CN118270795A - Preparation process of high-purity quartz sand based on acid leaching method - Google Patents
Preparation process of high-purity quartz sand based on acid leaching method Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 193
- 239000006004 Quartz sand Substances 0.000 title claims abstract description 155
- 239000002253 acid Substances 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 62
- 238000002386 leaching Methods 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005336 cracking Methods 0.000 claims abstract description 113
- 239000007788 liquid Substances 0.000 claims abstract description 80
- 238000011282 treatment Methods 0.000 claims abstract description 44
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000004321 preservation Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 230000008595 infiltration Effects 0.000 claims abstract description 7
- 238000001764 infiltration Methods 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000012544 monitoring process Methods 0.000 claims description 29
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 10
- 239000004576 sand Substances 0.000 claims description 10
- 230000000739 chaotic effect Effects 0.000 claims description 9
- 238000004220 aggregation Methods 0.000 claims description 8
- 230000002776 aggregation Effects 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 6
- 238000003837 high-temperature calcination Methods 0.000 claims description 6
- 230000003287 optical effect Effects 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 5
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 5
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 5
- 230000011218 segmentation Effects 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 238000004458 analytical method Methods 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- 230000002146 bilateral effect Effects 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 238000007872 degassing Methods 0.000 description 3
- 238000003708 edge detection Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 230000009295 sperm incapacitation Effects 0.000 description 3
- 230000001174 ascending effect Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The application relates to the technical field of high-purity quartz sand preparation, in particular to a high-purity quartz sand preparation process based on an acid leaching method, which comprises the following steps: sieving quartz sand raw ore, calcining at high temperature, performing heat preservation treatment, performing primary acid leaching, and placing into a light wave microwave oven for removing gas-liquid inclusion and infiltration treatment; acquiring quartz sand images at all times in a light wave microwave oven, acquiring inclusion matching indexes of all pixel points in the quartz sand images at all times, acquiring inclusion cracking trend indexes at all times, and determining the time for putting the quartz sand images into the light wave microwave oven based on the inclusion cracking trend indexes at all times; and then, carrying out secondary acid leaching on the quartz sand, putting the quartz sand into a hydrothermal reaction kettle, carrying out hydrothermal acid leaching treatment, finally, washing the quartz sand to be neutral by distilled water under the ultrasonic condition, and drying the quartz sand to obtain the high-purity quartz sand. The application aims to improve the purity and quality of the prepared quartz sand.
Description
Technical Field
The application relates to the technical field of high-purity quartz sand preparation, in particular to a high-purity quartz sand preparation process based on an acid leaching method.
Background
The high-purity quartz sand is regarded as a strategic resource, is relatively high-purity quartz sand and mainly consists of silicon dioxide. The high-purity quartz sand has excellent optical performance, thermal stability, electrical insulation and other excellent performances, so that the high-purity quartz sand has wide application in the optical field, the semiconductor industry, the chemical industry, the environmental engineering and the like. The process for preparing the high-purity quartz sand comprises a normal temperature method, a low temperature method, an acid leaching method and the like, and the acid leaching method has the advantages of high purity, strong controllability, high efficiency and the like, so that the process becomes a common method for preparing the high-purity quartz sand.
The technological process for preparing the high-purity quartz sand by the acid leaching method comprises sieving and grading, high-temperature calcination treatment, light wave microwave treatment, hydrothermal acid leaching treatment and washing and drying treatment, wherein in the light wave microwave treatment process, the treatment time is required to be strictly controlled, and if the treatment time is shorter, the gas and liquid in the gas-liquid inclusion are not completely removed, so that impurities in the gas-liquid inclusion still exist in the high-purity quartz sand, and the purity of the prepared quartz sand is reduced; if the treatment time is too long, the overheating problem may be caused, so that the mineral and crystal structures in the quartz sand are damaged, and the physical and chemical properties of the quartz sand are affected, so that the quality of the quartz sand is lower.
Disclosure of Invention
In order to solve the technical problems, the application provides a preparation process of high-purity quartz sand based on an acid leaching method, so as to solve the existing problems.
The preparation process of the high-purity quartz sand based on the acid leaching method adopts the following technical scheme:
One embodiment of the application provides a process for preparing high-purity quartz sand based on an acid leaching method, which comprises the following steps:
s1: sieving and grading the quartz sand raw ore, calcining at a high temperature, and then carrying out heat preservation treatment;
S2: performing primary acid leaching on the quartz sand treated in the step S1, and then placing the quartz sand into a light wave microwave oven for removing gas-liquid inclusion and infiltration treatment; the time of putting into the light wave microwave oven is adaptively adjusted, and the method specifically comprises the following steps:
(1) Acquiring quartz sand images at all moments in a light wave microwave oven; obtaining inclusion matching indexes of all pixel points in the quartz sand image at all times according to edge characteristics, texture characteristics and gray distribution characteristics of the pixel points in the quartz sand image;
(2) Obtaining inclusion cracking trend indexes at all times according to the inclusion matching indexes of all pixel points and the cracking degree differences of gas-liquid inclusion at different times;
(3) Determining the time for placing the optical wave microwave oven based on the inclusion cracking trend index at each moment;
s3: performing secondary acid leaching on the quartz sand treated in the step S2, and then placing the quartz sand into a hydrothermal reaction kettle for performing hydrothermal acid leaching treatment;
s4: and (3) cleaning the quartz sand treated in the step (S3) to be neutral by distilled water under the ultrasonic condition, and drying to obtain the high-purity quartz sand.
