CN111153409B - Method for purifying quartz sand by utilizing microwave heating and ultrasonic-assisted acid leaching for iron removal - Google Patents

Method for purifying quartz sand by utilizing microwave heating and ultrasonic-assisted acid leaching for iron removal Download PDF

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CN111153409B
CN111153409B CN202010043452.3A CN202010043452A CN111153409B CN 111153409 B CN111153409 B CN 111153409B CN 202010043452 A CN202010043452 A CN 202010043452A CN 111153409 B CN111153409 B CN 111153409B
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陈健
李飞飞
蒋雪松
班伯源
李京伟
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Hefei Institutes of Physical Science of CAS
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Abstract

本发明涉及一种利用微波加热使石英中的含杂质相在400‑1000℃的温度下被加热,促使含铁(Fe)杂质相本身以及相邻的石英基体发生相变,开裂,然后采用超声辅助酸浸的方法除铁。本发明提供的方法能够实现对石英砂中铁杂质超高效去除,铁的含量通过一次去除最低可以降低到0.383ppm以下,去除率最高可以达到99.87%以上,除铁效率要远超其他除铁方法。

Figure 202010043452

The invention relates to a method of using microwave heating to heat the impurity-containing phase in quartz at a temperature of 400-1000°C to promote the phase transformation and cracking of the iron (Fe)-containing impurity phase itself and the adjacent quartz matrix, and then use ultrasonic Auxiliary acid leaching method to remove iron. The method provided by the invention can achieve ultra-efficient removal of iron impurities in quartz sand, the iron content can be reduced to less than 0.383ppm at one time, the removal rate can reach more than 99.87%, and the iron removal efficiency is far higher than other iron removal methods.

Figure 202010043452

Description

一种利用微波加热和超声辅助酸浸除铁提纯石英砂的方法A method for purifying quartz sand by using microwave heating and ultrasonic assisted acid leaching to remove iron

技术领域technical field

本发明涉及矿物提纯领域,具体涉及石英砂生产技术领域,涉及一种利用微波加热和超声辅助酸浸除铁提纯石英砂的方法。The invention relates to the field of mineral purification, in particular to the technical field of quartz sand production, and relates to a method for purifying quartz sand by using microwave heating and ultrasonic-assisted acid leaching to remove iron.

背景技术Background technique

石英砂的主要成分是SiO2,是一种重要的工业原料,被广泛用于玻璃、陶瓷、耐火材料等方面。随着科技的发展,半导体、光纤通讯、航空航天、太阳能、电子等高科技领域对石英玻璃的需求越来越多,对高纯度石英原料的需求也随之不断增大。天然石英石中含有一些杂质元素,其中Fe的存在直接影响到石英砂的使用价值,降低产品的质量。例如,石英砂被用于制造太阳电池多晶硅铸锭的坩埚,由于石英砂中含有一定量的Fe,多晶硅铸锭凝固生长以后,在缓慢冷却过程中,石英坩埚中的Fe在高温下发生扩散从石英砂进入硅铸锭,会在多晶硅铸锭与石英坩埚接触的边沿区域形成不能用于制造太阳电池片的红区,使铸锭质量下降,所以,石英砂中的Fe含量在很多应用中需要尽可能的低。因此,需要尽可能地提高除Fe的效率,降低石英砂中Fe的含量。The main component of quartz sand is SiO 2 , which is an important industrial raw material and is widely used in glass, ceramics, refractory materials and so on. With the development of science and technology, the demand for quartz glass is increasing in high-tech fields such as semiconductors, optical fiber communications, aerospace, solar energy, and electronics, and the demand for high-purity quartz raw materials is also increasing. Natural quartz stone contains some impurity elements, among which the presence of Fe directly affects the use value of quartz sand and reduces the quality of the product. For example, quartz sand is used to manufacture polycrystalline silicon ingot crucibles for solar cells. Since the quartz sand contains a certain amount of Fe, after the polycrystalline silicon ingot solidifies and grows, during the slow cooling process, Fe in the quartz crucible diffuses from When quartz sand enters the silicon ingot, a red zone that cannot be used to manufacture solar cells will be formed in the edge area where the polysilicon ingot contacts the quartz crucible, which will reduce the quality of the ingot. Therefore, the Fe content in quartz sand is required in many applications. as low as possible. Therefore, it is necessary to improve the efficiency of removing Fe as much as possible and reduce the content of Fe in quartz sand.

