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CN117401686A - Quartz sand microwave purification device, purification method and high-purity quartz sand - Google Patents

Quartz sand microwave purification device, purification method and high-purity quartz sand Download PDF

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Publication number
CN117401686A
CN117401686A CN202311365589.0A CN202311365589A CN117401686A CN 117401686 A CN117401686 A CN 117401686A CN 202311365589 A CN202311365589 A CN 202311365589A CN 117401686 A CN117401686 A CN 117401686A
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microwave
quartz sand
ellipsoidal cavity
purification
generating mechanism
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李勇
赵小玻
王玉宝
林清莲
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Sinoma Intraocular Lens Research Institute Shandong Co ltd
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Sinoma Intraocular Lens Research Institute Shandong Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention provides a quartz sand microwave purification device, a purification method and high-purity quartz sand. The device comprises a microwave generating mechanism, a material placing mechanism and a shell, wherein an ellipsoidal cavity is formed by enclosing the inner wall of the shell, the device comprises an upper shell and a lower shell which are detachably connected, the upper shell is provided with an air outlet pipe and a feeding pipe which extend into the ellipsoidal cavity, and a material placing mechanism positioning piece is arranged at the position, corresponding to a long half shaft of the ellipsoidal cavity, of the lower shell; the microwave generating mechanism stretches into the ellipsoidal cavity from the position of the upper shell corresponding to the long half shaft of the ellipsoidal cavity, and the microwave generating position of the microwave generating mechanism is positioned at the upper focus of the ellipsoidal cavity; the material placing mechanism comprises a material carrying disc with an opening at the bottom and a storage groove connected with the material carrying disc and positioned below the material carrying disc. According to the invention, through the design of matching the ellipsoidal cavity double-focus structure with the microwave generation position of the microwave generation mechanism, the material carrying tray, the material storage groove and the like, the microwave-water quenching-acid washing integration is realized, the microwave utilization rate and the heating efficiency are improved, the purification efficiency is improved, the energy consumption is low, and the cost is low.

Description

一种石英砂微波提纯装置、提纯方法及高纯石英砂A quartz sand microwave purification device, purification method and high-purity quartz sand

技术领域Technical Field

本发明涉及石英砂提纯技术领域,具体而言,涉及一种石英砂微波提纯装置、提纯方法及高纯石英砂。The invention relates to the technical field of quartz sand purification, and in particular to a quartz sand microwave purification device, a purification method and high-purity quartz sand.

背景技术Background Art

高纯石英砂是光伏、半导体、通讯、国防军工等高端制造行业的基础原材料,随着这些应用领域的快速发展,优质高纯天然石英资源已供不应求,采用普通低品级天然石英矿进行深度提纯成为获取高纯石英砂的主流方向。然而,普通天然石英矿石受岩浆运动以及地质条件等的影响,杂质含量和分布、流体包裹物类型和化学元素等指标各不相同,不同地区甚至同一地区的石英矿石品质不均一,在一定的提纯周期下,现有提纯技术提纯后得到的石英砂品质不一,提纯后的石英砂很多都无法满足光伏、半导体、通讯、国防军工等高端制造行业的使用要求,要想达到所需要求,就需要延长提纯周期,能耗大,成本高,甚至于即使延长提纯周期也无法获得满足光伏、半导体、通讯、国防军工等高端制造行业使用要求的石英砂。因此,本领域亟需一种能耗小、成本低且可高效提纯的石英砂提纯方法和可实现该提纯方法的提纯装置。High-purity quartz sand is the basic raw material for high-end manufacturing industries such as photovoltaics, semiconductors, communications, and national defense and military industries. With the rapid development of these application fields, high-quality and high-purity natural quartz resources are in short supply, and deep purification of ordinary low-grade natural quartz ores has become the mainstream direction for obtaining high-purity quartz sand. However, ordinary natural quartz ores are affected by magma movement and geological conditions, and the impurity content and distribution, fluid inclusion types, and chemical elements are different. The quality of quartz ores in different regions or even in the same region is not uniform. Under a certain purification cycle, the quality of quartz sand obtained after purification by existing purification technology is different. Many of the purified quartz sands cannot meet the use requirements of high-end manufacturing industries such as photovoltaics, semiconductors, communications, and national defense and military industries. In order to meet the required requirements, it is necessary to extend the purification cycle, which consumes a lot of energy and has high costs. Even if the purification cycle is extended, it is still impossible to obtain quartz sand that meets the use requirements of high-end manufacturing industries such as photovoltaics, semiconductors, communications, and national defense and military industries. Therefore, there is an urgent need in the art for a quartz sand purification method with low energy consumption, low cost and high efficiency, and a purification device that can implement the purification method.

发明内容Summary of the invention

本发明提供了一种石英砂微波提纯装置、提纯方法及高纯石英砂,以解决现有石英砂提纯方法能耗大、成本高、提纯效率低等问题。The invention provides a quartz sand microwave purification device, a purification method and high-purity quartz sand, so as to solve the problems of high energy consumption, high cost and low purification efficiency in the existing quartz sand purification method.

一方面,本发明提供了一种石英砂微波提纯装置,包括微波发生机构、置料机构和壳体,所述壳体的内壁围成椭球形腔体,壳体包括上壳体和下壳体,上壳体和下壳体可拆卸连接,上壳体设有伸入椭球形腔体内的出气管和若干伸入椭球形腔体内的进料管,下壳体对应于椭球形腔体长半轴的位置设有置料机构定位件;所述微波发生机构自上壳体对应于椭球形腔体长半轴的位置伸入椭球形腔体内,微波发生机构的微波发生位置位于椭球形腔体的上焦点;所述置料机构包括载料盘和位于载料盘下方的储物槽,载料盘与储物槽连接,载料盘底部设有开孔。On the one hand, the present invention provides a quartz sand microwave purification device, comprising a microwave generating mechanism, a feeding mechanism and a shell, the inner wall of the shell forms an ellipsoidal cavity, the shell comprises an upper shell and a lower shell, the upper shell and the lower shell are detachably connected, the upper shell is provided with an air outlet pipe extending into the ellipsoidal cavity and a plurality of feeding pipes extending into the ellipsoidal cavity, the lower shell is provided with a feeding mechanism positioning piece at a position corresponding to the long semi-axis of the ellipsoidal cavity; the microwave generating mechanism extends into the ellipsoidal cavity from the position of the upper shell corresponding to the long semi-axis of the ellipsoidal cavity, and the microwave generating position of the microwave generating mechanism is located at the upper focus of the ellipsoidal cavity; the feeding mechanism comprises a loading tray and a storage trough located below the loading tray, the loading tray is connected to the storage trough, and an opening is provided at the bottom of the loading tray.

与现有技术相比,本发明具有以下有益效果:本发明提纯装置壳体具备椭球形腔体,通过椭球形腔体的双焦点结构,配合微波发生机构微波发生位置,将微波发生位置设于椭球形腔体的上焦点,微波发生机构启动后,微波自上焦点的微波发生位置射出,在椭球腔体内反射后,最终会汇聚到椭球形腔体的下焦点位置,实现高频率、高功率、低损耗的微波传输,下焦点处微波接收率接近100%,基于不同微波频率的特定波长,以下焦点为中心,形成不同大小的微波等离子体球形区域,配合载料盘位置,微波等离子体球形区域覆盖载料盘盛料区,最大效率的对载料盘中的石英砂进行加热,使得石英砂迅速升温,提高微波利用率和加热效率,能耗小且成本低,在此基础上借助微波等离子体选择加热的作用,石英砂中气液包裹体等杂质的温度和压力急剧上升,促使杂质爆裂或在杂质与石英砂基体的界面处产生微裂纹,在极短的时间内使得石英砂状态达到水粹要求,配合储物槽(储物槽可存储酸溶液)等的设计,产生微裂纹的的石英砂落入储物槽中存储的酸溶液中,经水淬促使气液包裹体等杂质的微裂纹延伸并通过酸洗对气液包裹体中杂质进行去除,大大节省了时间成本,实现微波-水淬-酸洗一体化,提高了提纯效率,且也可配合氯化处理,在借助微波对石英砂迅速升温后进行氯化处理,提高提纯效果。Compared with the prior art, the present invention has the following beneficial effects: the shell of the purification device of the present invention has an ellipsoidal cavity, and through the dual-focus structure of the ellipsoidal cavity, the microwave generating position is set at the upper focus of the ellipsoidal cavity in coordination with the microwave generating position of the microwave generating mechanism. After the microwave generating mechanism is started, the microwave is emitted from the microwave generating position of the upper focus, and after being reflected in the ellipsoidal cavity, it will eventually converge to the lower focus position of the ellipsoidal cavity, thereby realizing high-frequency, high-power, and low-loss microwave transmission. The microwave receiving rate at the lower focus is close to 100%. Based on the specific wavelengths of different microwave frequencies, microwave plasma spherical areas of different sizes are formed with the lower focus as the center. In coordination with the position of the loading tray, the microwave plasma spherical area covers the material holding area of the loading tray, and the quartz sand in the loading tray is heated with the greatest efficiency, so that the quartz sand is rapidly heated. The temperature is raised to improve the microwave utilization rate and heating efficiency, with low energy consumption and low cost. On this basis, with the help of the selective heating effect of microwave plasma, the temperature and pressure of impurities such as gas-liquid inclusions in quartz sand rise sharply, causing the impurities to burst or generate microcracks at the interface between the impurities and the quartz sand matrix, so that the quartz sand state meets the water purification requirements in a very short time. With the design of the storage tank (the storage tank can store acid solution), the quartz sand with microcracks falls into the acid solution stored in the storage tank, and the microcracks of impurities such as gas-liquid inclusions are extended through water quenching, and the impurities in the gas-liquid inclusions are removed through acid washing, which greatly saves time and cost, realizes the integration of microwave-water quenching-acid washing, and improves the purification efficiency. It can also be combined with chlorination treatment, and chlorination treatment is performed after the quartz sand is rapidly heated with the help of microwaves to improve the purification effect.

在本发明的一些实施方式中,所述上壳体和下壳体的开口端均设有法兰盘,上壳体和下壳体通过法兰盘上的安装开孔借助螺栓螺母结构连接;和/或,所述进料管伸入椭球形腔体内的一端朝向椭球形腔体的下焦点;和/或,所述置料机构定位件为凹槽状,置料机构定位件的形状与储物槽外表面相匹配,储物槽可嵌入置料机构定位件中。法兰盘方便上壳体和下壳体的连接与拆卸;进料管朝向椭球形腔体的下焦点方便控制料的输入方向,方便将石英砂通入载料盘,且便于石英砂与通入气体的充分接触。置料机构定位件方便实现置料机构的定位。In some embodiments of the present invention, the open ends of the upper shell and the lower shell are both provided with flanges, and the upper shell and the lower shell are connected by means of bolt and nut structures through the mounting openings on the flanges; and/or, one end of the feed pipe extending into the ellipsoidal cavity faces the lower focus of the ellipsoidal cavity; and/or, the positioning piece of the feeding mechanism is in the shape of a groove, and the shape of the positioning piece of the feeding mechanism matches the outer surface of the storage tank, and the storage tank can be embedded in the positioning piece of the feeding mechanism. The flange facilitates the connection and disassembly of the upper shell and the lower shell; the feed pipe faces the lower focus of the ellipsoidal cavity, which facilitates the control of the input direction of the material, facilitates the passage of quartz sand into the loading tray, and facilitates the full contact between the quartz sand and the introduced gas. The positioning piece of the feeding mechanism facilitates the positioning of the feeding mechanism.