Preferably, the size of the quartz sand after sieving and grading in the step S1 is 120 meshes; the high-temperature calcination temperature is 1100-1300 ℃ and the time is 4-6 hours.
Preferably, the temperature of the heat preservation treatment is 900-1100 ℃ and the time is 3-4 hours.
Preferably, the acid solution of the primary acid leaching is mixed acid composed of 6% of sulfuric acid, 2% of hydrochloric acid and 10% of oxalic acid, and the temperature in the light wave microwave oven is 120-140 ℃.
Preferably, the inclusion matching index of each pixel point in the quartz sand image at each moment includes:
Constructing inclusion monitoring windows with preset sizes in quartz sand images by taking pixel points as centers, acquiring all connected areas of all edge pixel points in the inclusion monitoring windows, linearly fitting pixel coordinates of all pixel points in the connected areas to obtain fitting goodness and fitting slope of linear fitting, counting the number of connected areas with the fitting goodness being greater than or equal to a preset fitting goodness threshold value in the inclusion monitoring windows, and taking all connected areas with the number being greater than or equal to a preset value in the inclusion monitoring windows as areas to be detected of all cracking stripes;
aiming at the inclusion monitoring window, acquiring intersection points of linear fitting straight lines of all crack stripe to-be-detected areas as to-be-detected crack intersection points, and taking a minimum circumscribed rectangular area containing all to-be-detected crack intersection points as a crack center to-be-detected area;
quartz sand image The crack intersection point aggregation index of the a-th pixel point in the array is recorded asThe expression is:
In the method, in the process of the invention, Quartz sand imageThe number of crack crossing points to be detected in the inclusion monitoring window of the a-th pixel point,Representing quartz sand imagesEuclidean distance between the to-be-detected cracking intersection point c and the to-be-detected cracking intersection point d in the inclusion monitoring window of the a-th pixel point,Representing a preset coordination factor greater than 0,A quartz sand image at the time t is represented;
For inclusion monitoring windows of all pixel points, calculating entropy of gray level co-occurrence matrixes of a to-be-detected area of a cracking center in multiple directions, calculating average value and standard deviation of all the entropy, calculating sum value of the standard deviation and a preset first coordination factor, and taking the ratio of the average value to the sum value as intersection chaotic entropy of all the pixel points;
Calculating the product of the crack intersection point aggregation index of each pixel point and a preset first weight, marking the product as a first product, calculating the product of the intersection point chaotic entropy of each pixel point and a preset second weight, marking the product as a second product, and taking the sum of the first product and the second product as the inclusion matching index of each pixel point.
Preferably, the inclusion cracking trend index at each time includes:
dividing each pixel point into a gas-liquid inclusion pixel point and a non-gas-liquid inclusion pixel point by adopting a threshold segmentation algorithm in combination with inclusion matching indexes of each pixel point, and taking a region formed by all the gas-liquid inclusion pixel points as each gas-liquid inclusion region;
Calculating the sum result of gray values of all pixel points and a preset second coordination factor according to all gas-liquid inclusion areas, calculating the ratio of the inclusion matching index of all pixel points to the sum result, taking the sum value of the ratio of all pixel points in the gas-liquid inclusion areas as the inclusion cracking potential index of all gas-liquid inclusion areas, and taking the product of the average value of the inclusion cracking potential indexes of all gas-liquid inclusion areas in a quartz sand image and the maximum value of the inclusion cracking potential index as the inclusion cracking index of the quartz sand image;
And forming inclusion cracking index sequences of all the moments by using inclusion cracking indexes of quartz sand images at the preset number of the moments before each moment, obtaining p values of the inclusion cracking index sequences which are subjected to hypothesis test by using a hypothesis test algorithm, calculating Sigmoid function values of differences between each element and the previous element in the inclusion cracking index sequences, and taking products of sum values of all the Sigmoid function values and the p values as inclusion cracking trend indexes at all the moments.
Preferably, the determining the time for placing the optical wave microwave oven based on the inclusion cracking trend index at each moment includes:
And when the normalized inclusion cracking trend index at L continuous moments is smaller than or equal to a preset inclusion cracking trend index threshold, ending the processing in the light wave microwave oven, otherwise, continuing the processing in the light wave microwave oven, wherein L is a preset value.
Preferably, the acid solution of the secondary acid leaching is mixed acid composed of 12% of thioglycollic acid, 8% of sulfuric acid and 10% of sodium sulfide by mass fraction.
Preferably, the liquid-solid ratio of the mixed acid to the quartz sand is 3:1.
