CN108128780B - A kind of method of cycle pickling quartz sand - Google Patents
A kind of method of cycle pickling quartz sand Download PDFInfo
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- CN108128780B CN108128780B CN201810051855.5A CN201810051855A CN108128780B CN 108128780 B CN108128780 B CN 108128780B CN 201810051855 A CN201810051855 A CN 201810051855A CN 108128780 B CN108128780 B CN 108128780B
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- quartz sand
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- compound grain
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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
Abstract
The invention discloses a kind of methods of cycle pickling quartz sand, mainly by being mixed into the first compound grain and the second compound grain in quartz sand, two kinds of composite particles can adsorb dissolved impurity metal ion in chelating pickling solution in acid cleaning process, the density of composite particles is smaller simultaneously, pickling solution upper layer can be floated on, is easily separated and recycles after pickling；Related method through the invention can effectively remove the metal ion dissolved in pickling solution in not having to and under conditions of pickling solution, and realize the recycling to metal ion, and operating method simple possible is environmentally protective, takes full advantage of various acid constituents.
Description
Technical field
The present invention relates to quartz sand manufacture field, in particular to a kind of method of cycle pickling quartz sand.
Background technique
As quartz sand plays increasingly important role in the industries such as photovoltaic, microelectronics, optical-fibre communications,
Social production made higher requirement required quartz sand in terms of quality and quantity, usually mined quartz
Ore contains the metal impurities such as more iron, aluminium, titanium, alkali metal, these impurity can seriously affect quartz ware light transmission rate,
The performances such as conductivity, thermal stability, therefore removing the quartz sand that various metal impurities obtain high-purity in quartz sand is deep processing
Quartz sand and the premise for producing quartz sand product.
In quartz sand processing industry, frequently with the technique of removal quartz sand impurity have scouring, magnetic separation, flotation, pickling
Deng, wherein pickling is significant to the removal effect of the foreign metals such as iron micro in quartz sand, aluminium, be obtain high-quality quartz sand have
Effect approach.Common pickling solution mainly includes the components such as hydrofluoric acid, hydrochloric acid, nitric acid, sulfuric acid, oxalic acid, and wherein hydrofluoric acid can be molten
Solving silica, dosage is not easy excessive, iron content can be substantially reduced by synergistic effect when hydrofluoric acid and nitric acid exist simultaneously, from
And obtain the quartz sand of high-purity.But the acid cleaning process of quartz sand and pickle liquor may cause serious environmental pollution,
For example hydrofluoric acid can generate volatility toxic gas ocratation in acid cleaning process, and pickle liquor is merely through in simple
It is just discharged with processing, to wherein various acid and metallic element, all there is biggish wastes.
Summary of the invention
For the shortcomings of the prior art, the present invention is by being bonded with the compound grain of polymer in pickling solution
Metal ion chelated, in not having to and pickle liquor in the case where, successfully eliminates the impurity metallic elements in system,
Enable pickling solution repeatedly cycle pickling quartz sand.
Dioxide-containing silica≤98%, iron content >=600ppm, the grain of quartz mine in quartz sand according to the present invention
For diameter in 20~40 mesh, specific technical solution is as follows:
1) it is put into the solid particle being made of quartz sand, the first compound grain and the second compound grain in pickling tank and mixes equal
Even, the total volume of the solid particle accounts for the 0.5~0.6 of pickling tank volume；Wherein, the described first compound grain is surface bonding seaweed
The PP GRANULES of sour sodium, the second compound grain are the PP GRANULESs of surface bonding chitosan；
2) injected from bottom into pickling tank containing hydrochloric acid, hydrofluoric acid, nitric acid pickling solution, when pickling solution floods solid
When grain, agitating device is opened, and continues to inject pickling solution to 0.8~0.95 times of pickling tank volume, is stirred in confined conditions
Pickling 5~6 hours；
3) 20~30 minutes are stood after stopping stirring, the first compound grain and the second compound grain swim in the acid on quartz sand upper layer
In washing lotion, from pickling tank top by containing there are two types of the discharge of the pickling solution of compound grain, it is discharged from pickling pot bottom without compound grain
Pickling solution；Quartz sand remained on surface pickling solution is rinsed, flushing liquor can be recycled after collecting, and it is dry that quartz sand is placed in drying chamber；
4) pickling solution on quartz sand upper layer is filtered off and is mixed with the pickling solution being discharged from pickling pot bottom after compound grain, when
It is accordingly supplemented when acid constituents concentration is lower than required concentration in mixed pickling solution, then proceedes to acid-washed quartz sand.
