CN115771897A - Method for purifying quartz sand by continuous acid washing - Google Patents
Method for purifying quartz sand by continuous acid washing Download PDFInfo
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- CN115771897A CN115771897A CN202211478654.6A CN202211478654A CN115771897A CN 115771897 A CN115771897 A CN 115771897A CN 202211478654 A CN202211478654 A CN 202211478654A CN 115771897 A CN115771897 A CN 115771897A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 170
- 239000002253 acid Substances 0.000 title claims abstract description 131
- 239000006004 Quartz sand Substances 0.000 title claims abstract description 125
- 238000000034 method Methods 0.000 title claims abstract description 57
- 238000005406 washing Methods 0.000 title claims abstract description 52
- 239000002245 particle Substances 0.000 claims abstract description 92
- 238000005554 pickling Methods 0.000 claims abstract description 57
- 239000007788 liquid Substances 0.000 claims abstract description 44
- 239000012535 impurity Substances 0.000 claims abstract description 28
- 238000007885 magnetic separation Methods 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000746 purification Methods 0.000 claims abstract description 12
- 238000005201 scrubbing Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 43
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 239000004576 sand Substances 0.000 claims description 16
- 239000010453 quartz Substances 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 239000004570 mortar (masonry) Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000007667 floating Methods 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 7
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 6
- 229920001661 Chitosan Polymers 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 6
- 239000006148 magnetic separator Substances 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 6
- 235000010413 sodium alginate Nutrition 0.000 claims description 6
- 229940005550 sodium alginate Drugs 0.000 claims description 6
- 239000000661 sodium alginate Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 3
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 3
- 239000006071 cream Substances 0.000 claims description 3
- 239000004571 lime Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 239000013589 supplement Substances 0.000 claims description 3
- 239000010813 municipal solid waste Substances 0.000 claims description 2
- 239000002699 waste material Substances 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 238000004064 recycling Methods 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 5
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- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 20
- 235000012239 silicon dioxide Nutrition 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 230000000694 effects Effects 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 230000004913 activation Effects 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000036632 reaction speed Effects 0.000 description 3
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
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- 239000004575 stone Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
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- 229910001579 aluminosilicate mineral Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- 238000005272 metallurgy Methods 0.000 description 1
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- 229910052618 mica group Inorganic materials 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
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- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a method for continuously pickling and purifying quartz sand, and relates to the technical field of deep processing of non-metallic ores. The method for continuously pickling and purifying the quartz sand comprises the following steps: s1, crushing raw materials; s2, ultrasonic scrubbing and magnetic separation; s3, high-temperature roasting; s4, acid washing, namely uniformly mixing the quartz sand and the impurity-removed particles in an acid washing container, heating the acid washing container in a water bath, pouring mixed acid liquor into the acid washing container for sealing and stirring, and collecting the mixed acid liquor for recycling after the acid washing is finished; s5, deacidifying and washing; and S6, recovering the acid, so that the acid can be continuously used according to the concentration of the acid, and can be recycled after being correspondingly supplemented in an inconformity way. Through A granule and B granule in the edulcoration granule, make quartz sand at the in-process of pickling purification, the impurity metallic element under the pickling can be got rid of to the pickling waste liquid, and the pickling waste liquid also can carry out cyclic utilization, cooperates high temperature calcination simultaneously, makes quartz sand change and acid liquor mixing reaction, improves product quality and production efficiency.
Description
Technical Field
The invention relates to the technical field of nonmetal ore deep processing, in particular to a method for continuously pickling and purifying quartz sand.
Background
The quartz sand is quartz particles formed by crushing and processing quartz stone, the quartz stone is a non-metallic mineral substance and is a silicate mineral with hardness, wear resistance and stable chemical property, and meanwhile, the quartz sand is used as an important industrial mineral raw material and a non-chemical dangerous product and is widely applied to the industrial fields of glass, casting, ceramics and fireproof materials, metallurgy, building, chemical industry, plastics, rubber and the like.