Preferably, in the hydrothermal acid leaching treatment, the volume ratio of the reactant to the hydrothermal reaction kettle is 1:5, the reaction temperature is 160-180 ℃, the reaction time is 2-5 hours, and the reaction pressure is 2-3 MPa.
The application has at least the following beneficial effects:
According to the application, the inclusion matching index is constructed by analyzing the shape and structure characteristics of the gas-liquid inclusion in the quartz sand, so that the degree that the pixel points accord with the characteristics of the gas-liquid inclusion is reflected, and the gas-liquid inclusion in the quartz sand can be identified more accurately; constructing an inclusion cracking potential index based on the inclusion matching index, reflecting the cracking degree of the gas-liquid inclusion, further constructing an inclusion cracking index, evaluating the integral cracking degree of the gas-liquid inclusion in the quartz sand image, and improving the accuracy of judging whether to finish the microwave treatment of the light wave or not; based on the inclusion cracking index, the degree of the gas-liquid inclusion change along with time is analyzed, and an inclusion cracking trend index is constructed, so that the cracking trend of the gas-liquid inclusion is reflected, whether the light wave microwave treatment should be ended or not is judged according to the cracking trend, the damage of minerals and crystal structures in the quartz sand is avoided, and the purity and quality of the prepared quartz sand are improved.
Drawings
In order to more clearly illustrate the embodiments of the application or the technical solutions and advantages of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are only some embodiments of the application, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a step flow chart of the acid leaching method-based high-purity quartz sand preparation process;
FIG. 2 is a flow chart of the time adjustment and control of the microwave processing of light waves.
Detailed Description
In order to further describe the technical means and effects adopted by the application to achieve the preset aim, the following is a detailed description of specific embodiments, structures, features and effects of the acid leaching method-based high-purity quartz sand preparation process according to the application with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "another embodiment" means that the embodiments are not necessarily the same. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
The specific scheme of the preparation process of the high-purity quartz sand based on the acid leaching method provided by the application is specifically described below with reference to the accompanying drawings.
The process for preparing high-purity quartz sand based on the acid leaching method provided by the embodiment of the application specifically provides the following process for preparing high-purity quartz sand based on the acid leaching method, referring to fig. 1, which comprises the following steps:
the specific process steps for preparing the high-purity quartz sand based on the acid leaching method in the application are as follows:
s1: and sieving and grading the quartz sand raw ore, calcining at a high temperature, and performing heat preservation treatment.
In the embodiment 1 of the application, the quartz sand raw ore is sieved and classified, 120-mesh quartz sand is put into a muffle furnace, high-temperature calcination treatment is carried out at 1100 ℃ for 4 hours, and then heat preservation treatment is carried out at 900 ℃ for 3 hours.
In the embodiment 2 of the application, the quartz sand raw ore is sieved and classified, 120-mesh quartz sand is put into a muffle furnace, high-temperature calcination treatment is carried out at 1200 ℃ for 5 hours, and then heat preservation treatment is carried out at 1000 ℃ for 3.5 hours.
In example 3 of the present application, a quartz sand raw ore was sieved and classified, 120 mesh quartz sand was put into a muffle furnace, high temperature calcination treatment was performed at 1300 ℃ for 6 hours, and then heat preservation treatment was performed at 1100 ℃ for 4 hours.
S2: and (3) carrying out primary acid leaching on the quartz sand treated in the step (S1), and then placing the quartz sand into a light wave microwave oven for removing gas-liquid inclusion and infiltration treatment.
In the embodiment 1 of the application, the quartz sand treated in the step S1 is subjected to primary acid leaching, wherein the acid solution is mixed acid consisting of 6% sulfuric acid, 2% hydrochloric acid and 10% oxalic acid by mass, and then the mixed acid is placed into a light wave microwave oven to be subjected to degassing liquid inclusion removal and infiltration treatment at the temperature of 120 ℃.
In the embodiment 2 of the application, the quartz sand treated in the step S1 is subjected to primary acid leaching, wherein the acid solution is mixed acid consisting of 6% sulfuric acid, 2% hydrochloric acid and 10% oxalic acid by mass, and then the mixed acid is placed into a light wave microwave oven to be subjected to degassing liquid inclusion removal and infiltration treatment at the temperature of 130 ℃.
In the embodiment 3 of the application, the quartz sand treated in the step S1 is subjected to primary acid leaching, wherein the acid solution is mixed acid consisting of 6% sulfuric acid, 2% hydrochloric acid and 10% oxalic acid by mass, and then the mixed acid is placed into a light wave microwave oven to be subjected to degassing liquid inclusion removal and infiltration treatment at the temperature of 140 ℃.
The treatment time of the step S2 in the light wave microwave oven is 2-4 hours; the time of putting into the light wave microwave oven is adaptively adjusted, and the method specifically comprises the following steps:
(1) Acquiring quartz sand images at all moments in a light wave microwave oven; and obtaining inclusion matching indexes of each pixel point in the quartz sand image at each moment according to the edge characteristics, the texture characteristics and the gray distribution characteristics of the pixel points in the quartz sand image.