Preferably, the first compound grain described in step 1) is placed in PP GRANULES dissolved with 8~10wt% alginic acid
In the 1mol/L sodium hydroxide solution of sodium, is stirred 50~60 minutes at 120~130 DEG C, 0.3mol/ is immediately placed in after heat filtering
Cooling cohesion, is drying to obtain after filtering in l hydrochloric acid solution.
Preferably, the second compound grain described in step 1) is placed in PP GRANULES dissolved with 8~10wt% chitosan
0.3mol/l hydrochloric acid solution in, stirred 50~60 minutes at 120~130 DEG C, 1mol/l hydrogen-oxygen be immediately placed in after heat filtering
Change cooling cohesion in sodium solution, is drying to obtain after filtering.
Preferably, the partial size of PP GRANULES described in step 1) is in 1~2mm.
Preferably, the mass ratio of quartz sand described in step 1), the first compound grain and second compound three is 1:
0.05~0.06: 0.1~0.12.
Preferably, the mass fraction of each component is 6~8wt% hydrochloric acid, 3~5wt% in pickling solution described in step 2)
Hydrofluoric acid, 8~10wt% nitric acid.
Preferably, the compound grain being filtered off described in step 4) is placed in the solution containing 0.5mol/L sodium hydroxide
Middle stirring 20~30 minutes, is centrifugated and is rinsed with deionized water, reusable after dry.
To the present invention and its advantages elaboration: to the key that quartz sand acid dilution recycles be removal pickling it
The metal ion dissolved in solution afterwards, conventional technique is to use alkali neutralization pickling solution at present, makes metal ion under alkaline condition
Precipitating, although eliminating metal ion in this way, acid solution is also wasted, and cannot achieve recycling for acid；The present invention
In the metal ion in solution removed by the chelation of chitosan, chitosan is carried on poly- third by specially treated first
The second compound grain is formed on alkene particle, the second compound grain can chelate adsorbing metal ions in acid cleaning process；Polypropylene simultaneously
Density ratio pickling solution is small, can swim in solution upper layer, and quartzy sand separation, so not changing system pH's after pickling
On the basis of, effectively remove metal ion in solution.
The PP GRANULES of surface bonding sodium alginate is also added into the present invention as the first compound grain, in pickling system
In its can also be floated on solution upper layer, the silicon tetrafluoride gas that sodium alginate generates hydrofluoric acid and silicon dioxde reaction have compared with
Good suction-operated, can be avoided ocratation toxic gas and is diffused into air；The first compound grain and second in system is multiple
Grain is closed after pickling, swims in pickling solution upper layer, by being simply separated by solid-liquid separation available removal metal ion
Pickling solution, but small part acid constituents can be lost, it can serve as pickling solution after supplement and be recycled；It is separated
Compound grain is put into sodium hydroxide solution, and sodium hydroxide can dissolve the ocratation adsorbed in sodium alginate, while chitosan
Or the metal ion for chelating or adsorbing in sodium alginate generates precipitating in sodium hydroxide, can be recycled.
Although sodium alginate can be dissolved in alkaline solution, PP GRANULES table is bonded in by specially treated
The sodium alginate in face can be kept preferable structural without departing from dispersion with PP GRANULES；PP GRANULES 120~
130 DEG C of condition lower surfaces start to soften, and are cross-linked with each other bonding with the long-chain of sodium alginate or chitosan, then change solution ring
Border particle can solidify reunion, and particle surface is by the corresponding polymer-modified compound grain obtained with specific function；By this hair
Method involved in bright can effectively remove the metal ion dissolved in pickling solution in not having to and under conditions of pickling solution, and
The recycling to metal ion is realized, operating method simple possible is environmentally protective, takes full advantage of various acid constituents.
Specific embodiment
The present invention is described in further detail below, to enable those skilled in the art's refer to the instruction text being capable of evidence
To implement.
Dioxide-containing silica≤98%, iron content >=600ppm in the quartz sand of institute's pickling processes of the present invention, quartz mine
Partial size in 20~40 mesh.
Embodiment 1
1) it is put into pickling tank and accounts for being obtained by mixing by quartz sand, the first compound grain and the second compound grain for tank volume half
Solid particle, the mass ratio of three is successively 1: 0.05: 0.1；
The preparation of first compound grain: partial size is placed in the PP GRANULES of 1~2mm dissolved with 8~10wt% sodium alginate
1mol/L sodium hydroxide solution in, stirred 60 minutes at 120~130 DEG C, 0.3mol/l hydrochloric acid be immediately placed in after heat filtering
Cooling cohesion, is drying to obtain after filtering in solution.