The quartz sand contains some accompanying aluminosilicate minerals such as feldspar, mica and the like, iron-containing substances and other impurities, therefore, the quartz sand needs to be purified before being applied to the industry to meet the requirement of the industry on high purity of the quartz sand, and the industry generally purifies the quartz sand by an acid pickling method at present, wherein inorganic acids such as sulfuric acid, nitric acid, hydrochloric acid and the like or organic acids such as oxalic acid, acetic acid and the like are used, and the principle that the impurity minerals can be mostly dissolved by strong acid liquid and the quartz sand is insoluble in the strong acid is utilized to carry out acid pickling purification treatment on the quartz sand, so that the high purity quartz sand is obtained.
Based on the analysis, the pickling waste liquid generated in the pickling process of the existing quartz sand can cause serious environmental pollution, for example, hydrofluoric acid can generate volatile toxic gas silicon tetrafluoride in the pickling process, and the pickling waste liquid is discharged only through simple neutralization treatment, so that great waste exists on various acids and metal elements in the pickling waste liquid, meanwhile, the quartz sand is difficult to be uniformly mixed with acid liquid for full reaction, the product quality is unstable, and the production efficiency is low.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for continuously pickling and purifying quartz sand, which solves the problems that the pickling waste liquor cannot remove impurity metal elements under pickling in the pickling and purifying process of the quartz sand, so that the pickling waste liquor cannot be recycled, meanwhile, the quartz sand is difficult to be uniformly mixed with acid liquor for full reaction, the product quality is unstable, and the production efficiency is low.
In order to achieve the purpose, the invention is realized by the following technical scheme: the quartz sand purified by continuous acid washing has the silicon dioxide content of less than or equal to 99 percent, the iron content of more than or equal to 490ppm, the aluminum content of more than or equal to 450ppm, and the particle size of the quartz sand raw material is 40-50 meshes, and the specific technical scheme is as follows:
s1, crushing raw materials: crushing quartz sand raw materials into quartz sand fragments with the particle size of 30-40 mm, cleaning and screening, and grinding the quartz sand fragments to 5-20 meshes by adopting a wet method to obtain quartz sand particles;
s2, ultrasonic scrubbing and magnetic separation: putting the quartz sand particles obtained in the step S1 into a solution with a dispersing agent to prepare mixed mortar, putting the mixed mortar into an ultrasonic crusher for ultrasonic scrubbing for 9-10 h, and adding the mixed mortar according to the proportion of 1:0.5 of lime cream, accelerating sedimentation, pouring out supernatant, namely quartz refined sand at the lower layer, sending the quartz refined sand into a magnetic separator for magnetic separation, and obtaining the floated quartz sand after the magnetic separation is finished;
s3, high-temperature roasting: putting the quartz sand obtained in the step S2 into a roasting furnace, heating at the high temperature of 900-950 ℃ for 180-200 min, and cooling the roasted quartz sand for 10-15 min for later use;
s4, acid washing:
s401, arranging an external water bath heating device of the pickling container, keeping the water temperature at 90-95 ℃, and then putting the pickling container with the proportion of 1:1, uniformly mixing quartz sand and impurity removal particles, wherein the impurity removal particles account for 0.4-0.48 time of the total volume of the pickling container;
s402, injecting mixed acid liquid into the pickling container, starting a stirring device to pre-stir when the mixed acid liquid submerges quartz refined sand and impurity-removing particles, continuously adding the mixed acid liquid until the volume of the pickling container reaches 0.7-0.75 time, sealing the pickling container, and uniformly stirring for 3-4 hours under a sealed condition;
s403, standing for 40-50 min after stirring is finished, discharging the upper mixed acid liquid and the impurity-removing particles floating on the upper mixed acid liquid into a particle barrel, and discharging the residual mixed acid liquid into a liquid mixing barrel through a liquid outlet at the lower part of the pickling container to obtain the pickled quartz sand;
s5, deacidifying and washing: washing acid liquor on the surface of the acid-washed quartz sand, collecting the acid liquor for recycling, sending the washed quartz sand into sand washing equipment, adding clear water which is 32-36 cm higher than the quartz sand, stirring for 3 times for 35-40 min, standing for 40min at intervals during each stirring, sending the quartz sand into a drying chamber for drying after the pH value of the quartz sand is neutral by water washing, and obtaining the acid-washed and purified quartz sand.