And acquiring quartz sand images in the light wave microwave oven at equal time intervals T by an endoscopic high-temperature infrared imager in the oven, wherein the acquired images are gray images. In the present application, the time interval t=5 seconds can be set by the practitioner according to the actual situation, and the embodiment is not limited herein, and the collection is stopped until the light wave microwave processing is finished.
In the process of collecting images, noise exists in the collected images possibly caused by factors such as environmental interference, and in order to avoid the influence of the noise on the subsequent analysis process, as one embodiment of the application, the application uses a bilateral filtering algorithm to carry out denoising treatment on the collected images; meanwhile, in order to make the edge detail part in the image clearer, the application uses the CLAHE algorithm to enhance the quartz sand image. The bilateral filtering denoising algorithm and the CLAHE algorithm are known in the prior art, and the detailed process is not repeated.
It should be understood that this embodiment only proposes a method for image denoising and image enhancement, that is, image denoising is performed by using bilateral filtering, image enhancement is performed by using the CLAHE algorithm, and on the premise that the purposes of image denoising and image enhancement can be achieved, as other embodiments, an implementer may also use other feasible image denoising and image enhancement algorithms in the prior art to preprocess the quartz sand image, which is not limited in this application.
Thus, a pretreated quartz sand image was obtained.
In the original quartz ore, a certain amount of gas-liquid inclusion may exist, and the gas-liquid inclusion in the quartz ore refers to a tiny cavity in which gas or liquid is enclosed inside the quartz crystal. These inclusions are formed during the growth of the quartz mineral, and when the quartz crystal is formed, the surrounding gas or liquid is trapped inside the crystal, forming these tiny inclusions. When quartz sand is treated by the light wave microwave oven, the gas-liquid inclusion in the quartz sand absorbs energy in microwaves, so that the internal temperature is increased, the gas-liquid inclusion is expanded due to the temperature increase in the closed space, the gas-liquid inclusion can be gradually cracked by taking the weak part of the gas-liquid inclusion as the center, namely a plurality of cracking stripes which are diffused to the periphery by taking the weak part of the gas-liquid inclusion as the center can appear in a quartz sand image, and meanwhile, impurities in the gas-liquid inclusion are diffused from the cracking part, so that granular impurities exist around the gas-liquid inclusion.
Based on the analysis, the inclusion matching index is constructed, the degree that each pixel point in the quartz sand image accords with the bubble inclusion characteristics is reflected, and the inclusion matching index is constructed as follows:
quartz sand image at time t For example, quartz sand is imagedThe square window with the a-th pixel point as the center and the side length of b is recorded as an inclusion monitoring window, in this embodiment, b=9, and an implementer can set the window according to practical situations, the embodiment does not limit the window, and the gray value of the pixel point in the inclusion monitoring window is used as the input of a Canny edge detection algorithm, and the gray value is output as the edge pixel point in the inclusion monitoring window. Carrying out connected domain analysis on the output edge pixel points to obtainEdge communication areas respectively toAnd (3) performing linear fitting by taking pixel coordinates of pixel points in each edge communication area as input of a least square method to obtain a fitting straight line, and outputting a fitting goodness and a fitting slope of the linear fitting. The Canny edge detection algorithm, the least square method and the connected domain analysis are all existing known techniques, and the detailed process is not repeated.
As an embodiment of the present application, the practitioner may select other feasible edge detection algorithms to obtain the edge pixel points in the inclusion monitoring window by himself, which is not limited herein.
In the inclusion monitoring window, if the number of edge connected areas with the goodness of fit larger than or equal to the goodness of fit threshold is smaller than a preset valueIndicating that a stripe region conforming to the characteristics of the cracking stripe does not exist in the inclusion monitoring window; if the number of the edge connected areas with the goodness of fit larger than or equal to the goodness of fit threshold is larger than or equal to a preset valueAnd indicating that a stripe region which accords with the characteristics of the cracking stripe possibly exists in the inclusion monitoring window, and marking all edge communication regions in the inclusion monitoring window as the region to be detected of the cracking stripe. Wherein the goodness-of-fit threshold is taken to be 0.7 in the present application,The implementation can be set by the practitioner according to the actual situation, and the embodiment is not limited herein.
Aiming at the inclusion monitoring window, the intersection points of the fitting linear equation corresponding to the areas to be detected of the cracking stripes are respectively marked as a cracking intersection point 1 to be detected, cracking intersection points 2 and … to be detected and a cracking intersection point to be detected，Indicating the number of crack intersections to be detected. And (3) marking an area surrounded by the minimum circumscribed rectangle containing all the crack intersection points to be detected as a crack center area to be detected, and calculating entropy of the gray level co-occurrence matrix of 0 degree, 45 degree, 90 degree and 135 degree in the four directions of the crack center area to be detected. The calculation of the entropy of the gray level co-occurrence matrix is a known technology, and the detailed process is not repeated in the present application.