The preparation of second compound grain: partial size is placed in the PP GRANULES of 1~2mm dissolved with 8~10wt% chitosan
In 0.3mol/l hydrochloric acid solution, is stirred 60 minutes at 120~130 DEG C, it is molten that 1mol/l sodium hydroxide is immediately placed in after heat filtering
Cooling cohesion, is drying to obtain after filtering in liquid.
2) injected from bottom into pickling tank containing 8wt% hydrochloric acid, 5wt% hydrofluoric acid, 10wt% nitric acid pickling solution, when
When pickling solution floods solid particle, agitating device is opened, and continues to inject pickling solution to 0.8 times of pickling tank volume, closed
Under the conditions of stirring and pickling 6 hours；
3) 30 minutes are stood after stopping stirring, the first compound grain and the second compound grain swim in the pickling solution on quartz sand upper layer
In, from pickling tank top by containing there are two types of the discharge of the pickling solution of compound grain, the pickling for being free of compound grain is discharged from pickling pot bottom
Liquid；Quartz sand remained on surface pickling solution is rinsed, flushing liquor can be recycled after collecting, and it is dry that quartz sand is placed in drying chamber；
4) pickling solution on quartz sand upper layer is filtered off and is mixed with the pickling solution being discharged from pickling pot bottom after compound grain, when
It is accordingly supplemented when acid constituents concentration is lower than required concentration in mixed pickling solution, then proceedes to acid-washed quartz sand；
5) the compound grain being filtered off in step 4) is placed in the solution containing 0.5mol/L sodium hydroxide and stirs 30 minutes, from
The heart is separated and is rinsed with deionized water, reusable after dry.
Embodiment 2
Pickling is carried out to quartz sand to have recycled pickling solution in 5 embodiments 1 and compound grain.
Embodiment 3
Pickling is carried out to quartz sand to have recycled pickling solution in 30 embodiments 1 and compound grain.
Comparative example 1
1) solid particle being obtained by mixing by quartz sand, the first compound grain for accounting for tank volume half is put into pickling tank,
The mass ratio of the two is 1: 0.15；
2) injected from bottom into pickling tank containing 8wt% hydrochloric acid, 5wt% hydrofluoric acid, 10wt% nitric acid pickling solution, when
When pickling solution floods solid particle, agitating device is opened, and continues to inject pickling solution to 0.8 times of pickling tank volume, closed
Under the conditions of stirring and pickling 6 hours；
3) 30 minutes are stood after stopping stirring, the first compound grain is swum in the pickling solution on quartz sand upper layer, from pickling tank
Top will be discharged containing the pickling solution of the first compound grain, and the pickling solution of compound grain is free of from the discharge of pickling pot bottom；Rinse quartz
Sand remained on surface pickling solution, flushing liquor can be recycled after collecting, and it is dry that quartz sand is placed in drying chamber；
4) pickling solution on quartz sand upper layer is filtered off and is mixed with the pickling solution being discharged from pickling pot bottom after the first compound grain
It closes, is accordingly supplemented when acid constituents concentration is lower than required concentration in mixed pickling solution, then proceed to acid-washed quartz sand；
5) the compound grain of first be filtered off in step 4), which is placed in the solution containing 0.5mol/L sodium hydroxide, stirs 30 points
Clock is centrifugated and is rinsed with deionized water, reuses after dry.
Comparative example 2
Pickling is carried out to have recycled pickling solution in 5 comparative examples 1 and compound grain to quartz sand.
Comparative example 3
1) solid particle being obtained by mixing by quartz sand, the second compound grain for accounting for tank volume half is put into pickling tank,
The mass ratio of the two is 1: 0.15；
2) injected from bottom into pickling tank containing 8wt% hydrochloric acid, 5wt% hydrofluoric acid, 10wt% nitric acid pickling solution, when
When pickling solution floods solid particle, agitating device is opened, and continues to inject pickling solution to 0.8 times of pickling tank volume, closed
Under the conditions of stirring and pickling 6 hours；
3) 30 minutes are stood after stopping stirring, the second compound grain is swum in the pickling solution on quartz sand upper layer, from pickling tank
Top will be discharged containing the pickling solution of the second compound grain, and the pickling solution of compound grain is free of from the discharge of pickling pot bottom；Rinse quartz
Sand remained on surface pickling solution, flushing liquor can be recycled after collecting, and it is dry that quartz sand is placed in drying chamber；
4) pickling solution on quartz sand upper layer is filtered off and is mixed with the pickling solution being discharged from pickling pot bottom after the second compound grain
It closes, is accordingly supplemented when acid constituents concentration is lower than required concentration in mixed pickling solution, then proceed to acid-washed quartz sand；
5) the compound grain of second be filtered off in step 4), which is placed in the solution containing 0.5mol/L sodium hydroxide, stirs 30 points
Clock is centrifugated and is rinsed with deionized water, reuses after dry.