在本发明的一些实施方式中,所述微波发生机构采用2.45GHz的固态微波源或915MHz的固态微波源;当将置料机构借助储物槽置于置料机构定位件时,置料机构位于椭球形腔体的长半轴上;且当微波发生机构采用2.45GHz的固态微波源时,载料盘的上表面距离椭球形腔体的下焦点的距离为30~45mm,5cm≤载料盘上端面的直径≤10cm;当微波发生机构采用915MHz的固态微波源时,载料盘的上表面距离椭球形腔体的下焦点的距离为75~125mm,5cm≤载料盘上端面的直径≤15cm。采用2.45GHz的固态微波源或915MHz的固态微波源,微波加热效果更好,更有利于石英砂急速升温。采用2.45GHz的固态微波源时,对应波长为12.24cm,以下焦点为中心的微波等离子体球的直径Dmax=λ/2=6.12cm,将载料盘上表面距离椭球形腔体下焦点的距离设计为30~45mm的同时满足5cm≤载料盘上端面的直径≤10cm,可以使微波等离子体球形区域覆盖载料盘盛料区,最大效率的对载料盘中的石英砂进行加热。当采用915MHz的固态微波源时,对应波长为33cm,以下焦点为中心的微波等离子体球的直径Dmax=λ/2=16.5cm,将载料盘上表面距离椭球形腔体下焦点的距离设计为75~125mm的同时满足5cm≤载料盘上端面的直径≤15cm,可以使微波等离子体球形区域覆盖载料盘盛料区,最大效率的对载料盘中的石英砂进行加热。In some embodiments of the present invention, the microwave generating mechanism adopts a 2.45GHz solid-state microwave source or a 915MHz solid-state microwave source; when the material placing mechanism is placed on the material placing mechanism positioning member by means of the storage tank, the material placing mechanism is located on the long semi-axis of the ellipsoidal cavity; and when the microwave generating mechanism adopts a 2.45GHz solid-state microwave source, the distance between the upper surface of the material loading plate and the lower focus of the ellipsoidal cavity is 30 to 45mm, and 5cm≤the diameter of the upper end surface of the material loading plate≤10cm; when the microwave generating mechanism adopts a 915MHz solid-state microwave source, the distance between the upper surface of the material loading plate and the lower focus of the ellipsoidal cavity is 75 to 125mm, and 5cm≤the diameter of the upper end surface of the material loading plate≤15cm. Using a 2.45GHz solid-state microwave source or a 915MHz solid-state microwave source, the microwave heating effect is better and more conducive to the rapid heating of quartz sand. When a 2.45GHz solid-state microwave source is used, the corresponding wavelength is 12.24cm, and the diameter of the microwave plasma sphere centered on the lower focus is Dmax=λ/2=6.12cm. The distance between the upper surface of the loading plate and the lower focus of the ellipsoidal cavity is designed to be 30-45mm while satisfying 5cm≤the diameter of the upper end face of the loading plate≤10cm, so that the microwave plasma spherical area can cover the loading plate holding area, and the quartz sand in the loading plate can be heated with maximum efficiency. When a 915MHz solid-state microwave source is used, the corresponding wavelength is 33cm, and the diameter of the microwave plasma sphere centered on the lower focus is Dmax=λ/2=16.5cm. The distance between the upper surface of the loading plate and the lower focus of the ellipsoidal cavity is designed to be 75-125mm while satisfying 5cm≤the diameter of the upper end face of the loading plate≤15cm, so that the microwave plasma spherical area can cover the loading plate holding area, and the quartz sand in the loading plate can be heated with maximum efficiency.

在本发明的一些实施方式中,所述载料盘与储物槽可拆卸连接,载料盘外表面间隔设有载料盘连接座,储物槽上部间隔设有储物槽连接座,载料盘连接座和储物槽连接座上均设有安装通孔,载料盘与储物槽可通过不同规格的弹性件借助安装通孔连接。载料盘与储物槽可拆卸连接,方便更换不同长度规格的弹性件调整载料盘与储物槽之间的距离,进而实现对载料盘上表面距离椭球形腔体下焦点的距离调整。In some embodiments of the present invention, the loading tray is detachably connected to the storage tank, a loading tray connection seat is provided at intervals on the outer surface of the loading tray, a storage tank connection seat is provided at intervals on the upper part of the storage tank, and both the loading tray connection seat and the storage tank connection seat are provided with mounting through holes, and the loading tray and the storage tank can be connected by elastic members of different specifications via the mounting through holes. The loading tray and the storage tank are detachably connected, which facilitates the replacement of elastic members of different lengths to adjust the distance between the loading tray and the storage tank, thereby achieving the adjustment of the distance between the upper surface of the loading tray and the lower focus of the ellipsoidal cavity.

在本发明的一些实施方式中,所述载料盘下方还连接有下料通道,所述下料通道与载料盘底部的开孔连通,下料通道的长度≤20cm;所述开孔处设有开孔开关,所述下料通道上设有振动机构。下料通道为石英砂下落到储物槽提供通道,防止石英砂自开孔直接掉落导致石英砂四散无法落入储物槽;下料通道的长度≤20cm则可防止下落距离较远导致降温过大影响水粹酸洗效果;开孔开关可控制开孔的开启与否,当石英砂被加热到所需温度后再开启,方便对下落时石英砂温度的控制;振动机构提供载料盘振动功能,通过振动实现石英砂在载料盘上均匀平铺和顺路下落,以利于控制石英砂经微波等离子体处理的时间和温度。In some embodiments of the present invention, a feeding channel is also connected below the loading tray, and the feeding channel is connected to the opening at the bottom of the loading tray, and the length of the feeding channel is ≤20cm; an opening switch is provided at the opening, and a vibration mechanism is provided on the feeding channel. The feeding channel provides a channel for the quartz sand to fall into the storage tank, preventing the quartz sand from falling directly from the opening, causing the quartz sand to scatter and be unable to fall into the storage tank; the length of the feeding channel is ≤20cm, which can prevent the long falling distance from causing excessive cooling and affecting the water pickling effect; the opening switch can control whether the opening is opened or not, and it is opened after the quartz sand is heated to the required temperature, which is convenient for controlling the temperature of the quartz sand when falling; the vibration mechanism provides the loading tray with a vibration function, and the quartz sand is evenly spread on the loading tray and falls along the way through vibration, so as to control the time and temperature of the quartz sand after microwave plasma treatment.

另一方面,本发明还提供了一种石英砂微波提纯方法,包括以下步骤:S1、破碎-筛分处理:对石英矿石进行破碎、筛分,得到预设尺寸的石英原砂;S2、初始提纯处理:通过包括磁选、浮选、酸洗的提纯方式对所述石英原砂进行初始提纯;S3、微波-水粹-酸洗一体化提纯处理:应用上述任一项所述的石英砂微波提纯装置,将酸溶液置于储物槽中,将置料机构置于下壳体的置料机构定位件上,封闭上壳体和下壳体以使椭球形腔体处于密封状态,通过出气管抽真空至椭球形腔体内的气压达到第一预设气压后,通过进料管向椭球形腔体内通入HCl气体直至椭球形腔体内的气压达到第二预设气压,启动微波发生机构,分别通过不同进料管向椭球形腔体内通入HCl气体和上一步提纯后得到的石英砂,石英砂落入载料盘并由微波发生机构加热后通过开孔落入储物槽的酸溶液中进行水粹酸洗;S4、微波-氯化提纯处理:应用另一上述任一项所述的石英砂微波提纯装置,将置料机构置于下壳体的置料机构定位件上,封闭上壳体和下壳体以使椭球形腔体处于密封状态,通过出气管抽真空至椭球形腔体内的气压达到第三预设气压后,自S3应用的石英砂微波提纯装置的出气管抽出其椭球形腔体内的气体,将抽出的气体通过S4应用的石英砂微波提纯装置的任一进料管通入椭球形腔体内,同时通过其他进料管向椭球形腔体内通入O2和Cl2,直至椭球形腔体内的气压达到第四预设气压,启动微波发生机构,分别通过不同进料管向椭球形腔体内通入抽出的气体、O2、Cl2和上一步提纯后得到的石英砂,石英砂落入载料盘并由微波发生机构加热后通过开孔落入储物槽中,完成微波-氯化提纯处理。On the other hand, the present invention also provides a quartz sand microwave purification method, comprising the following steps: S1, crushing-screening treatment: crushing and screening the quartz ore to obtain quartz raw sand of a preset size; S2, initial purification treatment: initially purifying the quartz raw sand by a purification method including magnetic separation, flotation, and acid washing; S3, microwave-water purification-acid washing integrated purification treatment: using any of the above-mentioned quartz sand microwave purification devices, placing an acid solution in a storage tank, placing a feeding mechanism on a feeding mechanism positioning member of a lower shell, closing the upper shell and the lower shell to make the ellipsoidal cavity in a sealed state, evacuating the ellipsoidal cavity through an air outlet pipe until the air pressure in the ellipsoidal cavity reaches a first preset air pressure, introducing HCl gas into the ellipsoidal cavity through a feed pipe until the air pressure in the ellipsoidal cavity reaches a second preset air pressure, and starting the microwave generator. S4, microwave-chlorination purification treatment: using another quartz sand microwave purification device described in any one of the above items, placing the feeding mechanism on the feeding mechanism positioning member of the lower shell, closing the upper shell and the lower shell to make the ellipsoidal cavity in a sealed state, and after vacuuming the ellipsoidal cavity through the air outlet pipe until the air pressure in the ellipsoidal cavity reaches a third preset air pressure, extracting the gas in the ellipsoidal cavity from the air outlet pipe of the quartz sand microwave purification device applied in S3, and passing the extracted gas into the ellipsoidal cavity through any feeding pipe of the quartz sand microwave purification device applied in S4, and at the same time, introducing O into the ellipsoidal cavity through other feeding pipes. 2 and Cl 2 until the gas pressure in the ellipsoidal cavity reaches a fourth preset gas pressure, the microwave generating mechanism is started, and the extracted gas, O 2 , Cl 2 and the quartz sand obtained after the previous purification step are respectively introduced into the ellipsoidal cavity through different feeding pipes, the quartz sand falls into the loading tray and is heated by the microwave generating mechanism, and then falls into the storage tank through the opening, completing the microwave-chlorination purification treatment.