Preferably, as an embodiment of the present application, the inclusion matching index of each pixel point in the quartz sand image at each moment has the following expression:
In the method, in the process of the invention, Representing quartz sand imagesThe crack intersection point aggregation index of the a-th pixel point,Quartz sand imageThe number of crack crossing points to be detected in the inclusion monitoring window of the a-th pixel point,Representing quartz sand imagesEuclidean distance between the to-be-detected cracking intersection point c and the to-be-detected cracking intersection point d in the inclusion monitoring window of the a-th pixel point,Representing a coordination factor which is preset to be larger than 0 and is used for avoiding incapacitation caused by zero denominator, and in the applicationThe practitioner can set himself according to the actual situation, and the embodiment is not limited here;
Representing quartz sand images The intersection chaotic entropy of the a-th pixel point in the (a),AndRespectively represent quartz sand imagesThe mean value and standard deviation of the gray level co-occurrence matrix entropy in the four directions in the cracking center to-be-detected area in the a-th pixel inclusion monitoring window,Representing a preset coordination factor greater than 0, and marking the coordination factor as a first coordination factor for avoiding incapacitation caused by zero denominatorThe practitioner can set himself according to the actual situation, and the embodiment is not limited here;
Representing quartz sand images The inclusion matching index of the a-th pixel point in the list,AndWeights of the crack intersection point aggregation index and intersection point chaotic entropy are respectively expressed,The first weight is noted as a first weight,Recorded as the second weight, in the present application、The implementation can be set by the practitioner according to the actual situation, and the embodiment is not limited herein. Will beThe first product is noted as a first product,And is noted as the second product.
In quartz sand imageIn the inclusion monitoring window of the a-th pixel point, if the Euclidean distance between the crack crossing points to be detected is smaller, namelyThe smaller the crack stripe to be monitored is, the more likely the different crack stripe to be monitored areas are obtained by dispersing from one point to the periphery, and the more accords with the characteristics of the crack stripe, so the calculated crack intersection point aggregation index is larger; meanwhile, the larger the average value of the gray level co-occurrence matrix entropy in the four directions in the region to be detected of the cracking center corresponding to the cracking intersection point to be detected is, namelyThe larger the standard deviation of the gray level co-occurrence matrix entropy in the four directions is, the smallerThe smaller the distribution of the pixel gray values in the to-be-detected area of the cracking center is, the more chaotic the distribution of the pixel gray values is, the more the distribution is in accordance with the characteristic that impurities in the cracking center area leak out of the gas-liquid inclusion, and therefore the larger the calculated intersection chaotic entropy is. The greater the crack intersection point aggregation index and intersection point chaotic entropy, i.eAndThe larger the inclusion, the more consistent the shape and structure characteristics of the gas-liquid inclusion, so the larger the calculated inclusion matching index.
(2) And obtaining the inclusion cracking trend index at each moment according to the inclusion matching index of each pixel point and the cracking degree difference of the gas-liquid inclusion at different moments.
The inclusion matching index obtained through the steps reflects the degree that each pixel point in the quartz sand image accords with the bubble inclusion, namely the possibility that the pixel point belongs to the bubble inclusion, the inclusion matching index of all the pixel points in the quartz sand image can be used as input of an Ojin threshold segmentation method and output as an inclusion matching index threshold, the pixel point which is larger than or equal to the inclusion matching index threshold in the quartz sand image is used as a gas-liquid inclusion pixel point, and the pixel point which is smaller than the inclusion matching index threshold in the quartz sand image is used as a non-gas-liquid inclusion pixel point, so that the formed image is marked as a gas-liquid inclusion feature map. And sequentially carrying out morphological expansion treatment and connected domain analysis on the gas-liquid inclusion feature map, and marking the region formed by the treated gas-liquid inclusion pixel points as a gas-liquid inclusion region. The method for segmenting the Ojin threshold, morphological dilation and analyzing the connected domain are all known techniques in the prior art, and the detailed process is not repeated.
The gas-liquid inclusion region in the quartz sand image is obtained through the steps, if the microwave heating time is sufficient, the gas-liquid inclusion is completely cracked, obvious cracking stripes can appear, namely the cracking stripes are darker in color, and the microwave heating can be stopped, so that the next stage of treatment can be carried out; if the microwave heating time is insufficient, the pressure of the gas-liquid inclusion after being heated and expanded is insufficient to completely break through the quartz sand, so that the cracking stripes are relatively light, and the microwave heating is needed to be continued so as to completely remove the gas-liquid inclusion. Based on the analysis, the application constructs the inclusion cracking potential index based on the inclusion matching index, reflects the cracking degree of the gas-liquid inclusion, and has the following calculation formula:
In the method, in the process of the invention, Representing quartz sand imagesInclusion cleavage potential index of the e-th gas-liquid inclusion region,Representing quartz sand imagesThe number of pixel points in the e-th gas-liquid inclusion region,AndRespectively represent quartz sand imagesThe inclusion matching index and gray value of the f pixel point in the e-th gas-liquid inclusion region,Representing a preset coordination factor greater than 0, and marking the coordination factor as a second coordination factor for avoiding incapacitation caused by zero denominatorThe implementation can be set by the practitioner according to the actual situation, and the embodiment is not limited herein.