Comparative example 4
Pickling is carried out to have recycled pickling solution in 5 comparative examples 3 and compound grain to quartz sand.
Comparative example 5
Pickling is carried out to have recycled pickling solution in 30 comparative examples 3 and compound grain to quartz sand.
Comparative example 6
1) solid particle being obtained by mixing by quartz sand, PP GRANULES for accounting for tank volume half is put into pickling tank,
The mass ratio of the two is 1: 0.15；
2) injected from bottom into pickling tank containing 8wt% hydrochloric acid, 5wt% hydrofluoric acid, 10wt% nitric acid pickling solution, when
When pickling solution floods solid particle, agitating device is opened, and continues to inject pickling solution to 0.8 times of pickling tank volume, closed
Under the conditions of stirring and pickling 6 hours；
3) 30 minutes are stood after stopping stirring, PP GRANULES is swum in the pickling solution on quartz sand upper layer, from pickling tank
Pickling solution containing PP GRANULES is discharged on top, and the pickling solution of compound grain is free of from the discharge of pickling pot bottom；Rinse quartz
Sand remained on surface pickling solution, flushing liquor can be recycled after collecting, and it is dry that quartz sand is placed in drying chamber；
4) pickling solution on quartz sand upper layer is filtered off and is mixed with the pickling solution being discharged from pickling pot bottom after PP GRANULES
It closes, is accordingly supplemented when acid constituents concentration is lower than required concentration in mixed pickling solution, then proceed to acid-washed quartz sand；
5) PP GRANULES being filtered off in step 4), which is placed in the solution containing 0.5mol/L sodium hydroxide, stirs 30 points
Clock is centrifugated and is rinsed with deionized water, dry.
Comparative example 7
With containing 8wt% hydrochloric acid, 5wt% hydrofluoric acid, 10wt% nitric acid pickling solution acid-washed quartz sand.
Dioxide-containing silica and iron in quartz sand of the test Jing Guo 1~6 pickling processes of Examples 1 to 3 and comparative example respectively
Constituent content, while metals content impurity in pickling solution is tested after method processing in Examples 1 to 3 and comparative example 1~6,
In test result record and table 1.
By the test result of Examples 1 to 3 it is known that using cycle pickling quartz sand according to the present invention side
The effect of method, can still be maintained the effect of preferable removing metal impurities after multiple acid-washed quartz sand, pickling solution not because
The number recycled increases and weakens, and only floats in error range, wherein remaining metal after spent picking solution per treatment
Impurity content is less, i.e., can almost completely remove the gold dissolved in pickling solution using the first compound grain and the second compound grain
Belong to ion；The recycle acid washing lotion process of comparative example 1 and comparative example 2 lacks the second compound grain, and the effect of the second compound grain makes to pass through
The metal ion in removal system is chelated, comparative example 1, which is shown in quartz sand in first time pickling, can reach preferable refining effect,
But concentration of metal ions is higher in its pickling solution, comparative example 2 shows that pickling solution is recycled 5 times later to the acid of quartz sand
Effect is washed, the effect of quartz sand after pickling cannot reach higher silica purity and lower iron content, i.e. pickling solution
It reduces obvious；The display of comparative example 3~5 is when lacking first compound, and when multiple recycle acid washing lotion also will affect metal in pickling solution
Impurity-eliminating effect, especially when pickling solution is recycled for 30 times or more, pickling solution purifies quartz sand effect and loses serious, this explanation the
One compound grain also has certain chelating suction-operated to the metal ion in solution, cooperates with the second compound grain mutual cooperation
Effect, can preferably remove foreign metal ion, realize the recycling of pickling solution；Comparative example 6 is with polypropylene
Grain replaces two kinds of compound grains, compared with the data of comparative example 7, it is found that method involved in comparative example 6 almost not can be removed solution
Middle institute's dissolved impurity metal impurities, the PP GRANULES that this explanation has only bonded particular polymers just have removing pickling molten
In liquid the effect of foreign metal, the first compound grain and the second compound grain are indispensable during cycle pickling quartz sand.
Table 1
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and embodiment shown here or comparative example.