石英砂除Fe的方法分为物理方法,化学方法和多种手段综合的方法。The methods for removing Fe from quartz sand are divided into physical methods, chemical methods and comprehensive methods.

物理方法包括磁选,色选等,但是只能去除带有磁性的或者有一定颜色的含Fe物质,无法将石英砂中的Fe含量降到很低的水平。Physical methods include magnetic separation, color separation, etc., but they can only remove magnetic or colored Fe-containing substances, and cannot reduce the Fe content in quartz sand to a very low level.

化学方法主要是酸浸法,又分为单一酸法和混合酸法,研究发现,几种酸的混合物能够在反应过程中产生协同作用,其效果比单一酸的浸取效果要好得多。Veglio F .等用草酸和硫酸混合浸取石英砂中的铁,其浸出率(去除率)为35-45%,而单独用硫酸,同样条件下的浸出率(去除率)仅为3-9%( “ Leahing test in iron removal from quartzusing oxalic and sulphuric acids”, Veglio F, Passariello B., Barbaro M.,Plescia P., Marabini A. M. Drum. Int. J. Miner. Process. 1998, 54, 183-200)。刘闯等通过碱溶蚀与硫酸浸取相结合的方法处理石英砂,达到除铁的目的(参见“ 石英砾石碱溶蚀法研制高纯石英砂”,刘闯等,资源调查与环境,2006,27(7),286-289)。由于石英砂中的Fe杂质只有部分是位于石英砂的表面,还有部分Fe杂质位于石英砂颗粒的内部,不能与酸液接触,因此单独依靠酸浸方法,也无法将石英砂中的Fe含量降低到很低的水平。The chemical method is mainly acid leaching method, which is divided into single acid method and mixed acid method. It is found that the mixture of several acids can produce synergistic effect in the reaction process, and its effect is much better than the leaching effect of single acid. Veglio F. etc. mixed oxalic acid and sulfuric acid to leaching iron in quartz sand, the leaching rate (removal rate) was 35-45%, while using sulfuric acid alone, the leaching rate (removal rate) was only 3-9% under the same conditions %("Leahing test in iron removal from quartzusing oxalic and sulfuric acids", Veglio F, Passariello B., Barbaro M., Plescia P., Marabini A. M. Drum. Int. J. Miner. Process. 1998, 54, 183-200 ). Liu Chuang et al. treated quartz sand by combining alkali dissolution and sulfuric acid leaching to achieve the purpose of iron removal (see "Preparation of High-purity Quartz Sand by Alkali Dissolution of Quartz Gravel", Liu Chuang et al., Resource Investigation and Environment, 2006, 27 (7), 286-289). Since the Fe impurities in the quartz sand are only partially located on the surface of the quartz sand, and some of the Fe impurities are located inside the quartz sand particles and cannot contact with the acid solution, so the acid leaching method alone cannot reduce the Fe content in the quartz sand. down to a very low level.