S6, acid recovery: separating the upper mixed acid solution poured into the particle barrel and the impurity removal particles floating on the upper mixed acid solution in the step S403 by using a filter screen, mixing the separated upper mixed acid solution with the residual mixed acid solution in the liquid mixing barrel, measuring and calculating the acid concentration by using an acid concentration analyzer after mixing, sending the mixed acid solution with the required acid concentration into the step S4 for continuous use, and recycling the mixed acid solution without corresponding supplement.
Preferably, in the step S1, the raw material crushing process flow is as follows: the method comprises the following steps of firstly roughly crushing a quartz sand raw material by a jaw crusher, then finely crushing the quartz sand raw material by a cone crusher, conveying the quartz sand raw material to a vibrating screen by a conveyer belt, washing fine ores on the vibrating screen by using high-pressure water, then screening the cleaned quartz sand raw material by a cylindrical roller screen with a screen mesh of 15-100 meshes, and after the screening is finished, conveying the quartz sand raw material to a rod mill for secondary grinding to obtain the required quartz sand particles.
Preferably, in the step S2, the concentration of the mixed mortar is 35-40%, the dosage of the dispersant is 1.45-2.05 kg/t, and the ultrasonic intensity is 6-12W/m 2 。
Preferably, in the step S2, the magnetic separation process includes: feeding the quartz refined sand into a selected vertical ring pulsating high-gradient strong magnetic separator for magnetic separation for 4-6 times, wherein the initial stage of the magnetic field intensity of the magnetic separation is 0.8T, the magnetic field intensity is sequentially increased along with the magnetic separation times, and the magnetic field intensity is increased by 0.8T each time, so that the required quartz sand is obtained after the magnetic separation is completed.
Preferably, in the step S401, the trash particle is composed of a particle a and a particle B, the particle a is a pp particle with surface bound sodium alginate, and the particle B is a pp particle with surface bound chitosan.
Preferably, the preparation method of the A particles comprises the following steps: firstly, pp particles are put into a sodium chloride solution dissolved with 11 to 15 weight percent of sodium alginate, the mixture is uniformly stirred for 30 to 40min at the temperature of between 150 and 160 ℃, the mixture is quickly placed into a hydrogen chloride aqueous solution for cooling and shaping after heat filtration, and the preparation is finished after the filtration and the drying.
Preferably, the preparation method of the B particles comprises the following steps: firstly, pp particles are put into aqueous solution of hydrogen chloride dissolved with 12 to 15 weight percent of chitosan, the mixture is evenly stirred for 30 to 40min at the temperature of between 150 and 160 ℃, the mixture is quickly placed into sodium hydroxide solution for cooling and shaping after hot filtration, and the preparation is finished after the filtration and the drying.
Preferably, in the step S402, the mixed acid solution is one or more of 10 to 30wt% of nitric acid, 20 to 40wt% of hydrochloric acid, and 35 to 50wt% of hydrofluoric acid, or 35 to 40wt% of hydrofluoric acid, 25 to 30wt% of oxalic acid solution, and 5 to 20wt% of concentrated sulfuric acid.
The invention provides a method for continuously pickling and purifying quartz sand. The method has the following beneficial effects:
1. according to the invention, the quartz sand is subjected to acid cleaning and purification treatment by using the impurity removing particles and the mixed acid liquid, so that metal impurities in the quartz sand are removed, metal ions dissolved in the mixed acid liquid after acid cleaning are also removed, the metal ions in the solution are removed by chelation of the impurity removing particles, and the acid-cleaned metal ions in the mixed acid liquid are absorbed by the aid of the particles A and the particles B in the impurity removing particles in the acid cleaning process, so that the mixed acid liquid can be recycled.
2. According to the invention, the quartz sand is subjected to high-temperature roasting treatment, so that obvious cracks and corrosion pits can appear on the surface of the quartz sand, the mixed acid liquid in the subsequent pickling process can be easily immersed into quartz sand particles, the impurity removal rate is improved, the quartz sand pickling reaction speed is further accelerated, and the purification of the quartz sand is improved.