与现有技术相比,本发明具有以下有益效果:本发明石英砂微波提纯方法在微波-水粹-酸洗一体化提纯处理和微波-氯化提纯处理阶段均应用本发明的石英砂微波提纯装置,使得石英砂迅速升温,在微波-水粹-酸洗一体化提纯处理阶段,借助微波等离子体选择加热的作用,石英砂中气液包裹体等杂质的温度和压力急剧上升,随后发生热爆裂,或者与石英砂基体热膨胀系数的差异使其在杂质与基体界面之间产生微裂纹,在极短的时间内使得石英砂状态达到水粹要求,配合储物槽等的设计,准备好的石英砂落入储物槽中存储的酸溶液中,经水淬促使在界面产生的微裂纹延伸通过酸洗对气液包裹体中杂质进行去除,提纯效率高,提纯程度高,处理后的石英砂纯度更高;在微波-氯化提纯处理阶段,也可使得石英砂迅速升温,进而借助反应气体对杂质氯化提纯,且反应气体可使用微波-水粹-酸洗一体化提纯处理完成后椭球形腔体内的气体,重复利用,降低成本,且提纯效率高,提纯程度高,处理后的石英砂纯度更高。Compared with the prior art, the present invention has the following beneficial effects: the microwave purification method for quartz sand of the present invention uses the microwave purification device for quartz sand of the present invention in both the microwave-water purification-acid washing integrated purification treatment and the microwave-chlorination purification treatment stage, so that the temperature of the quartz sand is rapidly increased. In the microwave-water purification-acid washing integrated purification treatment stage, with the help of the selective heating effect of microwave plasma, the temperature and pressure of impurities such as gas-liquid inclusions in the quartz sand rise sharply, and then thermal explosion occurs, or the difference in thermal expansion coefficient with the quartz sand matrix causes microcracks to be generated between the impurities and the matrix interface, so that the quartz sand reaches the water state in a very short time. According to the requirements of purification, in conjunction with the design of the storage tank, the prepared quartz sand falls into the acid solution stored in the storage tank, and the microcracks generated at the interface are extended by water quenching, and the impurities in the gas-liquid inclusions are removed by pickling, with high purification efficiency and high degree of purification, and the quartz sand after treatment has higher purity; in the microwave-chlorination purification stage, the quartz sand can also be rapidly heated, and then the impurities are purified by chlorination with the help of the reaction gas, and the reaction gas can use the gas in the ellipsoidal cavity after the integrated purification treatment of microwave-water purification-pickling is completed, which can be reused to reduce costs, and has high purification efficiency and high degree of purification, and the quartz sand after treatment has higher purity.

本发明引入氯化剂(HCl气体),在微波-水粹-酸洗一体化提纯处理阶段,其可以与石英砂中的杂质结合将其转化为气相或者凝结相从而将杂质从石英砂中脱离,初步去除一定量的金属杂质,为下一步的水粹酸洗做好准备工作,提高去除效率与概率;同时,HCl气体可作为下一阶段微波-氯化提纯处理阶段的工作气体之一,从而可以降低成本;另外,微波焙烧后保温的石英砂样品无需转移出来,避免了热量损失,直接经过水淬酸洗处理,保证了淬冷效果,有利于裂纹的延展,从而提高酸洗的效率。在微波-氯化提纯处理阶段,相较于固体氯源,气体氯源的引入能够将石英砂表面完全包裹,大大提高氯源与石英砂中杂质的接触面积,更有利于与杂质相凝聚从而将杂质相脱离石英砂基体,从而提高氯化焙烧的效率。本发明提纯方法适用于对不同地区以及同一地区品质不均一的石英矿石进行提纯,相比于现有技术,提纯效果好,提纯出的石英砂可获得更好的纯度。The present invention introduces a chlorinating agent (HCl gas), which can be combined with impurities in quartz sand to convert them into gas phase or condensed phase in the microwave-water scavenging-pickling integrated purification treatment stage, thereby separating impurities from quartz sand, preliminarily removing a certain amount of metal impurities, preparing for the next step of water scavenging and pickling, and improving removal efficiency and probability; at the same time, HCl gas can be used as one of the working gases in the next stage of microwave-chlorination purification treatment, thereby reducing costs; in addition, the quartz sand sample that is insulated after microwave roasting does not need to be transferred out, avoiding heat loss, and directly undergoes water quenching and pickling treatment, ensuring the quenching effect, which is conducive to the extension of cracks, thereby improving the efficiency of pickling. In the microwave-chlorination purification treatment stage, compared with a solid chlorine source, the introduction of a gaseous chlorine source can completely wrap the surface of quartz sand, greatly increasing the contact area between the chlorine source and the impurities in the quartz sand, and is more conducive to condensing with the impurity phase to separate the impurity phase from the quartz sand matrix, thereby improving the efficiency of chlorination roasting. The purification method of the present invention is suitable for purifying quartz ores of uneven quality in different regions and the same region. Compared with the prior art, the purification effect is good, and the purified quartz sand can obtain better purity.

在本发明的一些实施方式中,所述预设尺寸为50~425μm;和/或,S3中的酸溶液为盐酸与硝酸的混合水溶液,其中,酸溶液中盐酸与硝酸的重量比为1:(1~1.5),盐酸的浓度为1.5~2.0mol/L,硝酸的浓度为1.5~2.0mol/L,落入储物槽的石英砂与酸溶液的重量比为1:(3~8);和/或,S3-S4通入上一步提纯后得到的石英砂时,通过载料盘下方连接的与载料盘底部的开孔连通的下料通道上的振动机构对载料盘进行振动;和/或,所述第一预设气压和第三预设气压均≤1×10-2Pa,第二预设气压为13333~34666Pa,第四预设气压为6666.5~23000Pa。石英砂筛分至50~425μm的尺寸有利于提高微波-水粹-酸洗一体化提纯处理和微波-氯化提纯处理阶段的提纯效率及提纯效果。酸溶液为盐酸与硝酸的混合水溶液,硝酸的强氧化性使得石英砂表面的金属杂质与其发生反应生成硝酸盐,金属离子的硝酸盐在水中溶解度很高,经过长时间的酸洗可以使得杂质硝酸盐脱离石英砂,另外,盐酸可以提供强酸性环境,同时去除石英砂中的Fe,两种酸的结合不仅可以避免对石英砂的损伤,还可以提高除杂效果。酸溶液和石英砂与酸溶液用量的设计则可充分的保证对石英砂的酸洗效果及效率,酸溶液过量则造成不必要的额外成本,酸溶液过少则酸洗效果不佳。振动机构提供振动功能,通过振动实现石英砂在载料盘上均匀平铺和顺路下落,以利于控制石英砂经微波等离子体处理/氯化处理的时间和温度。In some embodiments of the present invention, the preset size is 50-425 μm; and/or, the acid solution in S3 is a mixed aqueous solution of hydrochloric acid and nitric acid, wherein the weight ratio of hydrochloric acid to nitric acid in the acid solution is 1:(1-1.5), the concentration of hydrochloric acid is 1.5-2.0 mol/L, the concentration of nitric acid is 1.5-2.0 mol/L, and the weight ratio of quartz sand falling into the storage tank to the acid solution is 1:(3-8); and/or, when S3-S4 is introduced into the quartz sand obtained after the previous step of purification, the loading tray is vibrated by a vibration mechanism on a feeding channel connected to the bottom of the loading tray and connected to the opening at the bottom of the loading tray; and/or, the first preset air pressure and the third preset air pressure are both ≤1×10 -2 Pa, the second preset air pressure is 13333-34666Pa, and the fourth preset air pressure is 6666.5-23000Pa. Quartz sand screening to a size of 50-425 μm is conducive to improving the purification efficiency and purification effect of the microwave-water purification-pickling integrated purification treatment and microwave-chlorination purification treatment stages. The acid solution is a mixed aqueous solution of hydrochloric acid and nitric acid. The strong oxidizing property of nitric acid causes the metal impurities on the surface of the quartz sand to react with it to form nitrates. The nitrates of metal ions have a high solubility in water. After a long period of pickling, the impurity nitrates can be separated from the quartz sand. In addition, hydrochloric acid can provide a strong acidic environment and remove Fe in the quartz sand at the same time. The combination of the two acids can not only avoid damage to the quartz sand, but also improve the impurity removal effect. The design of the acid solution and the amount of quartz sand and the acid solution can fully guarantee the pickling effect and efficiency of the quartz sand. Excessive acid solution will cause unnecessary additional costs, and too little acid solution will result in poor pickling effect. The vibration mechanism provides a vibration function, which realizes the uniform paving and falling of the quartz sand on the loading tray through vibration, so as to control the time and temperature of the quartz sand after microwave plasma treatment/chlorination treatment.

在本发明的一些实施方式中,当微波发生机构采用2.45GHz的固态微波源时,S3中通入的HCl气体流量为0.1~1.5L/min,通入上一步提纯后得到的石英砂的速度为0.5~2.5kg/min,石英砂由微波发生机构加热至950~1200℃;S4中通入的O2与通入的S3椭球形腔体内的气体的流量比为(0.1~2.4):100,通入的Cl2与通入的S3椭球形腔体内的气体的流量比为(3~20):100,通入上一步提纯后得到的石英砂的速度为0.5~2.5kg/min,石英砂由微波发生机构加热至800~1000℃。In some embodiments of the present invention, when the microwave generating mechanism adopts a 2.45 GHz solid-state microwave source, the flow rate of HCl gas introduced into S3 is 0.1 to 1.5 L/min, the speed of introducing the quartz sand obtained after the previous step of purification is 0.5 to 2.5 kg/min, and the quartz sand is heated to 950 to 1200°C by the microwave generating mechanism; the flow ratio of O2 introduced into S4 to the gas introduced into the ellipsoidal cavity of S3 is (0.1 to 2.4):100, the flow ratio of Cl2 introduced to the gas introduced into the ellipsoidal cavity of S3 is (3 to 20):100, the speed of introducing the quartz sand obtained after the previous step of purification is 0.5 to 2.5 kg/min, and the quartz sand is heated to 800 to 1000°C by the microwave generating mechanism.

在本发明的一些实施方式中,当微波发生机构采用915MHz的固态微波源时,S3中通入的HCl气体流量为0.35~6.5L/min,通入上一步提纯后得到的石英砂的速度为1.5~10kg/min,石英砂由微波发生机构加热至950~1200℃;S4中通入的O2与通入的S3椭球形腔体内的气体的流量比为(0.1~2.4):100,通入的Cl2与通入的S3椭球形腔体内的气体的流量比为(3~20):100,通入上一步提纯后得到的石英砂的速度为1.5~10kg/min,石英砂由微波发生机构加热至800~1000℃。In some embodiments of the present invention, when the microwave generating mechanism adopts a solid-state microwave source of 915 MHz, the flow rate of HCl gas introduced into S3 is 0.35-6.5 L/min, the speed of introducing the quartz sand obtained after the previous step of purification is 1.5-10 kg/min, and the quartz sand is heated to 950-1200°C by the microwave generating mechanism; the flow ratio of O2 introduced into S4 to the gas introduced into the ellipsoidal cavity of S3 is (0.1-2.4):100, the flow ratio of Cl2 introduced to the gas introduced into the ellipsoidal cavity of S3 is (3-20):100, the speed of introducing the quartz sand obtained after the previous step of purification is 1.5-10 kg/min, and the quartz sand is heated to 800-1000°C by the microwave generating mechanism.