采用多种手段综合提纯的方法可以获得比单独物理方法提纯或者化学方法提纯更好的提纯效果。主要工艺过程包括煅烧,水淬,破碎,磁选,浮选,酸浸,烘干等步骤。专利申请CN110510620A,将石英矿在1050-1100℃高温煅烧2-4hrs;然后水淬,再用草酸和硫氰酸的混合酸进行酸浸:提纯后石英砂中的Fe2O3含量为0.015%(150ppm)。在众多类似的专利申请以及工业生产实践中,一般石英矿石的煅烧温度在900-1100℃,酸浸都只是在一个容器中室温或者加热的情况下较长时间的浸泡,如果原矿中Fe的含量较高,通过这个过程,并不能快速把Fe的含量降到一个很低的水平。通常,采用较高的煅烧处理温度,由于石英材料基体在高温下会发生相转变,经过淬火处理以后产生微裂纹,处理温度越高,淬火以后产生的微裂纹会更多,从而有利于包裹体等杂质的去除,从这个方面看,提高石英材料的煅烧处理温度有利于杂质的去除。但是,石英砂由于具有一个比较开放的晶体结构,特别是由于石英在573℃和870℃分别存在有α石英-β石英的相变和石英-鳞石英的相变,转变为高温相以后,石英基体发生体积膨胀,晶体结构更加松散,Fe等间隙式杂质原子能够在石英基体松散的晶格中以更快的速度扩散。Fe在石英材料中,往往是以杂质相的形式富集于固相包裹体或者流体包裹体如长石、磁铁矿、液体包裹体中,在高温处理的条件下,Fe可以从杂质相向石英基体的晶格中发生扩散,进入石英晶格中,一旦Fe进入到石英基体晶格中,由于酸液无法进入石英晶格,所以再也无法用酸浸的方式去除,因此对石英材料采用高温煅烧处理,会导致Fe从杂质相向石英基体扩散进入石英晶格,成为晶格Fe而无法去除,石英砂杂质Fe的去除率降低,从而限制了高温煅烧的应用以及煅烧温度的提高。而且,依靠高温煅烧+水淬的方法使石英基体产生微裂纹的方法,还存在能耗高,操作繁琐的问题。A comprehensive purification method using multiple means can obtain a better purification effect than individual physical method purification or chemical method purification. The main process includes calcination, water quenching, crushing, magnetic separation, flotation, acid leaching, drying and other steps. Patent application CN110510620A, the quartz ore is calcined at 1050-1100°C for 2-4hrs; then quenched in water, and then pickled with a mixed acid of oxalic acid and thiocyanic acid: the content of Fe 2 O 3 in the purified quartz sand is 0.015% (150ppm). In many similar patent applications and industrial production practices, the calcination temperature of quartz ore is generally 900-1100°C, and the acid leaching is just soaking in a container at room temperature or heating for a long time. If the content of Fe in the raw ore Higher, through this process, the content of Fe cannot be quickly reduced to a very low level. Usually, a higher calcination treatment temperature is adopted, because the quartz material matrix will undergo phase transformation at high temperature, and microcracks will be generated after quenching treatment. The higher the treatment temperature, the more microcracks will be produced after quenching, which is beneficial to inclusions From this point of view, increasing the calcination temperature of quartz materials is beneficial to the removal of impurities. However, due to the relatively open crystal structure of quartz sand, especially because quartz has a phase transition of α-quartz-β-quartz and a phase transition of quartz-tridymite at 573°C and 870°C respectively, after it transforms into a high-temperature phase, the quartz The volume of the matrix expands, the crystal structure becomes looser, and interstitial impurity atoms such as Fe can diffuse at a faster rate in the loose crystal lattice of the quartz matrix. In quartz materials, Fe is often enriched in solid phase inclusions or fluid inclusions such as feldspar, magnetite, and liquid inclusions in the form of impurity phases. Under high temperature treatment, Fe can move from impurities to quartz. Diffusion occurs in the crystal lattice of the matrix and enters the quartz lattice. Once Fe enters the quartz matrix lattice, since the acid solution cannot enter the quartz lattice, it can no longer be removed by acid leaching. Therefore, high temperature is used for quartz materials. Calcination treatment will cause Fe to diffuse from the impurity phase to the quartz matrix and enter the quartz lattice, becoming lattice Fe and cannot be removed, and the removal rate of quartz sand impurity Fe is reduced, which limits the application of high-temperature calcination and the increase of calcination temperature. Moreover, relying on high-temperature calcination + water quenching to produce microcracks in the quartz substrate also has the problems of high energy consumption and cumbersome operations.

随着科技的发展,对石英砂的纯度要求越来越高,如何快速高效率去除石英砂中的Fe杂质也变得越来越重要,而现有的技术难以满足高效快速除Fe的要求。With the development of science and technology, the requirements for the purity of quartz sand are getting higher and higher, and how to quickly and efficiently remove Fe impurities in quartz sand is becoming more and more important, but the existing technology is difficult to meet the requirements of high-efficiency and rapid removal of Fe.

发明内容Contents of the invention

为了解决上述问题,采用微波加热和超声辅助酸浸的方法来实现高效除铁。In order to solve the above problems, microwave heating and ultrasonic assisted acid leaching are used to achieve efficient iron removal.

本发明是通过以下技术方案实现的:The present invention is achieved through the following technical solutions:

一种利用微波加热和超声辅助酸浸除铁提纯石英砂的方法,所述方法包括以下步骤:A method for purifying quartz sand by microwave heating and ultrasonic-assisted acid leaching to remove iron, said method comprising the following steps:

(1) 将石英矿石使用微波加热至预定温度并保温一定时间后,关闭微波功率冷却至室温;(1) After heating the quartz ore to a predetermined temperature using microwaves and keeping it warm for a certain period of time, turn off the microwave power and cool it down to room temperature;

(2) 将步骤(1)加热处理后的石英矿石进行机械破碎至形成石英砂;(2) mechanically crushing the quartz ore after the heat treatment in step (1) to form quartz sand;