3. The preparation process is simple, reasonable and efficient in design, and the iron element and aluminum element impurities in the prepared high-purity quartz sand are greatly reduced by crushing quartz sand raw materials, ultrasonically scrubbing and magnetically separating, roasting at high temperature, pickling, deacidifying, washing and acid recovering, so that the purification quality of the finished quartz sand product is more stable, the efficiency is high, and the method is suitable for large-scale popularization and application.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
The quartz sand purified by continuous acid washing has the silicon dioxide content of less than or equal to 99 percent, the iron content of more than or equal to 490ppm, the aluminum content of more than or equal to 450ppm, and the particle size of the quartz sand raw material is 40-50 meshes.
Example 1:
the embodiment of the invention provides a method for continuously pickling and purifying quartz sand, which comprises the following steps:
s1, crushing raw materials: crushing quartz sand raw materials into quartz sand fragments with the particle size of 30mm, cleaning and screening, and grinding the quartz sand fragments to 5 meshes by adopting a wet method to obtain quartz sand particles;
s2, ultrasonic scrubbing and magnetic separation: putting the quartz sand particles obtained in the step S1 into a solution with a dispersing agent to prepare mixed mortar, putting the mixed mortar into an ultrasonic crusher for ultrasonic scrubbing for 9 hours, and adding the mixture into the ultrasonic crusher according to the proportion of 1:0.5 of lime cream, accelerating sedimentation, pouring out supernatant, namely quartz refined sand at the lower layer, sending the quartz refined sand into a magnetic separator for magnetic separation, and obtaining the floated quartz sand after the magnetic separation is finished;
the concentration of the mixed mortar is 35 percent, the dosage of the dispersant is 2.05kg/t, and the ultrasonic intensity is 6W/m 2 。
The magnetic separation process comprises the following steps: and (3) feeding the quartz refined sand into a selected vertical ring pulsating high-gradient strong magnetic separator for magnetic separation for 4-6 times, wherein the initial stage of the magnetic field intensity of the magnetic separation is 0.8T, the magnetic field intensity is sequentially increased along with the magnetic separation times, the magnetic field intensity is increased by 0.8T each time, and the required quartz sand is obtained after the magnetic separation is finished.
S3, high-temperature roasting: putting the quartz sand obtained in the step S2 into a roasting furnace, heating at the high temperature of 900 ℃ for 180min, and cooling the roasted quartz sand for 10min for later use;
s4, acid washing:
s401, arranging a water bath heating device outside the pickling container, keeping the water temperature at 90 ℃, and then putting the pickling container with the proportion of 1:1, uniformly mixing quartz sand and impurity removal particles, wherein the impurity removal particles account for 0.4 time of the total volume of the pickling container;
the impurity removal particles consist of particles A and particles B, wherein the particles A are pp particles with surface adhered sodium alginate, and the particles B are pp particles with surface adhered chitosan.
The preparation method of the A particle comprises the following steps: firstly, pp particles are put into a sodium chloride solution dissolved with 11wt% of sodium alginate, the mixture is uniformly stirred for 30min at the temperature of 150 ℃, the mixture is quickly placed into a hydrogen chloride aqueous solution for cooling and shaping after hot filtration, and the preparation is finished after the filtration and drying.
The preparation method of the B particles comprises the following steps: the preparation method comprises the steps of firstly, putting pp particles into a hydrogen chloride aqueous solution dissolved with 12wt% of chitosan, uniformly stirring for 30min at 150 ℃, quickly placing the mixture into a sodium hydroxide solution for cooling and shaping after hot filtration, and drying after filtration to obtain the product.
S402, injecting mixed acid liquid into the pickling container, starting a stirring device to pre-stir when the mixed acid liquid submerges quartz refined sand and impurity-removing particles, continuously adding the mixed acid liquid until the volume of the pickling container reaches 0.7-0.75 time, sealing the pickling container, and uniformly stirring for 3-4 hours under a sealed condition;
the mixed acid solution is one or more than two of 20wt% nitric acid, 30wt% hydrochloric acid and 40wt% hydrofluoric acid or 35wt% hydrofluoric acid, 25wt% oxalic acid solution and 15wt% concentrated sulfuric acid.