本发明采用2.45GHz的固态微波源或915MHz的固态微波源时,以上述气体流量、石英砂通入速度、加热温度、反应气体流量比等进行微波-水粹-酸洗一体化提纯处理和微波-氯化提纯处理阶段时,微波对石英砂的加热效果更好,石英砂与反应气体、酸溶液等的接触时机更好,更有利于石英砂的提纯。When the present invention adopts a 2.45 GHz solid-state microwave source or a 915 MHz solid-state microwave source, and performs microwave-water purification-acid washing integrated purification treatment and microwave-chlorination purification treatment stages with the above-mentioned gas flow rate, quartz sand introduction speed, heating temperature, reaction gas flow ratio, etc., the microwave has a better heating effect on the quartz sand, the contact timing between the quartz sand and the reaction gas, acid solution, etc. is better, and it is more conducive to the purification of the quartz sand.

另一方面,本发明还提供了一种高纯石英砂,其根据上述任一项所述的石英砂微波提纯方法提纯得到。本发明高纯石英砂纯度高,满足光伏、半导体、通讯、国防军工等高端制造行业的使用要求。On the other hand, the present invention also provides a high-purity quartz sand, which is purified according to any of the above-mentioned quartz sand microwave purification methods. The high-purity quartz sand of the present invention has high purity and meets the use requirements of high-end manufacturing industries such as photovoltaics, semiconductors, communications, and national defense.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

为了更清楚地说明本发明实施例中的技术方案,下面将对本发明实施例中所需要使用的附图进行说明。In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings required for use in the embodiments of the present invention will be described below.

图1为本发明的一种实施例的石英砂微波提纯装置的透视图,其中,置料机构定位件、载料盘连接座、储物槽连接座和弹性件未示出;FIG1 is a perspective view of a quartz sand microwave purification device according to an embodiment of the present invention, wherein a material placement mechanism positioning member, a material loading tray connection seat, a storage tank connection seat and an elastic member are not shown;

图2为本发明的一种实施例的石英砂微波提纯装置的过其长半轴与进料管中心所在平面的剖视图;2 is a cross-sectional view of a quartz sand microwave purification device according to an embodiment of the present invention, taken along a plane where its long semi-axis and the center of a feed pipe are located;

图3为本发明的一种实施例的石英砂微波提纯方法的流程图,其中,示出了微波-水粹-酸洗一体化提纯处理与微波-氯化提纯处理过程中应用本发明一种实施例的石英砂微波提纯装置的示意图;FIG3 is a flow chart of a method for microwave purification of quartz sand according to an embodiment of the present invention, wherein a schematic diagram of a microwave purification device for quartz sand according to an embodiment of the present invention is shown in the microwave-water purification-acid washing integrated purification process and the microwave-chlorination purification process;

图4为通过本发明一种实施例的石英砂微波提纯方法提纯后的石英砂与未提纯的石英砂加热后吹泡对比图,其中,图4(a)为未提纯的石英砂加热后吹泡状态图,4(b)为通过本发明一种实施例的石英砂微波提纯方法提纯后的石英砂加热后吹泡状态图。Figure 4 is a comparison diagram of quartz sand purified by a quartz sand microwave purification method according to an embodiment of the present invention and unpurified quartz sand after heating and bubbling, wherein Figure 4(a) is a diagram of the bubbling state of unpurified quartz sand after heating, and Figure 4(b) is a diagram of the bubbling state of quartz sand purified by a quartz sand microwave purification method according to an embodiment of the present invention after heating.

具体实施方式DETAILED DESCRIPTION

为使本发明的目的、技术方案和优点更加清楚,以下将结合具体实施例对本发明涉及的各个方面进行详细说明,但这些具体实施例仅用于举例说明本发明,并不对本发明的保护范围和实质内容构成任何限定。In order to make the objectives, technical solutions and advantages of the present invention more clear, various aspects of the present invention will be described in detail in conjunction with specific embodiments below, but these specific embodiments are only used to illustrate the present invention and do not constitute any limitation on the scope of protection and essential content of the present invention.

实施例1Example 1

本实施例提供一种石英砂微波提纯装置,如图1-2所示,包括微波发生机构1、置料机构2和壳体3。壳体3的内壁围成椭球形腔体,壳体3包括上壳体31和下壳体32,上壳体31和下壳体32可拆卸连接,上壳体31设有伸入椭球形腔体内的出气管311和若干伸入椭球形腔体内的进料管312,下壳体32对应于椭球形腔体长半轴的位置设有置料机构定位件321。在本实施例中,进料管312的数量不受限制,可按需设置;优选地,出气管311和进料管312上设有阀门开关,用于控制出气管311和进料管312的开关;优选地,进料管312伸入椭球形腔体内的一端朝向椭球形腔体的下焦点。在本实施例中,上壳体31和下壳体32的可拆卸连接方式不受限制,例如,上壳体31和下壳体32的开口端均设有法兰盘33,上壳体31和下壳体32通过法兰盘33上的安装开孔借助螺栓螺母结构连接;优选地,连接处可设置密封件。The present embodiment provides a quartz sand microwave purification device, as shown in Fig. 1-2, comprising a microwave generating mechanism 1, a feeding mechanism 2 and a shell 3. The inner wall of the shell 3 forms an ellipsoidal cavity, and the shell 3 comprises an upper shell 31 and a lower shell 32, which are detachably connected, and the upper shell 31 is provided with an air outlet pipe 311 extending into the ellipsoidal cavity and a plurality of feeding pipes 312 extending into the ellipsoidal cavity, and the lower shell 32 is provided with a feeding mechanism positioning member 321 corresponding to the position of the long semi-axis of the ellipsoidal cavity. In the present embodiment, the number of feeding pipes 312 is not limited and can be set as needed; preferably, valve switches are provided on the air outlet pipe 311 and the feeding pipe 312 to control the opening and closing of the air outlet pipe 311 and the feeding pipe 312; preferably, one end of the feeding pipe 312 extending into the ellipsoidal cavity faces the lower focus of the ellipsoidal cavity. In this embodiment, the detachable connection method of the upper shell 31 and the lower shell 32 is not restricted. For example, the open ends of the upper shell 31 and the lower shell 32 are provided with flanges 33, and the upper shell 31 and the lower shell 32 are connected by means of bolt and nut structures through the mounting openings on the flanges 33; preferably, a seal can be provided at the connection.

在本实施例中,微波发生机构1自上壳体31对应于椭球形腔体长半轴的位置伸入椭球形腔体内,微波发生机构1的微波发生位置11位于椭球形腔体的上焦点。在本实施例中,微波发生机构1的具体结构不受限制,可采用市售产品。在本实施例中,优选地,微波发生机构1采用2.45GHz的固态微波源或915MHz的固态微波源。In this embodiment, the microwave generating mechanism 1 extends into the ellipsoidal cavity from the position of the upper shell 31 corresponding to the long semi-axis of the ellipsoidal cavity, and the microwave generating position 11 of the microwave generating mechanism 1 is located at the upper focus of the ellipsoidal cavity. In this embodiment, the specific structure of the microwave generating mechanism 1 is not limited, and commercially available products can be used. In this embodiment, preferably, the microwave generating mechanism 1 uses a 2.45 GHz solid-state microwave source or a 915 MHz solid-state microwave source.

在本实施例中,置料机构2包括载料盘21和位于载料盘21下方的储物槽22,载料盘21与储物槽22连接,载料盘21底部设有开孔。在本实施例中,优选地,置料机构定位件321为凹槽状,置料机构定位件321的形状与储物槽22外表面相匹配,储物槽22可嵌入置料机构定位件321中。In this embodiment, the material placement mechanism 2 includes a material loading tray 21 and a storage tank 22 located below the material loading tray 21, the material loading tray 21 is connected to the storage tank 22, and an opening is provided at the bottom of the material loading tray 21. In this embodiment, preferably, the material placement mechanism positioning member 321 is in the shape of a groove, the shape of the material placement mechanism positioning member 321 matches the outer surface of the storage tank 22, and the storage tank 22 can be embedded in the material placement mechanism positioning member 321.

在本实施例中,当将置料机构2借助储物槽22置于置料机构定位件321时,置料机构2位于椭球形腔体的长半轴上,载料盘21位于下焦点下方。当微波发生机构1采用2.45GHz的固态微波源时,载料盘21的上表面距离椭球形腔体的下焦点的距离H为30~45mm,5cm≤载料盘上端面的直径≤10cm;当微波发生机构1采用915MHz的固态微波源时,载料盘21的上表面距离椭球形腔体的下焦点的距离H为75~125mm,5cm≤载料盘上端面的直径≤15cm。In this embodiment, when the material placement mechanism 2 is placed on the material placement mechanism positioning member 321 by means of the storage tank 22, the material placement mechanism 2 is located on the long semi-axis of the ellipsoidal cavity, and the material loading plate 21 is located below the lower focus. When the microwave generating mechanism 1 adopts a 2.45GHz solid-state microwave source, the distance H between the upper surface of the material loading plate 21 and the lower focus of the ellipsoidal cavity is 30 to 45mm, and 5cm≤the diameter of the upper end surface of the material loading plate≤10cm; when the microwave generating mechanism 1 adopts a 915MHz solid-state microwave source, the distance H between the upper surface of the material loading plate 21 and the lower focus of the ellipsoidal cavity is 75 to 125mm, and 5cm≤the diameter of the upper end surface of the material loading plate≤15cm.

在本实施例中,载料盘21与储物槽22可拆卸连接,载料盘21外表面间隔设有载料盘连接座211,储物槽22上部间隔设有储物槽连接座,载料盘连接座211和储物槽连接座上均设有安装通孔,载料盘21与储物槽22可通过不同规格的弹性件23借助安装通孔连接。在本实施例中,不同规格的弹性件23可以为长度不同的弹簧,以便于根据实际需求调节载料盘21的上表面距离椭球形腔体的下焦点的距离。In this embodiment, the loading tray 21 and the storage tank 22 are detachably connected, the outer surface of the loading tray 21 is provided with a loading tray connection seat 211, and the upper part of the storage tank 22 is provided with a storage tank connection seat, and the loading tray connection seat 211 and the storage tank connection seat are provided with mounting through holes, and the loading tray 21 and the storage tank 22 can be connected by elastic members 23 of different specifications through the mounting through holes. In this embodiment, the elastic members 23 of different specifications can be springs of different lengths, so as to adjust the distance between the upper surface of the loading tray 21 and the lower focus of the ellipsoidal cavity according to actual needs.