(3) 将步骤(2)所获得石英砂样品与酸性溶液混合形成矿浆,将矿浆放入超声清洗设备中在室温或者加热条件下进行超声辅助酸浸处理,酸浸处理完成后,关闭超声,矿浆自然冷却至室温;(3) Mix the quartz sand sample obtained in step (2) with an acidic solution to form a pulp, put the pulp into an ultrasonic cleaning device and perform ultrasonic-assisted acid leaching at room temperature or under heating conditions, after the acid leaching is completed, turn off the ultrasonic, The pulp is naturally cooled to room temperature;

(4) 将步骤(3)中的石英砂从矿浆中过滤分离出来以后用去离子水冲洗至pH接近中性后放入干净的容器中烘干,获得低铁的石英砂产品。(4) After the quartz sand in step (3) is filtered and separated from the pulp, it is rinsed with deionized water until the pH is close to neutral, and then put into a clean container for drying to obtain a low-iron quartz sand product.

其中,步骤(1)所述石英矿石是颗粒尺寸大于1mm的含有大量SiO2成分的天然矿石,微波加热温度是400-1000℃,保温时间30-600min。优选地,步骤(1)所述微波加热温度是400-870℃。进一步优选地,步骤(1)所述微波加热温度是400-573℃。Wherein, the quartz ore in the step (1) is a natural ore with a particle size greater than 1 mm containing a large amount of SiO 2 , the microwave heating temperature is 400-1000° C., and the holding time is 30-600 min. Preferably, the microwave heating temperature in step (1) is 400-870°C. Further preferably, the microwave heating temperature in step (1) is 400-573°C.

优选地,步骤(3)所述酸性溶液为HNO3、H2SO4、HCl、HF、H3PO4、CH3COOH、C2H2O4中的一种或者两种以上的混合物与水形成的酸液,酸液浓度可以依据实际情况进行调节:矿浆的固/液比依据情况进行调节。Preferably, the acidic solution in step (3) is one or a mixture of two or more of HNO 3 , H 2 SO 4 , HCl, HF, H 3 PO 4 , CH 3 COOH, C 2 H 2 O 4 and The acid liquid formed by water, the concentration of the acid liquid can be adjusted according to the actual situation: the solid/liquid ratio of the pulp can be adjusted according to the situation.

本发明的有益效果在于:The beneficial effects of the present invention are:

微波具有选择性加热的特性,石英砂基体吸收微波能量的能力很弱,不能被微波有效加热,而石英砂内部的含Fe杂质相可以较好地吸收微波的能量,能够被快速地加热,由于热传导效应,含铁杂质相邻近的石英基体也会达到比较高的温度,而与杂质相距离较远的基体依然维持在相对较低的温度,当石英基体温度超过相变点温度时,会发生相变,石英基体发生体积膨胀,在随后的淬火快速冷却时,石英基体发生收缩,在这个冷热循环中,杂质相周边的基体中会产生微裂纹。因此采用微波加热,冷却石英,可以在促进杂质相附近产生微裂纹的同时,较好地抑制Fe在高温下从杂质相向石英基体的扩散,再将微波加热处理过的石英矿石通过机械破碎制成石英砂,然后通过超声波辅助酸浸,促进酸液在超声波的协助下,沿着微裂纹进入石英砂内部,和含Fe杂质相反应,使Fe溶解以后去除。实现对石英砂中铁杂质超高效去除,铁的含量通过一次去除最低可以降低到0.383ppm以下,去除率最高可以达到99.87%以上,除铁效率要远超其他除铁的方法。Microwaves have the characteristic of selective heating. The ability of the quartz sand matrix to absorb microwave energy is very weak and cannot be effectively heated by microwaves. However, the Fe-containing impurity phase inside the quartz sand can absorb microwave energy well and can be heated rapidly. Due to the heat conduction effect, the quartz matrix adjacent to the iron-containing impurities will also reach a relatively high temperature, while the matrix far away from the impurities will still maintain a relatively low temperature. When the temperature of the quartz matrix exceeds the phase transition temperature, it will A phase transition occurs, and the volume of the quartz matrix expands. When the subsequent quenching and rapid cooling occurs, the quartz matrix shrinks. In this cold and hot cycle, microcracks will be generated in the matrix around the impurity phase. Therefore, the use of microwave heating and cooling of quartz can promote the generation of microcracks near the impurity phase, and at the same time, it can better inhibit the diffusion of Fe from the impurity phase to the quartz matrix at high temperature, and then the microwave-heated quartz ore is made by mechanical crushing. The quartz sand is then acid leached by ultrasonic waves to promote the acid solution to enter the interior of the quartz sand along the micro-cracks with the assistance of ultrasonic waves, and react with Fe-containing impurities to dissolve and remove Fe. Realize the ultra-efficient removal of iron impurities in quartz sand. The iron content can be reduced to less than 0.383ppm after one removal, and the removal rate can reach more than 99.87%. The iron removal efficiency is far higher than other iron removal methods.

