discharge
Except losing no time, repeats cleaning 3 times, glass sand can be obtained；
(4) CaO is added into the cleaning waste liquid of exclusion, can settles to form CaCl2, obtained after filtering more pure
Water is applied to the cleaning process after pickling again, achievees the purpose that recycle.
Comparative example 1
Raw ore material passes through ore hand sorting early period, high-temperature water quenching, sand processed, 50~150 mesh of sub-sieve, and magnetic separation removes process
In machinery iron, after then being reacted 5~7 days using three acid unification plastics acid-resistant container static state pickling of tradition, using flotation, pure
Water purification cleaning, dehydration, drying, obtain glass sand greater than after the techniques such as 13000 Gauss electromagnetic separations and electric separation.
Comparative example 2
Raw ore material passes through ore hand sorting early period, high-temperature water quenching, sand processed, 50~150 mesh of sub-sieve, and magnetic separation removes process
In machinery iron, then heated after 50-60 DEG C of pickling react 5~7 days using three acid unification reaction kettles of saturation, using flotation,
Pure water cleaning, dehydration, drying, greater than after the techniques such as 13000 Gauss electromagnetic separations and electric separation obtain glass sand (.
Analyze the content of 13 kinds of elements in the finished product glass sand obtained by distinct methods, analysis analysis result
As shown in table 1.
The content (ppm) of impurity element in 1 raw ore material of table and the quartz sand obtained after being handled according to distinct methods
The comparison of impurity content in glass sand obtained in pickling processes method by the above distinct methods, can be with
Obtain by method of purification improved in invention, compared with the prior art for, containing for impurity in quartz sand can actually be reduced
Amount, obtains the higher quartz sand of purity.
In addition become single HCl acid-washed quartz sand from three traditional acid unifications in improved method of the invention, satisfied by tradition
It is improved to the half-dried bored method acid washing method of a small amount of HCl with pickling, is had and is saved raw material, reduce with sour amount, pollution abatement, improve acid
Wash effect, the purpose that waste water control is recycled.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of the technical program, should all be covered in the present invention
Scope of the claims in.
Claims (7)
1. a kind of improved method of pickling high-purity quartz sand purifying technique, which is characterized in that described method includes following steps:
(1) the bipyramid reaction kettle that polytetrafluoroethylene material is inner-wall material is chosen, quartz is added according to the weight ratio of 100:7~10
Sand and technical hydrochloric acid；
(2) the bipyramid reaction kettle is warming up to 100~120 DEG C, the reaction kettle internal temperature keeps the temperature 4 at 100 DEG C or more
~6 hours, while the reaction kettle being kept to be in operating mixing；
(3) water that temperature is 65 DEG C or more, operating cleaning quartz is added after heat preservation terminates in step (2) into the reaction kettle
Sand stops heating after cleaning, exclude cleaning waste liquid, repeat to clean, glass sand can be obtained.
2. a kind of improved method of pickling high-purity quartz sand purifying technique according to claim 1, which is characterized in that step
(2) drain tap that the reaction kettle is opened in heating described in and the insulating process, returns the exhaust gas generated by exhaust gas
Tower is received to be neutralized.
3. a kind of improved method of pickling high-purity quartz sand purifying technique according to claim 1, which is characterized in that the fortune
Revolving speed when turning is 18~22 turns/min.
4. a kind of improved method of pickling high-purity quartz sand purifying technique according to claim 1, which is characterized in that step
(3) the volume mass ratio of quartz sand described in water described in and step (1) is 2:1.
5. a kind of improved method of pickling high-purity quartz sand purifying technique according to claim 1, which is characterized in that step
(3) cleaning waste liquid described in uses high-pressure pump intensifier discharge in exclusion process.
6. a kind of improved method of pickling high-purity quartz sand purifying technique according to claim 1, which is characterized in that step
(3) time cleaned every time in is 30min.
7. a kind of improved method of pickling high-purity quartz sand purifying technique according to claim 6, which is characterized in that step
(3) processing method of waste liquid is cleaned described in are as follows: CaO is added into the cleaning waste liquid and is neutralized, settles CaCl2Afterwards
Filtering, the water that can be recycled.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111393022A (en) * | 2020-03-23 | 2020-07-10 | 黄冈师范学院 | Preparation method of high-purity low-hydroxyl quartz glass raw material |
| CN112076889A (en) * | 2020-08-27 | 2020-12-15 | 湖北菲利华融鉴科技有限公司 | Method for efficiently discharging mixed acid for purifying high-purity quartz sand in reaction kettle |
| CN113457836A (en) * | 2020-03-15 | 2021-10-01 | 新沂市磊晶石英材料有限公司 | Quartz raw material cleaning method |
| CN114618824A (en) * | 2022-03-17 | 2022-06-14 | 湖南亿胜新材料有限公司 | Acid pickling purification device for refined quartz sand |
| CN116143133A (en) * | 2022-12-29 | 2023-05-23 | 黄冈师范学院 | Method for preparing quartz sand as inner layer raw material of quartz crucible for growth of semiconductor monocrystalline silicon |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641123A (en) * | 2013-11-21 | 2014-03-19 | 龚坚 | Quartz sand purification pickling technology and apparatus thereof |
-
2019
- 2019-08-28 CN CN201910802543.8A patent/CN110436468A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641123A (en) * | 2013-11-21 | 2014-03-19 | 龚坚 | Quartz sand purification pickling technology and apparatus thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457836A (en) * | 2020-03-15 | 2021-10-01 | 新沂市磊晶石英材料有限公司 | Quartz raw material cleaning method |
| CN111393022A (en) * | 2020-03-23 | 2020-07-10 | 黄冈师范学院 | Preparation method of high-purity low-hydroxyl quartz glass raw material |
| CN111393022B (en) * | 2020-03-23 | 2022-11-01 | 黄冈师范学院 | Preparation method of high-purity low-hydroxyl quartz glass raw material |
| CN112076889A (en) * | 2020-08-27 | 2020-12-15 | 湖北菲利华融鉴科技有限公司 | Method for efficiently discharging mixed acid for purifying high-purity quartz sand in reaction kettle |
| CN114618824A (en) * | 2022-03-17 | 2022-06-14 | 湖南亿胜新材料有限公司 | Acid pickling purification device for refined quartz sand |
| CN116143133A (en) * | 2022-12-29 | 2023-05-23 | 黄冈师范学院 | Method for preparing quartz sand as inner layer raw material of quartz crucible for growth of semiconductor monocrystalline silicon |
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