In quartz sand imageIn the medium gas-liquid inclusion region, the smaller the gray value of the pixel point is, namelySmaller indicates darker color, darker cracking stripes, i.e., greater cracking degree of the cracking stripes, and greater inclusion matching index of the pixels, i.eThe larger the pixel points are, the larger the degree that the pixel points accord with the characteristics of the gas-liquid inclusion is, namely, the more obvious the cracking degree of the gas-liquid inclusion is, so that the calculated inclusion cracking potential index is larger.
Imaging quartz sandTaking the product of the average value and the maximum value of inclusion cracking potential indexes of all gas-liquid inclusion as a quartz sand imageIs a inclusion cracking index. The greater the degree of cracking, the greater the calculated inclusion cracking index.
The inclusion cracking index of the quartz sand image at each moment can be calculated and obtained through the steps, the integral cracking degree of the gas-liquid inclusion in the quartz sand at each moment is reflected, and in order to avoid the situation that the position of part of the gas-liquid inclusion in the quartz sand is deeper, the cracking characteristic of the gas-liquid inclusion can not appear in short-time microwave heating, so that misjudgment is caused on the removing degree of the gas-liquid inclusion, and the purity of the finally prepared quartz sand is affected. The application constructs inclusion cracking trend index based on inclusion cracking index, reflects the cracking trend of gas-liquid inclusion at each moment, and the construction process of the inclusion cracking trend index is as follows:
The sequence formed by the inclusion cracking indexes at the first g times of the t time is recorded as an inclusion cracking index sequence, in this embodiment, g=10, and the embodiment can be set by the practitioner according to practical situations, and the embodiment is not limited herein, and if the number of times before the t time is less than g, the sequence is complemented by a regression filling method, so that the length of the inclusion cracking index sequence is g. The inclusion cracking index sequence is used as input of a Wilcoxon hypothesis test, the original hypothesis is that the inclusion cracking index sequence has an ascending trend, and the p value of the hypothesis test is output. The regression filling method and the Wilcoxon hypothesis test are all known techniques, and the specific process is not repeated. From this, the inclusion cracking trend index at each time was calculated as:
In the method, in the process of the invention, The inclusion cracking trend index at time t is shown,The p value representing the hypothesis test of the inclusion cracking index sequence at time t, g representing the length of the inclusion cracking index sequence, sig () representing the Sigmoid function,AndThe values of the ith element and the ith-1 element in the inclusion cracking index sequence at the time t are respectively shown.
The greater the p-value of the inclusion cracking index sequence hypothesis test, i.eThe larger the inclusion cracking index sequence, the more obvious the ascending trend exists, namely the cracking degree of gas-liquid inclusion in quartz sand becomes larger gradually, the more obvious the cracking trend is, and the greater the cracking index of inclusion becomes with time change, namelyThe larger the silica sand, the larger the degree of cracking of the gas-liquid inclusion in the silica sand, so the calculated inclusion cracking trend index is larger.
(3) And determining the time of putting the quartz sand into the light wave microwave oven based on the inclusion cracking trend index at each moment.
The inclusion cracking trend index at each moment can be obtained through the steps, the cracking trend of the gas-liquid inclusion at each moment is reflected, the inclusion cracking trend index at each moment is normalized by using the Z-score method, the normalized inclusion cracking trend index is obtained, if the normalized inclusion cracking trend index is smaller than an inclusion cracking trend index threshold value, the gas-liquid inclusion in quartz sand is basically removed, wherein the inclusion cracking trend index threshold value is 0.2, an implementer can set the inclusion cracking trend index according to actual conditions, and the embodiment is not limited herein. In order to avoid misjudgment of quartz sand images at individual moments, the application judges that the normalized inclusion cracking trend index at continuous L moments is smaller than an inclusion cracking trend index threshold as a condition for ending the microwave processing of the light waves, namely the normalized inclusion cracking trend index at continuous L moments is smaller than or equal to the inclusion cracking trend index threshold, which indicates that the gas-liquid inclusion in the quartz sand is basically removed, and the processing of the light wave microwave processing stage should be ended for the next stage. In the present application, l=10, and the practitioner can set the settings according to the actual situation, and the present embodiment is not limited herein.
Thus, the quartz sand after the light wave microwave treatment is obtained, and a light wave microwave treatment time regulation flow chart is shown in figure 2.
S3: and (3) carrying out secondary acid leaching on the quartz sand treated by the S2, and then placing the quartz sand into a hydrothermal reaction kettle for hydrothermal acid leaching treatment.