附图说明Description of drawings

图1为本发明石英砂高效除铁方法的工艺流程图。Fig. 1 is the process flow diagram of the high-efficiency iron removal method for quartz sand of the present invention.

具体实施方式detailed description

下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。The present invention will be described in detail below in conjunction with specific embodiments. The following examples will help those skilled in the art to further understand the present invention, but do not limit the present invention in any form. It should be noted that those skilled in the art can make several modifications and improvements without departing from the concept of the present invention. These all belong to the protection scope of the present invention.

实施例1-4,采用微波加热,将矿石加热至400、600、800、1000℃,保温1hr,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2 mol/L HNO3,在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的284.876ppm分别下降到:0.383ppm、2.063ppm、6.823ppm、8.410ppm,去除率分别达到99.87%、99.28%、97.61%、97.05%。通过上述步骤处理以后,Fe的含量均得到大幅度降低,但是随着微波加热温度的提高,残余Fe的含量逐步提高,Fe的去除率逐步降低。Example 1-4, using microwave heating, heating the ore to 400, 600, 800, 1000°C, and keeping it warm for 1hr. After the sample is cooled, take the ore out of the microwave heating device, and use the mechanical crushing method to crush the quartz ore to 80- 120 mesh, and then, with 2 mol/L HNO 3 , ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 284.876ppm of the quartz raw ore to: 0.383ppm, 2.063ppm, 6.823ppm, 8.410ppm, and the removal rates reach 99.87%, 99.28ppm, respectively. %, 97.61%, 97.05%. After the above steps, the content of Fe was greatly reduced, but with the increase of microwave heating temperature, the content of residual Fe gradually increased, and the removal rate of Fe decreased gradually.

实施例5-8,采用微波加热,将矿石加热至400℃,保温30、45、60、600min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2mol/L HNO3,在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm分别下降到:0.534ppm、0.895ppm、0.958ppm、1.845ppm,去除率分别为:99.836%、99.725%、99.705%、99.432%。通过上述步骤处理以后,Fe的含量均得到大幅度降低,但是随着微波加热时间增长,残余Fe的含量逐步提高,Fe的去除率逐步降低。Example 5-8, microwave heating is used to heat the ore to 400°C and keep it warm for 30, 45, 60, and 600 minutes. After the sample is cooled, the ore is taken out from the microwave heating device, and the quartz ore is crushed to 80- 120 mesh, and then, with 2mol/L HNO 3 , ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the quartz raw ore to: 0.534ppm, 0.895ppm, 0.958ppm, 1.845ppm, and the removal rates are: 99.836%, 99.725ppm %, 99.705%, 99.432%. After the above steps, the content of Fe was greatly reduced, but with the increase of microwave heating time, the content of residual Fe gradually increased, and the removal rate of Fe gradually decreased.

实施例9-13,采用微波加热,将矿石加热至400℃,保温30min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,分别用2、1、2、1、1mol/L的CH3COOH、C2H2O4、HCl、H3PO4、H2SO4在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm分别下降到:10.016ppm、1.838ppm、6.370ppm、8.880ppm、5.921ppm去除率分别为: 96.9%、99.43%、98.04%、97.27%、98.18%。综合实施例5,可以知道,通过上述步骤处理以后,Fe的含量均得到大幅度降低,不同种类的酸对石英砂中的Fe均有较显著的去除效果。Examples 9-13, microwave heating is used to heat the ore to 400°C and keep it warm for 30 minutes. After the sample is cooled, the ore is taken out from the microwave heating device, and the quartz ore is crushed to 80-120 mesh by mechanical crushing method, and then, respectively Use 2, 1, 2, 1, 1 mol/L CH 3 COOH, C 2 H 2 O 4 , HCl, H 3 PO 4 , H 2 SO 4 for ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the raw quartz ore to: 10.016ppm, 1.838ppm, 6.370ppm, 8.880ppm, 5.921ppm. The removal rates are respectively: 96.9% , 99.43%, 98.04%, 97.27%, 98.18%. Based on Example 5, it can be seen that after the above steps, the content of Fe is greatly reduced, and different types of acids have a significant removal effect on Fe in quartz sand.