在本实施例中,载料盘21下方还连接有下料通道24,下料通道24与载料盘21底部的开孔连通,下料通道的长度≤20cm。开孔处设有开孔开关25,在本实施例中,开孔开关的具体形式不受限制,只要能堵住开孔和开放开孔即可,优选地,开孔开关与外部控制设备电连接;或者,开孔开关也可以是靠承重打开的开关,例如,开孔开关为瓣膜状开关,瓣膜状开关包括若干围绕开孔内壁周向设置的弹片,弹片一端与开孔内壁连接,弹片远离开孔内壁的一端为自由端。在本实施例中,优选地,下料通道24上设有振动机构26,振动机构的具体形式不受限制,可采用市售产品;优选地,振动机构与外部控制设备电连接,以控制其振动频率。在本实施例中,优选地,载料盘21外表面可设置温度传感器,温度传感器与外部控制设备电连接,便于精确获取开孔开关开启时机。In this embodiment, a material discharge channel 24 is also connected below the loading tray 21, and the material discharge channel 24 is connected to the opening at the bottom of the loading tray 21, and the length of the material discharge channel is ≤20cm. An opening switch 25 is provided at the opening. In this embodiment, the specific form of the opening switch is not limited, as long as it can block the opening and open the opening. Preferably, the opening switch is electrically connected to an external control device; or, the opening switch can also be a switch that is opened by bearing weight, for example, the opening switch is a valve-shaped switch, and the valve-shaped switch includes a number of springs arranged circumferentially around the inner wall of the opening, one end of the spring is connected to the inner wall of the opening, and the end of the spring away from the inner wall of the opening is a free end. In this embodiment, preferably, a vibration mechanism 26 is provided on the material discharge channel 24, and the specific form of the vibration mechanism is not limited, and a commercially available product can be used; preferably, the vibration mechanism is electrically connected to an external control device to control its vibration frequency. In this embodiment, preferably, a temperature sensor can be provided on the outer surface of the loading tray 21, and the temperature sensor is electrically connected to an external control device, so as to accurately obtain the opening time of the opening switch.

本实施例还提供一种石英砂微波提纯方法,如图3所示,包括以下步骤:This embodiment also provides a quartz sand microwave purification method, as shown in FIG3, comprising the following steps:

S1、破碎-筛分处理:对石英矿石进行破碎、筛分,得到预设尺寸的石英原砂。在本实施例中,石英矿石可经颚式、圆锥、对辊三道工序进行破碎;将破碎后的石英砂进行筛分至合适颗粒尺寸,一般控制在50~425μm的预设尺寸,所配套筛网规格对应目数∈[300,40]目,优选地,预设尺寸∈[75,250]μm,筛网规格∈[200,60]目。S1. Crushing-screening treatment: crushing and screening the quartz ore to obtain quartz raw sand of preset size. In this embodiment, the quartz ore can be crushed by three processes: jaw, cone, and roller; the crushed quartz sand is screened to a suitable particle size, generally controlled within a preset size of 50 to 425 μm, and the matching screen specification corresponds to a mesh number ∈ [300, 40] mesh, preferably, the preset size ∈ [75, 250] μm, and the screen specification ∈ [200, 60] mesh.

S2、初始提纯处理:通过包括磁选、浮选、酸洗的提纯方式对所述石英原砂进行初始提纯。在本实施例中,将筛分后得到的预设尺寸的石英原砂利用强磁选矿机进行磁选,清除弱磁性杂质矿物后,再进行浮选去除非磁性伴生杂质矿物,最后再利用石英化学性质较为稳定的特点,通过盐酸和硝酸的混合酸进行酸洗,以进一步对石英砂表面化学处理提纯。S2. Initial purification treatment: The quartz raw sand is initially purified by purification methods including magnetic separation, flotation, and pickling. In this embodiment, the quartz raw sand of a preset size obtained after screening is subjected to magnetic separation using a strong magnetic separator to remove weakly magnetic impurity minerals, and then flotation is performed to remove non-magnetic associated impurity minerals. Finally, the quartz sand is pickled by a mixed acid of hydrochloric acid and nitric acid using the relatively stable chemical properties of quartz to further chemically treat and purify the surface of the quartz sand.

S3、微波-水粹-酸洗一体化提纯处理:应用本实施例的石英砂微波提纯装置,将酸溶液置于储物槽中,将置料机构置于下壳体的置料机构定位件上,封闭上壳体和下壳体以使椭球形腔体处于密封状态,通过出气管抽真空至椭球形腔体内的气压达到第一预设气压后,通过进料管向椭球形腔体内通入HCl气体直至椭球形腔体内的气压达到第二预设气压,启动微波发生机构,分别通过不同进料管向椭球形腔体内通入HCl气体和上一步提纯后得到的石英砂,石英砂落入载料盘并由微波发生机构加热后通过开孔落入储物槽的酸溶液中进行水粹酸洗。S3. Integrated purification treatment by microwave-water purification-pickling: Using the microwave purification device for quartz sand of the present embodiment, an acid solution is placed in a storage tank, a feeding mechanism is placed on a feeding mechanism positioning member of the lower shell, the upper shell and the lower shell are closed to seal the ellipsoidal cavity, and after vacuuming the ellipsoidal cavity through an air outlet pipe until the air pressure in the ellipsoidal cavity reaches a first preset air pressure, HCl gas is introduced into the ellipsoidal cavity through a feeding pipe until the air pressure in the ellipsoidal cavity reaches a second preset air pressure, the microwave generating mechanism is started, and HCl gas and the quartz sand obtained after the previous purification step are introduced into the ellipsoidal cavity through different feeding pipes respectively, the quartz sand falls into a loading tray and is heated by the microwave generating mechanism, and then falls into the acid solution in the storage tank through an opening for water purification and pickling.

在本实施例中,S3中的酸溶液为盐酸与硝酸的混合水溶液,其中,酸溶液中盐酸与硝酸的重量比为1:(1~1.5),盐酸的浓度为1.5~2.0mol/L,硝酸的浓度为1.5~2.0mol/L,落入储物槽的石英砂与酸溶液的重量比为1:(3~8);和/或,S3通入上一步提纯后得到的石英砂时,通过载料盘下方连接的与载料盘底部的开孔连通的下料通道上的振动机构对载料盘进行振动;和/或,第一预设气压≤1×10-2Pa,第二预设气压为13333~34666Pa;和/或,载料盘为石英载料盘,材质为高纯石英玻璃或者陶瓷,纯度≥99.995%。In this embodiment, the acid solution in S3 is a mixed aqueous solution of hydrochloric acid and nitric acid, wherein the weight ratio of hydrochloric acid to nitric acid in the acid solution is 1:(1-1.5), the concentration of hydrochloric acid is 1.5-2.0 mol/L, the concentration of nitric acid is 1.5-2.0 mol/L, and the weight ratio of the quartz sand falling into the storage tank to the acid solution is 1:(3-8); and/or, when S3 is passed through the quartz sand obtained after the previous step of purification, the loading tray is vibrated by a vibration mechanism on a feeding channel connected to the bottom of the loading tray and connected to the opening at the bottom of the loading tray; and/or, the first preset air pressure is ≤1×10 -2 Pa, and the second preset air pressure is 13333-34666 Pa; and/or, the loading tray is a quartz loading tray, and the material is high-purity quartz glass or ceramic with a purity of ≥99.995%.

在本实施例中,当微波发生机构采用2.45GHz的固态微波源时,S3中通入的HCl气体流量为0.1~1.5L/min,通入上一步提纯后得到的石英砂的速度为0.5~2.5kg/min,石英砂由微波发生机构加热至950~1200℃。当微波发生机构采用915MHz的固态微波源时,S3中通入的HCl气体流量为0.35~6.5L/min,通入上一步提纯后得到的石英砂的速度为1.5~10kg/min,石英砂由微波发生机构加热至950~1200℃。具体地,根据不同微波源规格,工艺参数关系如下表1所示。In this embodiment, when the microwave generating mechanism adopts a 2.45 GHz solid-state microwave source, the flow rate of HCl gas introduced into S3 is 0.1 to 1.5 L/min, the speed of introducing the quartz sand obtained after the previous step of purification is 0.5 to 2.5 kg/min, and the quartz sand is heated to 950 to 1200° C. by the microwave generating mechanism. When the microwave generating mechanism adopts a 915 MHz solid-state microwave source, the flow rate of HCl gas introduced into S3 is 0.35 to 6.5 L/min, the speed of introducing the quartz sand obtained after the previous step of purification is 1.5 to 10 kg/min, and the quartz sand is heated to 950 to 1200° C. by the microwave generating mechanism. Specifically, according to different microwave source specifications, the relationship between process parameters is shown in Table 1 below.

表1不同微波源规格下S3步骤工艺参数Table 1 Process parameters of step S3 under different microwave source specifications

S4、微波-氯化提纯处理:应用另一本实施例的石英砂微波提纯装置,将置料机构置于下壳体的置料机构定位件上,封闭上壳体和下壳体以使椭球形腔体处于密封状态,通过出气管抽真空至椭球形腔体内的气压达到第三预设气压后,自S3应用的石英砂微波提纯装置的出气管抽出其椭球形腔体内的气体,将抽出的气体通过S4应用的石英砂微波提纯装置的任一进料管通入椭球形腔体内,同时通过其他进料管向椭球形腔体内通入O2和Cl2,直至椭球形腔体内的气压达到第四预设气压,启动微波发生机构,分别通过不同进料管向椭球形腔体内通入抽出的气体、O2、Cl2和上一步提纯后得到的石英砂,石英砂落入载料盘并由微波发生机构加热后通过开孔落入储物槽中,完成微波-氯化提纯处理。S4, microwave-chlorination purification treatment: another quartz sand microwave purification device of the present embodiment is used, the feeding mechanism is placed on the feeding mechanism positioning piece of the lower shell, the upper shell and the lower shell are closed to make the ellipsoidal cavity in a sealed state, and after the air pressure in the ellipsoidal cavity reaches the third preset air pressure through the air outlet pipe, the gas in the ellipsoidal cavity is extracted from the air outlet pipe of the quartz sand microwave purification device used in S3, and the extracted gas is introduced into the ellipsoidal cavity through any feed pipe of the quartz sand microwave purification device used in S4, and O2 and Cl2 are introduced into the ellipsoidal cavity through other feed pipes until the air pressure in the ellipsoidal cavity reaches the fourth preset air pressure, the microwave generating mechanism is started, and the extracted gas, O2 , Cl2 and the quartz sand obtained after the previous purification are respectively introduced into the ellipsoidal cavity through different feed pipes, the quartz sand falls into the loading tray and is heated by the microwave generating mechanism and then falls into the storage tank through the opening, completing the microwave-chlorination purification treatment.