S403, standing for 40min after stirring is finished, discharging the upper mixed acid liquid and impurity-removing particles floating on the upper mixed acid liquid into a particle barrel, and discharging the residual mixed acid liquid into a liquid mixing barrel through a liquid outlet at the lower part of the pickling container to obtain the pickled quartz sand;
s5, deacidifying and washing: washing the acid liquor on the surface of the quartz sand after acid washing, collecting the acid liquor for recycling, sending the washed quartz sand into sand washing equipment, adding clear water which is 32cm over the quartz sand, stirring for 3 times and 35min, standing for 40min at intervals during each stirring, sending the quartz sand into a drying chamber for drying after the quartz sand is washed to be neutral in pH value, and obtaining the quartz sand after acid washing and purification.
S6, acid recovery: separating the upper mixed acid solution poured into the particle barrel and the impurity removal particles floating on the upper mixed acid solution in the step S403 by using a filter screen, mixing the separated upper mixed acid solution with the residual mixed acid solution in the liquid mixing barrel, measuring and calculating the acid concentration by using an acid concentration analyzer after mixing, sending the mixed acid solution with the required acid concentration into the step S4 for continuous use, and recycling the mixed acid solution without corresponding supplement.
Example 2:
except that the acid mixture and the impurity-removed particles in example 1 were continuously recycled for 10 times to perform acid washing on the quartz sand and the high-temperature calcination temperature was adjusted to 920 ℃, the other steps were identical to the experimental steps and methods of example 1 and were characterized by the same method, and the obtained quartz sand acid washing parameters are shown in table 1 below.
Example 3:
except that the mixed acid solution and the impurity-removed particles in example 1 were continuously recycled 40 times to perform acid washing on the quartz sand and the high-temperature calcination temperature was adjusted to 930 ℃, the other steps were identical to the experimental steps and methods of example 1, and the same methods were used for characterization, and the obtained quartz sand acid washing parameters are shown in table 1 below.
Example 4:
except that the mixed acid solution and the impurity-removed particles in the example 1 are continuously recycled for 60 times to perform acid washing on the quartz sand and the high-temperature roasting temperature is adjusted to 940 ℃, other steps are consistent with the experimental steps and the method in the example 1, and the same method is adopted for characterization, so that the obtained acid washing parameters of the quartz sand are shown in the following table 1.
Comparative example 1:
the impurity-removed particle composition of example 1 was adjusted to consist of one particle a alone, and the other steps were identical to the experimental steps and methods of example 1 and were characterized in the same manner, and the pickling parameters of the quartz sand were as shown in table 1 below.
Comparative example 2
Except for continuously recycling 10 times of the mixed acid solution and the impurity-removed particles in the comparative example 1 to perform acid washing on the quartz sand, the other steps are consistent with the experimental steps and the method of the comparative example 1, and the same method is adopted for characterization, and the obtained acid washing parameters of the quartz sand are shown in the following table 1.
Comparative example 3:
the impurity-removed particle composition of example 1 was adjusted to consist of one particle B alone, and the other steps were identical to the experimental steps and methods of example 1 and were characterized in the same manner, and the pickling parameters of the quartz sand were as shown in table 1 below.
Comparative example 4:
except for continuously recycling 10 times of the mixed acid solution and the impurity-removed particles in the comparative example 3 to perform acid washing on the quartz sand, the other steps are consistent with the experimental steps and the method of the comparative example 3, and the same method is adopted for characterization, and the obtained acid washing parameters of the quartz sand are shown in the following table 1.
Comparative example 5:
the high temperature calcination step of example 1 was eliminated, and the other steps were identical to and characterized by the same procedure as the experimental steps and method of example 1, and the pickling parameters of the resulting silica sand are shown in table 1 below.
Comparative example 6:
except for continuously recycling 10 times of the mixed acid solution and the impurity-removed particles in the comparative example 5 to perform acid washing on the quartz sand, the other steps are consistent with the experimental steps and the method of the comparative example 5, and the same method is adopted for characterization, and the obtained acid washing parameters of the quartz sand are shown in the following table 1.
Comparative example 7:
the quartz sand was pickled with a mixed acid solution containing 20wt% of nitric acid, 30wt% of hydrochloric acid and 40wt% of hydrofluoric acid.
The silica content, the iron element content and the aluminum element content of the quartz sand acid-washed in examples 1 to 4 and comparative examples 1 to 6 were measured, respectively, and the metal impurity content of the mixed acid solution recycled after the treatment by the methods in examples 1 to 4 and comparative examples 1 to 6 was measured, and the test results are recorded in table 1.