Claims (7)
1. a kind of method of cycle pickling quartz sand, which comprises the following steps:
1) it is put into the solid particle being made of quartz sand, the first compound grain and the second compound grain in pickling tank and is uniformly mixed,
The total volume of the solid particle accounts for the 0.5~0.6 of pickling tank volume；Wherein, the described first compound grain is surface bonding alginic acid
The PP GRANULES of sodium, the second compound grain are the PP GRANULESs of surface bonding chitosan；
2) injected from bottom into pickling tank containing hydrochloric acid, hydrofluoric acid, nitric acid pickling solution, when pickling solution floods solid particle
When, agitating device is opened, and continue to inject pickling solution to 0.8~0.95 times of pickling tank volume, stirring is sour in confined conditions
It washes 5~6 hours；
3) 20~30 minutes are stood after stopping stirring, the first compound grain and the second compound grain swim in the pickling solution on quartz sand upper layer
In, from pickling tank top by containing there are two types of the discharge of the pickling solution of compound grain, the pickling for being free of compound grain is discharged from pickling pot bottom
Liquid；Quartz sand remained on surface pickling solution is rinsed, flushing liquor can be recycled after collecting, and it is dry that quartz sand is placed in drying chamber；
4) pickling solution on quartz sand upper layer is filtered off and is mixed with the pickling solution being discharged from pickling pot bottom after compound grain, work as mixing
It is accordingly supplemented when acid constituents concentration is lower than required concentration in pickling solution afterwards, then proceedes to acid-washed quartz sand.
2. the method according to claim 1, wherein the first compound grain described in step 1) is by PP GRANULES
It is placed in the 1mol/L sodium hydroxide solution dissolved with 8~10wt% sodium alginate, is stirred 50~60 minutes at 120~130 DEG C,
It is immediately placed in 0.3mol/l hydrochloric acid solution cooling cohesion after heat filtering, is drying to obtain after filtering.
3. the method according to claim 1, wherein the second compound grain described in step 1) is by PP GRANULES
It is placed in the 0.3mol/l hydrochloric acid solution dissolved with 8~10wt% chitosan, is stirred 50~60 minutes at 120~130 DEG C, hot mistake
It is immediately placed in 1mol/l sodium hydroxide solution cooling cohesion after filter, is drying to obtain after filtering.
4. the method according to claim 1, wherein the partial size of PP GRANULES described in step 1) 1~
2mm。
5. the method according to claim 1, wherein quartz sand described in step 1), the first compound grain and second
The mass ratio of compound grain three is 1: 0.05~0.06: 0.1~0.12.
6. the method according to claim 1, wherein in pickling solution described in step 2) each component mass fraction
For 6~8wt% hydrochloric acid, 3~5wt% hydrofluoric acid, 8~10wt% nitric acid.
7. containing the method according to claim 1, wherein the compound grain being filtered off described in step 4) is placed in
Have in the solution of 0.5mol/L sodium hydroxide and stir 20~30 minutes, be centrifugated and rinsed with deionized water, can be weighed after dry
It is multiple to use.
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| CN111334091B (en) * | 2020-03-07 | 2021-08-03 | 廉江市东兴硅质材料有限公司 | Quartz sand modification method |
| CN113003781A (en) * | 2021-03-15 | 2021-06-22 | 蕲春县昌兴石英设备有限公司 | Treatment method of quartz sand pickling sewage |
| CN115771897A (en) * | 2022-11-23 | 2023-03-10 | 平远县正远实业有限公司 | Method for purifying quartz sand by continuous acid washing |
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| CN103382087A (en) * | 2013-07-05 | 2013-11-06 | 田辉明 | Method of preparing low iron-containing quartz sand for photovoltaic glass from pyrite type quartzite and pickling purification apparatus |
| CN103449455A (en) * | 2013-08-30 | 2013-12-18 | 连云港市弘扬石英制品有限公司 | Method for producing high-quality quartz sand by taking low-grade quartz mines as raw materials |
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| KR101574416B1 (en) * | 2014-03-10 | 2015-12-03 | 수원대학교산학협력단 | Method for producing granular meso-porous silica |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103382087A (en) * | 2013-07-05 | 2013-11-06 | 田辉明 | Method of preparing low iron-containing quartz sand for photovoltaic glass from pyrite type quartzite and pickling purification apparatus |
| CN103449455A (en) * | 2013-08-30 | 2013-12-18 | 连云港市弘扬石英制品有限公司 | Method for producing high-quality quartz sand by taking low-grade quartz mines as raw materials |
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Effective date of registration: 20190909 Address after: 221412 eastern part of Hebu 323 provincial road, Xinyi, Xuzhou, Jiangsu Applicant after: Xuzhou Wanda quartz Co., Ltd. Address before: 221412 silicon industry science and Technology Industrial Park, Xinyi, Xuzhou, Jiangsu Applicant before: JIANGSU ZELONG QUARTZ CO., LTD. |