在本实施例中,可将S3椭球形腔体内的气体抽出并存储在气体存储设备中,当S3椭球形腔体内为常压左右时,打开壳体取出酸溶液中的石英砂烘干后备用做S4的提纯对象,将自S3椭球形腔体内抽出的气体从气体存储设备抽出并通入S4应用的石英砂微波提纯装置。In this embodiment, the gas in the S3 ellipsoidal cavity can be extracted and stored in a gas storage device. When the pressure in the S3 ellipsoidal cavity is around normal pressure, the shell is opened to take out the quartz sand in the acid solution, dry it and use it as the purification object of S4. The gas extracted from the S3 ellipsoidal cavity is extracted from the gas storage device and passed into the quartz sand microwave purification device used in S4.

在本实施例中,S4通入上一步提纯后得到的石英砂时,通过载料盘下方连接的与载料盘底部的开孔连通的下料通道上的振动机构对载料盘进行振动;和/或,第三预设气压≤1×10-2Pa,第四预设气压为6666.5~23000Pa。In this embodiment, when S4 is introduced into the quartz sand obtained after the previous step of purification, the loading tray is vibrated by a vibration mechanism on a feeding channel connected to the bottom of the loading tray and connected to an opening at the bottom of the loading tray; and/or, the third preset air pressure is ≤1×10 -2 Pa, and the fourth preset air pressure is 6666.5~23000Pa.

在本实施例中,当微波发生机构采用2.45GHz的固态微波源时,S4中通入的O2与通入的S3椭球形腔体内的气体的流量比为(0.1~2.4):100,通入的Cl2与通入的S3椭球形腔体内的气体的流量比为(3~20):100,通入上一步提纯后得到的石英砂的速度为0.5~2.5kg/min,石英砂由微波发生机构加热至800~1000℃。当微波发生机构采用915MHz的固态微波源时,S4中通入的O2与通入的S3椭球形腔体内的气体的流量比为(0.1~2.4):100,通入的Cl2与通入的S3椭球形腔体内的气体的流量比为(3~20):100,通入上一步提纯后得到的石英砂的速度为1.5~10kg/min,石英砂由微波发生机构加热至800~1000℃。具体地,根据不同微波源规格,工艺参数关系如下表2所示。In this embodiment, when the microwave generating mechanism adopts a 2.45 GHz solid-state microwave source, the flow ratio of O2 introduced into S4 and the gas introduced into the S3 ellipsoidal cavity is (0.1-2.4):100, the flow ratio of Cl2 introduced into the S3 ellipsoidal cavity is (3-20):100, the speed of introducing the quartz sand obtained after the previous step of purification is 0.5-2.5 kg/min, and the quartz sand is heated to 800-1000°C by the microwave generating mechanism. When the microwave generating mechanism adopts a 915MHz solid-state microwave source, the flow ratio of O2 introduced into S4 to the gas introduced into the S3 ellipsoidal cavity is (0.1-2.4):100, the flow ratio of Cl2 introduced to the gas introduced into the S3 ellipsoidal cavity is (3-20):100, the speed of introducing the quartz sand obtained after the previous step of purification is 1.5-10kg/min, and the quartz sand is heated to 800-1000°C by the microwave generating mechanism. Specifically, according to different microwave source specifications, the relationship between process parameters is shown in Table 2 below.

表2不同微波源规格下S4步骤工艺参数Table 2 Process parameters of step S4 under different microwave source specifications

在本实施例中,优选地,可根据实际情况进行S2-S4步骤的再次或多次循环,直至石英砂纯度合格。In this embodiment, preferably, steps S2-S4 can be cycled again or multiple times according to actual conditions until the purity of the quartz sand is qualified.

本实施例还提供一种高纯石英砂,其根据本实施例的石英砂微波提纯方法提纯得到。This embodiment also provides a high-purity quartz sand, which is purified according to the quartz sand microwave purification method of this embodiment.

实施例2Example 2

本实施例提供一种石英砂微波提纯装置、应用该石英砂微波提纯装置的石英砂微波提纯方法及应用该石英砂微波提纯方法提纯得到的高纯石英砂。本实施例仅在石英砂微波提纯方法的一些工艺参数上与实施例1存在不同,相同之处不再赘述,仅对不同之处进行说明。This embodiment provides a quartz sand microwave purification device, a quartz sand microwave purification method using the quartz sand microwave purification device, and high-purity quartz sand purified by using the quartz sand microwave purification method. This embodiment differs from Example 1 only in some process parameters of the quartz sand microwave purification method, and the similarities are not repeated here, and only the differences are described.

在本实施例的石英砂微波提纯方法中:In the quartz sand microwave purification method of the present embodiment:

S1、破碎-筛分处理:对石英矿石进行破碎、筛分,得到预设尺寸为75μm的石英原砂。S1. Crushing-screening process: crushing and screening the quartz ore to obtain quartz raw sand with a preset size of 75 μm.

S3中的酸溶液中盐酸与硝酸的重量比为1:1,盐酸的浓度为1.5mol/L,硝酸的浓度为1.5mol/L,落入储物槽的石英砂与酸溶液的重量比为1:3;第一预设气压≤1×10-2Pa,第二预设气压为13333Pa。微波发生机构采用2.45GHz的固态微波源,S3中通入的HCl气体流量为0.1L/min,通入上一步提纯后得到的石英砂的速度为0.5kg/min,石英砂由微波发生机构加热至950℃。具体地,工艺参数关系如下表3所示。The weight ratio of hydrochloric acid to nitric acid in the acid solution in S3 is 1:1, the concentration of hydrochloric acid is 1.5 mol/L, the concentration of nitric acid is 1.5 mol/L, and the weight ratio of quartz sand falling into the storage tank to the acid solution is 1:3; the first preset air pressure is ≤1×10 -2 Pa, and the second preset air pressure is 13333 Pa. The microwave generating mechanism adopts a 2.45 GHz solid-state microwave source, the flow rate of HCl gas introduced into S3 is 0.1 L/min, the speed of introducing the quartz sand obtained after the previous step of purification is 0.5 kg/min, and the quartz sand is heated to 950°C by the microwave generating mechanism. Specifically, the relationship between the process parameters is shown in Table 3 below.

表3 S3步骤工艺参数Table 3 Process parameters of step S3

微波源规格Microwave source specifications 2.45GHz2.45GHz 微波输出功率Microwave output power 4kw4kw HCl气体流量HCl gas flow rate 0.1L/min0.1L/min 石英加料量Quartz feeding amount 0.5kg/min0.5kg/min 控制石英砂微波加热温度Controlling the temperature of quartz sand microwave heating 950℃950℃ 石英载料盘椭球体与下焦点距离Distance between the quartz carrier plate ellipsoid and the lower focus 30mm30mm 石英载料盘振频Quartz carrier plate vibration frequency 1Hz1Hz

S4中第三预设气压≤1×10-2Pa,第四预设气压为6666.5Pa。微波发生机构采用2.45GHz的固态微波源,S4中通入的O2与通入的S3椭球形腔体内的气体的流量比为0.1:100,通入的Cl2与通入的S3椭球形腔体内的气体的流量比为3:100,通入上一步提纯后得到的石英砂的速度为0.5kg/min,石英砂由微波发生机构加热至800℃。具体地,工艺参数关系如下表4所示。The third preset gas pressure in S4 is ≤1×10 -2 Pa, and the fourth preset gas pressure is 6666.5 Pa. The microwave generating mechanism adopts a 2.45GHz solid-state microwave source, the flow ratio of O 2 introduced into S4 to the gas introduced into the S3 ellipsoidal cavity is 0.1:100, the flow ratio of Cl 2 introduced to the gas introduced into the S3 ellipsoidal cavity is 3:100, the speed of introducing the quartz sand obtained after the previous step of purification is 0.5kg/min, and the quartz sand is heated to 800°C by the microwave generating mechanism. Specifically, the relationship between the process parameters is shown in Table 4 below.

表4S4步骤工艺参数Table 4 S4 step process parameters

在本实施例中,S2-S4步骤的循环次数为2次。In this embodiment, the number of cycles of steps S2-S4 is 2 times.

实施例3Example 3

本实施例提供一种石英砂微波提纯装置、应用该石英砂微波提纯装置的石英砂微波提纯方法及应用该石英砂微波提纯方法提纯得到的高纯石英砂。本实施例仅在石英砂微波提纯方法的一些工艺参数上与实施例2存在不同,相同之处不再赘述,仅对不同之处进行说明。This embodiment provides a quartz sand microwave purification device, a quartz sand microwave purification method using the quartz sand microwave purification device, and high-purity quartz sand purified by using the quartz sand microwave purification method. This embodiment differs from Example 2 only in some process parameters of the quartz sand microwave purification method, and the similarities are not repeated here, and only the differences are described.

在本实施例的石英砂微波提纯方法中:In the quartz sand microwave purification method of the present embodiment:

S3中微波发生机构采用915MHz的固态微波源,S3中通入的HCl气体流量为0.35L/min,通入上一步提纯后得到的石英砂的速度为1.5kg/min。具体地,工艺参数关系如下表5所示。The microwave generating mechanism in S3 uses a solid-state microwave source of 915 MHz, the flow rate of HCl gas introduced into S3 is 0.35 L/min, and the speed of introducing the quartz sand obtained after the previous step of purification is 1.5 kg/min. Specifically, the relationship between the process parameters is shown in Table 5 below.

表5S3步骤工艺参数Table 5 S3 step process parameters

S4中微波发生机构采用915MHz的固态微波源,S4中通入上一步提纯后得到的石英砂的速度为1.5kg/min。具体地,工艺参数关系如下表6所示。The microwave generating mechanism in S4 uses a solid-state microwave source of 915 MHz, and the speed of introducing the quartz sand obtained after the previous step of purification into S4 is 1.5 kg/min. Specifically, the relationship between the process parameters is shown in Table 6 below.

表6 S4步骤工艺参数Table 6 Process parameters of step S4

微波源规格Microwave source specifications 915MHz915MHz 微波输出功率Microwave output power 12kw12kw 石英加料量Quartz feeding amount 1.5kg/min1.5kg/min 石英载料盘椭球体与下焦点距离Distance between the quartz carrier plate ellipsoid and the lower focus 75mm75mm 石英载料盘振频Quartz carrier plate vibration frequency 0.1Hz0.1Hz

实施例4Example 4

本实施例提供一种石英砂微波提纯装置、应用该石英砂微波提纯装置的石英砂微波提纯方法及应用该石英砂微波提纯方法提纯得到的高纯石英砂。本实施例仅在石英砂微波提纯方法的一些工艺参数上与实施例1存在不同,相同之处不再赘述,仅对不同之处进行说明。This embodiment provides a quartz sand microwave purification device, a quartz sand microwave purification method using the quartz sand microwave purification device, and high-purity quartz sand purified by using the quartz sand microwave purification method. This embodiment differs from Example 1 only in some process parameters of the quartz sand microwave purification method, and the similarities are not repeated here, and only the differences are described.