In the embodiment 1 of the application, the quartz sand treated by the S2 is placed in a hydrothermal reaction kettle containing an acid solution for secondary acid leaching, and is placed in a blast drying box for hydrothermal acid leaching treatment, wherein the acid solution is mixed acid consisting of 12% of thioglycollic acid, 8% of sulfuric acid and 10% of sodium sulfide by mass, the volume solid-liquid ratio of the quartz sand to the mixed acid is 1:3, the volume ratio of reactants to the hydrothermal reaction kettle is 1:5, the reaction temperature is 160 ℃, the reaction time is 2 hours, and the reaction pressure is 2MPa.
In the embodiment 2 of the application, the quartz sand treated by the S2 is placed in a hydrothermal reaction kettle containing an acid solution for secondary acid leaching, and is placed in a blast drying box for hydrothermal acid leaching treatment, wherein the acid solution is mixed acid consisting of 12% of thioglycollic acid, 8% of sulfuric acid and 10% of sodium sulfide by mass, the volume solid-liquid ratio of the quartz sand to the mixed acid is 1:3, the volume ratio of reactants to the hydrothermal reaction kettle is 1:5, the reaction temperature is 170 ℃, the reaction time is 3.5 hours, and the reaction pressure is 2.5MPa.
In the embodiment 3 of the application, the quartz sand treated by the S2 is placed in a hydrothermal reaction kettle containing an acid solution for secondary acid leaching, and is placed in a blast drying box for hydrothermal acid leaching treatment, wherein the acid solution is mixed acid consisting of 12% of thioglycollic acid, 8% of sulfuric acid and 10% of sodium sulfide by mass, the volume solid-liquid ratio of the quartz sand to the mixed acid is 1:3, the volume ratio of reactants to the hydrothermal reaction kettle is 1:5, the reaction temperature is 180 ℃, the reaction time is 5 hours, and the reaction pressure is 3MPa.
S4: and (3) repeatedly flushing the quartz sand treated in the step (S3) to be neutral by distilled water under the ultrasonic condition, and drying to obtain the high-purity quartz sand.
ICP-MS analysis and detection are carried out on the content of silicon dioxide and impurity metals in the high-purity quartz sand prepared according to the steps, and the detection result of the example 1 is shown in the components and the content of the high-purity quartz sand in table 1.
TABLE 1
The results of the test in example 2 are shown in Table 2, which shows the components and contents of the high purity silica sand.
TABLE 2
The results of the test in example 3 are shown in Table 3, which shows the components and contents of the high purity silica sand.
TABLE 3 Table 3
It should be noted that: the sequence of the embodiments of the present application is only for description, and does not represent the advantages and disadvantages of the embodiments. And the foregoing description has been directed to specific embodiments of this specification. In addition, the processes depicted in the accompanying figures do not necessarily require the particular order shown, or sequential order, to achieve desirable results. In some embodiments, multitasking and parallel processing are also possible or may be advantageous.
In this specification, each embodiment is described in a progressive manner, and the same or similar parts of each embodiment are referred to each other, and each embodiment mainly describes differences from other embodiments.
The above embodiments are only for illustrating the technical solution of the present application, and not for limiting the same; the technical solutions described in the foregoing embodiments are modified or some of the technical features are replaced equivalently, so that the essence of the corresponding technical solutions does not deviate from the scope of the technical solutions of the embodiments of the present application, and all the technical solutions are included in the protection scope of the present application.
Claims (10)
1. The preparation process of the high-purity quartz sand based on the acid leaching method is characterized by comprising the following steps of:
s1: sieving and grading the quartz sand raw ore, calcining at a high temperature, and then carrying out heat preservation treatment;
S2: performing primary acid leaching on the quartz sand treated in the step S1, and then placing the quartz sand into a light wave microwave oven for removing gas-liquid inclusion and infiltration treatment; the time of putting into the light wave microwave oven is adaptively adjusted, and the method specifically comprises the following steps:
(1) Acquiring quartz sand images at all moments in a light wave microwave oven; obtaining inclusion matching indexes of all pixel points in the quartz sand image at all times according to edge characteristics, texture characteristics and gray distribution characteristics of the pixel points in the quartz sand image;
(2) Obtaining inclusion cracking trend indexes at all times according to the inclusion matching indexes of all pixel points and the cracking degree differences of gas-liquid inclusion at different times;
(3) Determining the time for placing the optical wave microwave oven based on the inclusion cracking trend index at each moment;
s3: performing secondary acid leaching on the quartz sand treated in the step S2, and then placing the quartz sand into a hydrothermal reaction kettle for performing hydrothermal acid leaching treatment;
s4: and (3) cleaning the quartz sand treated in the step (S3) to be neutral by distilled water under the ultrasonic condition, and drying to obtain the high-purity quartz sand.
2. The process for preparing high-purity silica sand based on acid leaching method according to claim 1, wherein the size of the silica sand after sieving and classifying in S1 is 120 mesh; the high-temperature calcination temperature is 1100-1300 ℃ and the time is 4-6 hours.
3. The process for preparing high-purity quartz sand based on the acid leaching method according to claim 1, wherein the temperature of the heat preservation treatment is 900-1100 ℃ and the time is 3-4 hours.