Table 1:
from the test results of the embodiments 1 to 4, it can be seen that, by using the method for continuously pickling and purifying quartz sand according to the present invention, the pickling and purification in the steps S1 to S5 can achieve a better effect of removing metal impurities from quartz sand, and the used mixed acid solution can be matched with the effect of removing impurity particles, so as to further improve the purification quality, and simultaneously, the mixed acid solution can be recycled, so that the pickling effect of the mixed acid solution is not greatly reduced and weakened due to the increase of the use times, the floating range of the pickling effect is small, the capability of removing metal impurities is strong, that is, the impurity removal particles formed by the combination of the particles a and the particles B are used to remove metal ions dissolved in the pickling solution, and then, the pickling reaction speed is faster after the combination with the high-temperature roasting treatment, the activation energy is lower, and the iron removal rate is higher.
According to the test results of the comparative example 1 and the comparative example 2, the quartz sand can achieve a good purification effect in the first pickling of the comparative example 1, but when reaching the comparative example 2, the mixed acid solution and the impurity removal particles formed by the single A particles are pickled in a matched manner, metal ions in the quartz sand cannot be effectively removed, and meanwhile, when too much mixed acid solution is used, metal impurities in the mixed acid solution are too much accumulated and cannot be removed and recycled, so that resource waste and a poor quartz sand purification effect are caused.
According to the comparative examples 5 and 6, the quartz sand is in a normal temperature state when the high-temperature roasting condition exists, no obvious cracks or corrosion pits appear on the surface, acid liquid is not beneficial to being immersed into the inside of particles, the impurity removal rate is low, aluminum metal impurities cannot be removed too much, the purification effect of the quartz sand is influenced, and therefore roasting treatment is needed to enable the quartz sand pickling reaction speed to be higher, the activation energy to be lower and the iron and aluminum removal rate to be higher. Meanwhile, the activation energy of the traditional acid washing reaction is 30.88kJ/mol, the activation energy of the acid washing reaction without roasting is 36.18kJ/mol, and the activation energy is reduced by 17.2% after roasting, which indicates that the crystal form transformation caused by roasting is beneficial to acid washing of quartz sand.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for continuously pickling and purifying quartz sand is characterized by comprising the following steps: the method comprises the following steps:
s1, crushing raw materials: crushing quartz sand raw materials into quartz sand fragments with the particle size of 30-40 mm, cleaning and screening, and grinding the quartz sand fragments to 5-20 meshes by adopting a wet method to obtain quartz sand particles;
s2, ultrasonic scrubbing and magnetic separation: putting the quartz sand particles obtained in the step S1 into a solution with a dispersing agent to prepare mixed mortar, putting the mixed mortar into an ultrasonic crusher for ultrasonic scrubbing for 9-10 h, and adding the mixture into the ultrasonic crusher according to the proportion of 1:0.5 of lime cream, accelerating sedimentation, pouring out supernatant, namely quartz refined sand at the lower layer, sending the quartz refined sand into a magnetic separator for magnetic separation, and obtaining the floated quartz sand after the magnetic separation is finished;
s3, high-temperature roasting: putting the quartz sand obtained in the step S2 into a roasting furnace, heating at the high temperature of 900-950 ℃ for 180-200 min, and cooling the roasted quartz sand for 10-15 min for later use;
s4, acid washing:
s401, arranging an external water bath heating device of the pickling container, keeping the water temperature at 90-95 ℃, and then putting the pickling container with the proportion of 1:1, uniformly mixing quartz sand and impurity removal particles, wherein the impurity removal particles account for 0.4-0.48 time of the total volume of the pickling container;
s402, injecting mixed acid liquid into the pickling container, starting a stirring device to pre-stir when the mixed acid liquid submerges quartz refined sand and impurity-removing particles, continuously adding the mixed acid liquid until the volume of the pickling container reaches 0.7-0.75 time, sealing the pickling container, and uniformly stirring for 3-4 hours under a sealed condition;
s403, standing for 40-50 min after stirring is finished, discharging the upper mixed acid liquid and the impurity-removing particles floating on the upper mixed acid liquid into a particle barrel, and discharging the residual mixed acid liquid into a liquid mixing barrel through a liquid outlet at the lower part of the pickling container to obtain the pickled quartz sand;
s5, deacidifying and washing: washing the acid liquor on the surface of the quartz sand after acid washing, wherein the acid liquor can be collected and recycled, sending the washed quartz sand into sand washing equipment, adding clear water which is 32-36 cm higher than the quartz sand, stirring for 3 times for 35-40 min, standing for 40min at intervals during each stirring, sending the quartz sand into a drying chamber for drying after the quartz sand is washed to be neutral in pH value, and obtaining the quartz sand after acid washing and purification.