在本实施例的石英砂微波提纯方法中:In the quartz sand microwave purification method of the present embodiment:

S1、破碎-筛分处理:对石英矿石进行破碎、筛分,得到预设尺寸为150μm的石英原砂。S1. Crushing-screening process: crushing and screening the quartz ore to obtain quartz raw sand with a preset size of 150 μm.

S3中的酸溶液中盐酸与硝酸的重量比为1:1.25,盐酸的浓度为1.7mol/L,硝酸的浓度为1.7mol/L,落入储物槽的石英砂与酸溶液的重量比为1:5;第一预设气压≤1×10- 2Pa,第二预设气压为20000Pa。微波发生机构采用2.45GHz的固态微波源,S3中通入的HCl气体流量为1.0L/min,通入上一步提纯后得到的石英砂的速度为1.5kg/min,石英砂由微波发生机构加热至1000℃。具体地,工艺参数关系如下表7所示。The weight ratio of hydrochloric acid to nitric acid in the acid solution in S3 is 1:1.25, the concentration of hydrochloric acid is 1.7 mol/L, the concentration of nitric acid is 1.7 mol/L, and the weight ratio of quartz sand falling into the storage tank to the acid solution is 1:5; the first preset air pressure is ≤1×10 - 2 Pa, and the second preset air pressure is 20000 Pa. The microwave generating mechanism adopts a 2.45GHz solid-state microwave source, the flow rate of HCl gas introduced into S3 is 1.0L/min, the speed of introducing the quartz sand obtained after the previous step of purification is 1.5kg/min, and the quartz sand is heated to 1000°C by the microwave generating mechanism. Specifically, the relationship between the process parameters is shown in Table 7 below.

表7 S3步骤工艺参数Table 7 Process parameters of step S3

S4中第三预设气压≤1×10-2Pa,第四预设气压为10000Pa。微波发生机构采用2.45GHz的固态微波源,S4中通入的O2与通入的S3椭球形腔体内的气体的流量比为1:100,通入的Cl2与通入的S3椭球形腔体内的气体的流量比为10:100,通入上一步提纯后得到的石英砂的速度为1.5kg/min,石英砂由微波发生机构加热至900℃。具体地,工艺参数关系如下表8所示。The third preset gas pressure in S4 is ≤1×10 -2 Pa, and the fourth preset gas pressure is 10000 Pa. The microwave generating mechanism adopts a 2.45GHz solid-state microwave source, the flow ratio of O 2 introduced into S4 to the gas introduced into the S3 ellipsoidal cavity is 1:100, the flow ratio of Cl 2 introduced to the gas introduced into the S3 ellipsoidal cavity is 10:100, the speed of introducing the quartz sand obtained after the previous step of purification is 1.5kg/min, and the quartz sand is heated to 900°C by the microwave generating mechanism. Specifically, the relationship between the process parameters is shown in Table 8 below.

表8S4步骤工艺参数Table 8 S4 step process parameters

在本实施例中,S2-S4步骤的循环次数为3次。In this embodiment, the number of cycles of steps S2-S4 is 3 times.

实施例5Example 5

本实施例提供一种石英砂微波提纯装置、应用该石英砂微波提纯装置的石英砂微波提纯方法及应用该石英砂微波提纯方法提纯得到的高纯石英砂。本实施例仅在石英砂微波提纯方法的一些工艺参数上与实施例4存在不同,相同之处不再赘述,仅对不同之处进行说明。This embodiment provides a quartz sand microwave purification device, a quartz sand microwave purification method using the quartz sand microwave purification device, and high-purity quartz sand purified by using the quartz sand microwave purification method. This embodiment differs from Example 4 only in some process parameters of the quartz sand microwave purification method, and the similarities are not repeated here, and only the differences are described.

在本实施例的石英砂微波提纯方法中:In the quartz sand microwave purification method of the present embodiment:

S3中微波发生机构采用915MHz的固态微波源,S3中通入的HCl气体流量为3.5L/min,通入上一步提纯后得到的石英砂的速度为5kg/min。具体地,工艺参数关系如下表9所示。The microwave generating mechanism in S3 uses a solid-state microwave source of 915 MHz, the flow rate of HCl gas introduced into S3 is 3.5 L/min, and the speed of introducing the quartz sand obtained after the previous step of purification is 5 kg/min. Specifically, the relationship between the process parameters is shown in Table 9 below.

表9S3步骤工艺参数Table 9S3 step process parameters

S4中微波发生机构采用915MHz的固态微波源,S4中通入上一步提纯后得到的石英砂的速度为5kg/min。具体地,工艺参数关系如下表10所示。The microwave generating mechanism in S4 uses a solid-state microwave source of 915 MHz, and the speed of introducing the quartz sand obtained after the previous step of purification into S4 is 5 kg/min. Specifically, the relationship between the process parameters is shown in Table 10 below.

表10 S4步骤工艺参数Table 10 Process parameters of step S4

微波源规格Microwave source specifications 915MHz915MHz 微波输出功率Microwave output power 35kw35kw 石英加料量Quartz feeding amount 5kg/min5kg/min 石英载料盘椭球体与下焦点距离Distance between the quartz carrier plate ellipsoid and the lower focus 90mm90mm 石英载料盘振频Quartz carrier plate vibration frequency 8Hz8Hz

实施例6Example 6

本实施例提供一种石英砂微波提纯装置、应用该石英砂微波提纯装置的石英砂微波提纯方法及应用该石英砂微波提纯方法提纯得到的高纯石英砂。本实施例仅在石英砂微波提纯方法的一些工艺参数上与实施例1存在不同,相同之处不再赘述,仅对不同之处进行说明。This embodiment provides a quartz sand microwave purification device, a quartz sand microwave purification method using the quartz sand microwave purification device, and high-purity quartz sand purified by using the quartz sand microwave purification method. This embodiment differs from Example 1 only in some process parameters of the quartz sand microwave purification method, and the similarities are not repeated here, and only the differences are described.

在本实施例的石英砂微波提纯方法中:In the quartz sand microwave purification method of the present embodiment:

S1、破碎-筛分处理:对石英矿石进行破碎、筛分,得到预设尺寸为250μm的石英原砂。S1. Crushing-screening process: crushing and screening the quartz ore to obtain quartz raw sand with a preset size of 250 μm.

S3中的酸溶液中盐酸与硝酸的重量比为1:1.5,盐酸的浓度为2.0mol/L,硝酸的浓度为2.0mol/L,落入储物槽的石英砂与酸溶液的重量比为1:8;第一预设气压≤1×10-2Pa,第二预设气压为34666Pa。微波发生机构采用2.45GHz的固态微波源,S3中通入的HCl气体流量为1.5L/min,通入上一步提纯后得到的石英砂的速度为2.5kg/min,石英砂由微波发生机构加热至1200℃。具体地,工艺参数关系如下表11所示。The weight ratio of hydrochloric acid to nitric acid in the acid solution in S3 is 1:1.5, the concentration of hydrochloric acid is 2.0 mol/L, the concentration of nitric acid is 2.0 mol/L, and the weight ratio of quartz sand falling into the storage tank to the acid solution is 1:8; the first preset air pressure is ≤1×10 -2 Pa, and the second preset air pressure is 34666 Pa. The microwave generating mechanism adopts a 2.45 GHz solid-state microwave source, the flow rate of HCl gas introduced into S3 is 1.5 L/min, the speed of introducing the quartz sand obtained after the previous step of purification is 2.5 kg/min, and the quartz sand is heated to 1200°C by the microwave generating mechanism. Specifically, the relationship between the process parameters is shown in Table 11 below.

表11 S3步骤工艺参数Table 11 Process parameters of step S3

S4中第三预设气压≤1×10-2Pa,第四预设气压为23000Pa。微波发生机构采用2.45GHz的固态微波源,S4中通入的O2与通入的S3椭球形腔体内的气体的流量比为2.4:100,通入的Cl2与通入的S3椭球形腔体内的气体的流量比为20:100,通入上一步提纯后得到的石英砂的速度为2.5kg/min,石英砂由微波发生机构加热至1000℃。具体地,工艺参数关系如下表12所示。The third preset gas pressure in S4 is ≤1×10 -2 Pa, and the fourth preset gas pressure is 23000 Pa. The microwave generating mechanism adopts a 2.45GHz solid-state microwave source, the flow ratio of O 2 introduced into S4 to the gas introduced into the S3 ellipsoidal cavity is 2.4:100, the flow ratio of Cl 2 introduced to the gas introduced into the S3 ellipsoidal cavity is 20:100, the speed of introducing the quartz sand obtained after the previous step of purification is 2.5kg/min, and the quartz sand is heated to 1000°C by the microwave generating mechanism. Specifically, the relationship between the process parameters is shown in Table 12 below.

表12S4步骤工艺参数Table 12S4 step process parameters

在本实施例中,S2-S4步骤的循环次数为3次。In this embodiment, the number of cycles of steps S2-S4 is 3 times.

本实施例对本实施例的石英砂微波提纯方法提纯得到的高纯石英砂进行杂质检测,检测结果如下表13所示。In this embodiment, impurity detection is performed on the high-purity quartz sand obtained by the quartz sand microwave purification method of this embodiment. The detection results are shown in Table 13 below.

表13原始石英矿石与本实施例提纯得到的高纯石英砂的杂质含量对比表Table 13 Comparison of impurity content of original quartz ore and high-purity quartz sand purified in this example

由表13可知,相较于未提纯处理的原始石英矿石,本实施例提纯后得到的高纯石英砂,杂质含量极低,提纯后部分原有杂质未检测出,进一步说明了应用本实施例的提纯装置进行提纯,提纯效果好。图4示出了本实施例的石英砂微波提纯方法提纯后的石英砂与未提纯的石英砂加热后吹泡对比图,由图4可知,原始石英矿石(未提纯的石英砂)含有大量杂质,本实施例的石英砂微波提纯方法提纯后的石英砂杂质含量极少,应用本实施例的提纯装置进行提纯,提纯效果好。As shown in Table 13, compared with the original quartz ore that has not been purified, the high-purity quartz sand obtained after purification in this embodiment has extremely low impurity content, and some of the original impurities are not detected after purification, which further illustrates that the purification effect is good when the purification device of this embodiment is used for purification. FIG4 shows a comparison diagram of quartz sand purified by the quartz sand microwave purification method of this embodiment and bubbling after heating the unpurified quartz sand. As shown in FIG4, the original quartz ore (unpurified quartz sand) contains a large amount of impurities, and the quartz sand purified by the quartz sand microwave purification method of this embodiment has extremely low impurity content. The purification effect is good when the purification device of this embodiment is used for purification.