4. The process for preparing high-purity quartz sand based on the acid leaching method according to claim 1, wherein the acid solution of the primary acid leaching is mixed acid consisting of 6% of sulfuric acid, 2% of hydrochloric acid and 10% of oxalic acid by mass, and the temperature in the light wave microwave oven is 120-140 ℃.
5. The process for preparing high-purity quartz sand based on acid leaching method according to claim 1, wherein the inclusion matching index of each pixel point in the quartz sand image at each moment comprises:
Constructing inclusion monitoring windows with preset sizes in quartz sand images by taking pixel points as centers, acquiring all connected areas of all edge pixel points in the inclusion monitoring windows, linearly fitting pixel coordinates of all pixel points in the connected areas to obtain fitting goodness and fitting slope of linear fitting, counting the number of connected areas with the fitting goodness being greater than or equal to a preset fitting goodness threshold value in the inclusion monitoring windows, and taking all connected areas with the number being greater than or equal to a preset value in the inclusion monitoring windows as areas to be detected of all cracking stripes;
aiming at the inclusion monitoring window, acquiring intersection points of linear fitting straight lines of all crack stripe to-be-detected areas as to-be-detected crack intersection points, and taking a minimum circumscribed rectangular area containing all to-be-detected crack intersection points as a crack center to-be-detected area;
quartz sand image The crack intersection point aggregation index of the a-th pixel point in the array is recorded asThe expression is:
In the method, in the process of the invention, Quartz sand imageThe number of crack crossing points to be detected in the inclusion monitoring window of the a-th pixel point,Representing quartz sand imagesEuclidean distance between the to-be-detected cracking intersection point c and the to-be-detected cracking intersection point d in the inclusion monitoring window of the a-th pixel point,Representing a preset coordination factor greater than 0,A quartz sand image at the time t is represented;
For inclusion monitoring windows of all pixel points, calculating entropy of gray level co-occurrence matrixes of a to-be-detected area of a cracking center in multiple directions, calculating average value and standard deviation of all the entropy, calculating sum value of the standard deviation and a preset first coordination factor, and taking the ratio of the average value to the sum value as intersection chaotic entropy of all the pixel points;
Calculating the product of the crack intersection point aggregation index of each pixel point and a preset first weight, marking the product as a first product, calculating the product of the intersection point chaotic entropy of each pixel point and a preset second weight, marking the product as a second product, and taking the sum of the first product and the second product as the inclusion matching index of each pixel point.
6. The process for preparing high purity silica sand based on acid leaching as claimed in claim 1, wherein the inclusion cracking trend index at each time comprises:
dividing each pixel point into a gas-liquid inclusion pixel point and a non-gas-liquid inclusion pixel point by adopting a threshold segmentation algorithm in combination with inclusion matching indexes of each pixel point, and taking a region formed by all the gas-liquid inclusion pixel points as each gas-liquid inclusion region;
Calculating the sum result of gray values of all pixel points and a preset second coordination factor according to all gas-liquid inclusion areas, calculating the ratio of the inclusion matching index of all pixel points to the sum result, taking the sum value of the ratio of all pixel points in the gas-liquid inclusion areas as the inclusion cracking potential index of all gas-liquid inclusion areas, and taking the product of the average value of the inclusion cracking potential indexes of all gas-liquid inclusion areas in a quartz sand image and the maximum value of the inclusion cracking potential index as the inclusion cracking index of the quartz sand image;
And forming inclusion cracking index sequences of all the moments by using inclusion cracking indexes of quartz sand images at the preset number of the moments before each moment, obtaining p values of the inclusion cracking index sequences which are subjected to hypothesis test by using a hypothesis test algorithm, calculating Sigmoid function values of differences between each element and the previous element in the inclusion cracking index sequences, and taking products of sum values of all the Sigmoid function values and the p values as inclusion cracking trend indexes at all the moments.
7. The process for preparing high purity silica sand based on acid leaching according to claim 1, wherein the determining the time of putting into the light wave microwave oven based on the inclusion cracking trend index at each time comprises:
And when the normalized inclusion cracking trend index at L continuous moments is smaller than or equal to a preset inclusion cracking trend index threshold, ending the processing in the light wave microwave oven, otherwise, continuing the processing in the light wave microwave oven, wherein L is a preset value.
8. The process for preparing high-purity quartz sand based on acid leaching method according to claim 1, wherein the acid solution of the secondary acid leaching is mixed acid composed of 12% thioglycollic acid, 8% sulfuric acid and 10% sodium sulfide by mass fraction.
9. The process for preparing high-purity silica sand according to claim 8, wherein the liquid-solid ratio of the mixed acid to the silica sand is 3:1.
10. The process for preparing high-purity quartz sand based on the acid leaching method according to claim 1, wherein in the hydrothermal acid leaching treatment, the volume ratio of reactants to a hydrothermal reaction kettle is 1:5, the reaction temperature is 160-180 ℃, the reaction time is 2-5 hours, and the reaction pressure is 2-3 MPa.
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