S6, acid recovery: and (4) separating the upper mixed acid liquid poured into the particle barrel and the impurity-removing particles floating on the upper mixed acid liquid in the step (S403) through a filter screen, mixing the separated upper mixed acid liquid with the residual mixed acid liquid in the liquid mixing barrel, measuring and calculating the acid concentration by using an acid concentration analyzer after mixing, sending the acid concentration meeting the requirement into the step (S4) for continuous use, and reusing the acid concentration after not meeting the requirement of corresponding supplement.
2. The method for purifying quartz sand by continuous acid washing according to claim 1, wherein the method comprises the following steps: in the step S1, the raw material crushing process flow is as follows: the method comprises the steps of firstly roughly crushing quartz sand raw materials through a jaw crusher, then finely crushing the raw materials in a cone crusher, conveying the quartz sand raw materials to a vibrating screen through a conveying belt, washing fine ores on the vibrating screen by using high-pressure water, then screening the cleaned raw materials in a cylindrical roller screen with a screen mesh of 15-100 meshes, and conveying the cleaned raw materials to a rod mill for secondary grinding after screening is finished, so that required quartz sand particles are obtained.
3. The method for purifying quartz sand by continuous acid washing according to claim 1, characterized in that: in the step S2, the concentration of the mixed mortar is 35-40%, the dosage of the dispersant is 1.45-2.05 kg/t, and the ultrasonic intensity is 6-12W/m 2 。
4. The method for purifying quartz sand by continuous acid washing according to claim 1, characterized in that: in the step S2, the magnetic separation process flow is as follows: feeding the quartz refined sand into a selected vertical ring pulsating high-gradient strong magnetic separator for magnetic separation for 4-6 times, wherein the initial stage of the magnetic field intensity of the magnetic separation is 0.8T, the magnetic field intensity is sequentially increased along with the magnetic separation times, and the magnetic field intensity is increased by 0.8T each time, so that the required quartz sand is obtained after the magnetic separation is completed.
5. The method for purifying quartz sand by continuous acid washing according to claim 1, wherein the method comprises the following steps: in the step S401, the trash removal particle is composed of a particle a and a particle B, where the particle a is a pp particle with surface bound with sodium alginate, and the particle B is a pp particle with surface bound with chitosan.
6. The method for purifying quartz sand by continuous acid washing as claimed in claim 5, wherein: the preparation method of the A particles comprises the following steps: firstly, pp particles are put into a sodium chloride solution dissolved with 11 to 15 weight percent of sodium alginate, the mixture is uniformly stirred for 30 to 40min at the temperature of between 150 and 160 ℃, the mixture is quickly placed into a hydrogen chloride aqueous solution for cooling and shaping after heat filtration, and the preparation is finished after the filtration and the drying.
7. The method for purifying quartz sand by continuous acid washing as claimed in claim 5, wherein: the preparation method of the B particles comprises the following steps: firstly, pp particles are put into aqueous solution of hydrogen chloride dissolved with 12 to 15 weight percent of chitosan, the mixture is evenly stirred for 30 to 40min at the temperature of between 150 and 160 ℃, the mixture is quickly placed into sodium hydroxide solution for cooling and shaping after hot filtration, and the preparation is finished after the filtration and the drying.
8. The method for purifying quartz sand by continuous acid washing according to claim 1, wherein the method comprises the following steps: in the step S402, the mixed acid solution is one or more than two of 10-30 wt% nitric acid, 20-40 wt% hydrochloric acid and 35-50 wt% hydrofluoric acid or 35-40 wt% hydrofluoric acid, 25-30 wt% oxalic acid solution and 5-20 wt% concentrated sulfuric acid.
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