实施例7Example 7

本实施例提供一种石英砂微波提纯装置、应用该石英砂微波提纯装置的石英砂微波提纯方法及应用该石英砂微波提纯方法提纯得到的高纯石英砂。本实施例仅在石英砂微波提纯方法的一些工艺参数上与实施例6存在不同,相同之处不再赘述,仅对不同之处进行说明。This embodiment provides a quartz sand microwave purification device, a quartz sand microwave purification method using the quartz sand microwave purification device, and high-purity quartz sand purified by using the quartz sand microwave purification method. This embodiment differs from Example 6 only in some process parameters of the quartz sand microwave purification method, and the similarities are not repeated here, and only the differences are described.

在本实施例的石英砂微波提纯方法中:In the quartz sand microwave purification method of the present embodiment:

S3中微波发生机构采用915MHz的固态微波源,S3中通入的HCl气体流量为6.5L/min,通入上一步提纯后得到的石英砂的速度为10kg/min。具体地,工艺参数关系如下表14所示。The microwave generating mechanism in S3 uses a solid-state microwave source of 915 MHz, the flow rate of HCl gas introduced into S3 is 6.5 L/min, and the speed of introducing the quartz sand obtained after the previous step of purification is 10 kg/min. Specifically, the relationship between the process parameters is shown in Table 14 below.

表14 S3步骤工艺参数Table 14 Process parameters of step S3

S4中微波发生机构采用915MHz的固态微波源,S4中通入上一步提纯后得到的石英砂的速度为10kg/min。具体地,工艺参数关系如下表15所示。The microwave generating mechanism in S4 uses a solid-state microwave source of 915 MHz, and the speed of introducing the quartz sand obtained after the previous step of purification into S4 is 10 kg/min. Specifically, the relationship between the process parameters is shown in Table 15 below.

表15 S4步骤工艺参数Table 15 Process parameters of step S4

微波源规格Microwave source specifications 915MHz915MHz 微波输出功率Microwave output power 70kw70kw 石英加料量Quartz feeding amount 10kg/min10kg/min 石英载料盘椭球体与下焦点距离Distance between the quartz carrier plate ellipsoid and the lower focus 125mm125mm 石英载料盘振频Quartz carrier plate vibration frequency 15Hz15Hz

以上结合具体实施方式对本发明进行了说明,这些具体实施方式仅仅是示例性的,不能以此限定本发明的保护范围,本领域技术人员在不脱离本发明实质的前提下可以进行各种修改、变化或替换。因此,根据本发明所作的各种等同变化,仍属于本发明所涵盖的范围。The present invention has been described above in conjunction with specific embodiments. These specific embodiments are merely exemplary and cannot be used to limit the scope of protection of the present invention. Those skilled in the art may make various modifications, changes or substitutions without departing from the essence of the present invention. Therefore, various equivalent changes made according to the present invention still fall within the scope covered by the present invention.

Claims (10)

1. A quartz sand microwave purifying device is characterized by comprising a microwave generating mechanism, a material placing mechanism and a shell,
the inner wall of the shell encloses an ellipsoidal cavity, the shell comprises an upper shell and a lower shell, the upper shell and the lower shell are detachably connected, the upper shell is provided with an air outlet pipe extending into the ellipsoidal cavity and a plurality of feeding pipes extending into the ellipsoidal cavity, and a positioning part of a material placing mechanism is arranged at the position of the lower shell corresponding to a long half shaft of the ellipsoidal cavity;
the microwave generating mechanism stretches into the ellipsoidal cavity from the position of the upper shell corresponding to the long half shaft of the ellipsoidal cavity, and the microwave generating position of the microwave generating mechanism is positioned at the upper focus of the ellipsoidal cavity;
the material placing mechanism comprises a material carrying disc and a storage groove positioned below the material carrying disc, the material carrying disc is connected with the storage groove, and an opening is formed in the bottom of the material carrying disc.
2. The quartz sand microwave purifying device according to claim 1, wherein the opening ends of the upper shell and the lower shell are respectively provided with a flange, and the upper shell and the lower shell are connected by a bolt and nut structure through mounting holes on the flanges; and/or one end of the feeding pipe extending into the ellipsoidal cavity faces to the lower focus of the ellipsoidal cavity; and/or the positioning piece of the material placing mechanism is in a groove shape, the shape of the positioning piece of the material placing mechanism is matched with the outer surface of the storage groove, and the storage groove can be embedded into the positioning piece of the material placing mechanism.
3. The quartz sand microwave purification apparatus of claim 1, wherein the microwave generation mechanism employs a 2.45GHz solid state microwave source or a 915MHz solid state microwave source;
when the material placing mechanism is placed on the material placing mechanism positioning piece by means of the storage groove, the material placing mechanism is positioned on the long half shaft of the ellipsoidal cavity; when the microwave generating mechanism adopts a 2.45GHz solid microwave source, the distance between the upper surface of the material carrying disc and the lower focus of the ellipsoidal cavity is 30-45 mm, and the diameter of the upper end surface of the material carrying disc is less than or equal to 5cm and less than or equal to 10cm; when the microwave generating mechanism adopts a 915MHz solid-state microwave source, the distance between the upper surface of the material carrying tray and the lower focus of the ellipsoidal cavity is 75-125 mm, and the diameter of the upper end surface of the material carrying tray is less than or equal to 5cm and less than or equal to 15cm.
4. The quartz sand microwave purifying device according to claim 1, wherein the loading tray is detachably connected with the storage tank, the outer surface of the loading tray is provided with loading tray connecting seats at intervals, the upper part of the storage tank is provided with storage tank connecting seats at intervals, mounting through holes are formed in the loading tray connecting seats and the storage tank connecting seats, and the loading tray and the storage tank can be connected through elastic pieces with different specifications by means of the mounting through holes.
5. The quartz sand microwave purification device according to claim 1, wherein a blanking channel is further connected below the loading tray, the blanking channel is communicated with an opening at the bottom of the loading tray, and the length of the blanking channel is less than or equal to 20cm;
The opening is provided with an opening switch, and the blanking channel is provided with a vibrating mechanism.
6. The quartz sand microwave purification method is characterized by comprising the following steps of:
s1, crushing-screening treatment: crushing and screening quartz ores to obtain quartz raw sand with preset size;
s2, initial purification treatment: the quartz raw sand is initially purified in a purification mode comprising magnetic separation, flotation and acid washing;
s3, microwave-water extraction-acid washing integrated purification treatment: applying the quartz sand microwave purification device according to any one of claims 1-5, placing an acid solution in a storage tank, placing a material placing mechanism on a material placing mechanism positioning piece of a lower shell, sealing the upper shell and the lower shell to enable an ellipsoidal cavity to be in a sealed state, vacuumizing through an air outlet pipe until the air pressure in the ellipsoidal cavity reaches a first preset air pressure, introducing HCl gas into the ellipsoidal cavity through a feed pipe until the air pressure in the ellipsoidal cavity reaches a second preset air pressure, starting a microwave generating mechanism, introducing HCl gas into the ellipsoidal cavity through different feed pipes and obtaining quartz sand after the previous purification, wherein the quartz sand falls into a material carrying disc and is heated by the microwave generating mechanism and then falls into the acid solution in the storage tank through an opening for water extraction and acid washing;
S4, microwave-chlorination purification treatment: use of the other claim1-5, placing a material placing mechanism on a material placing mechanism positioning piece of a lower shell, sealing the upper shell and the lower shell to enable an ellipsoidal cavity to be in a sealing state, vacuumizing through an air outlet pipe until the air pressure in the ellipsoidal cavity reaches a third preset air pressure, extracting air in the ellipsoidal cavity from the air outlet pipe of the quartz sand microwave purifying device applied by S3, introducing the extracted air into the ellipsoidal cavity through any one of the feed pipes of the quartz sand microwave purifying device applied by S4, and introducing O into the ellipsoidal cavity through other feed pipes 2 And Cl 2 Starting the microwave generating mechanism until the air pressure in the ellipsoidal cavity reaches a fourth preset air pressure, and respectively introducing the extracted air and O into the ellipsoidal cavity through different feeding pipes 2 、Cl 2 And quartz sand obtained after the purification in the last step falls into a material carrying disc, is heated by a microwave generating mechanism and falls into a storage tank through an opening, and thus the microwave-chlorination purification treatment is completed.
7. The quartz sand microwave purification method of claim 6, wherein the preset size is 50-425 μm; and/or the acid solution in the S3 is a mixed aqueous solution of hydrochloric acid and nitric acid, wherein the weight ratio of the hydrochloric acid to the nitric acid in the acid solution is 1 (1-1.5), the concentration of the hydrochloric acid is 1.5-2.0 mol/L, the concentration of the nitric acid is 1.5-2.0 mol/L, and the weight ratio of quartz sand falling into the storage tank to the acid solution is 1 (3-8); and/or, when S3-S4 is introduced into the quartz sand obtained after the purification in the previous step, vibrating the material carrying disc through a vibrating mechanism on a discharging channel connected below the material carrying disc and communicated with an opening at the bottom of the material carrying disc; and/or, the first preset air pressure and the third preset air pressure are both less than or equal to 1 multiplied by 10 -2 Pa, the second preset air pressure is 13333-34666 Pa, and the fourth preset air pressure is 6666.5-23000 Pa.
8. The method for purifying quartz sand by microwave as claimed in claim 6, wherein when the microwave generating mechanism adopts a 2.45GHz solid microwave source, the flow rate of HCl gas introduced in S3 is 0.1-1.5L/min, and the velocity of quartz sand obtained after the previous purification is 0.5 d2.5kg/min, heating quartz sand to 950-1200 ℃ by a microwave generating mechanism; o introduced in S4 2 The flow ratio of the gas to the gas in the S3 ellipsoidal cavity is (0.1-2.4): 100, and the Cl is introduced 2 The flow ratio of the quartz sand to the gas in the introduced S3 ellipsoidal cavity is (3-20): 100, the speed of the quartz sand obtained after the purification in the last step is 0.5-2.5 kg/min, and the quartz sand is heated to 800-1000 ℃ by a microwave generating mechanism.
9. The quartz sand microwave purification method as claimed in claim 6, wherein when the microwave generating mechanism adopts a 915MHz solid microwave source, the flow rate of HCl gas introduced in S3 is 0.35-6.5L/min, the velocity of quartz sand obtained after the previous purification is 1.5-10 kg/min, and the quartz sand is heated to 950-1200 ℃ by the microwave generating mechanism; o introduced in S4 2 The flow ratio of the gas to the gas in the S3 ellipsoidal cavity is (0.1-2.4): 100, and the Cl is introduced 2 The flow ratio of the quartz sand to the gas in the introduced S3 ellipsoidal cavity is (3-20): 100, the speed of the quartz sand obtained after the purification in the last step is 1.5-10 kg/min, and the quartz sand is heated to 800-1000 ℃ by a microwave generating mechanism.
10. A high purity silica sand, characterized in that it is purified by the silica sand microwave purification method according to any one of claims 6 to 9.
CN202311365589.0A 2023-10-20 2023-10-20 Quartz sand microwave purification device, purification method and high-purity quartz sand Pending CN117401686A (en)

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