在对比例1中,石英砂处理流程与实施例1-4相似,只是把微波加热温度进一步降低到200℃,处理以后,石英砂中残余的Fe的含量从石英原矿的284.876ppm下降至24.630ppm,去除率为91.36%,残余Fe的含量显著高于实施例1-4的情况。In Comparative Example 1, the quartz sand treatment process is similar to that of Examples 1-4, except that the microwave heating temperature is further reduced to 200°C. After the treatment, the residual Fe content in the quartz sand drops from 284.876ppm of the raw quartz ore to 24.630ppm , the removal rate was 91.36%, and the content of residual Fe was significantly higher than that of Examples 1-4.

在对比例2中,不采用微波加热处理石英矿,直接破碎,然后采用酸浸处理,获得的石英砂中残余的Fe的含量从石英原矿的325ppm下降至51.234ppm,去除率为84.236%,残余Fe的含量显著高于实施例的情况。In Comparative Example 2, the quartz ore was directly crushed without microwave heating, and then treated with acid leaching. The content of residual Fe in the obtained quartz sand dropped from 325ppm of the original quartz ore to 51.234ppm, and the removal rate was 84.236%. The content of Fe was significantly higher than in the case of Examples.

在对比例3中,采用普通的电阻加热到800℃,保温2hrs。采用机械破碎方法将石英矿破碎至80-120目,使用2 mol/L HNO3,在90℃酸浸2hrs,所获得的样品Fe的含量从石英原矿的325ppm下降至81.126ppm,去除率为75.038 %,残余Fe的含量大幅度高于实施例的情况。In comparative example 3, ordinary resistance heating was used to heat to 800° C., and the temperature was kept for 2 hrs. The quartz ore was crushed to 80-120 mesh by mechanical crushing method, and 2 mol/L HNO 3 was used for acid leaching at 90°C for 2hrs. The content of Fe in the obtained sample dropped from 325ppm of the raw quartz ore to 81.126ppm, and the removal rate was 75.038 %, the content of residual Fe is significantly higher than that of the examples.

在对比例4中,采用微波加热到400℃,缩短保温时间到15min,样品冷却后。采用机械破碎方法将石英矿破碎至80-120目,使用2 mol/L HNO3,在90℃酸浸2hrs,所获得的样品Fe的含量从石英原矿的325ppm下降至15.859ppm,去除率为95.120 %,残余Fe的含量大幅度高于实施例5-8的情况。In comparative example 4, the microwave was used to heat to 400°C, the holding time was shortened to 15min, and the sample was cooled. The quartz ore was crushed to 80-120 mesh by mechanical crushing method, and 2 mol/L HNO 3 was used for acid leaching at 90°C for 2 hours. The content of Fe in the obtained sample decreased from 325ppm of the raw quartz ore to 15.859ppm, and the removal rate was 95.120 %, the content of residual Fe is significantly higher than that of Examples 5-8.

实施例和对比例如下:Embodiment and comparative example are as follows:

实施例1Example 1

如图1所示,先将石英矿石放进微波加热装置中,打开微波,对石英矿石进行加热到400℃,保温1hr,关闭微波,使矿石自然冷却。冷却以后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2 mol/L HNO3,在90℃超声酸浸2hrs。所获得的样品Fe的含量从石英原矿的284.876ppm下降至0.383ppm,去除率达到99.87%。As shown in Figure 1, put the quartz ore into the microwave heating device first, turn on the microwave, heat the quartz ore to 400°C, keep it warm for 1 hour, turn off the microwave, and let the ore cool naturally. After cooling, the ore is taken out from the microwave heating device, and the quartz ore is crushed to 80-120 mesh by mechanical crushing method, and then ultrasonic acid leaching is performed at 90°C for 2hrs with 2 mol/L HNO 3 . The content of Fe in the obtained samples decreased from 284.876ppm of quartz ore to 0.383ppm, and the removal rate reached 99.87%.

实施例2Example 2

将石英矿石放进微波加热装置中,打开微波,对石英矿石进行加热到600℃,保温1hr,关闭微波,使矿石自然冷却。冷却以后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2 mol/L HNO3,在90℃超声酸浸2hrs。所获得的样品Fe的含量从石英原矿的284.876ppm下降至2.063ppm,去除率达到99.28%。Put the quartz ore into the microwave heating device, turn on the microwave, heat the quartz ore to 600°C, keep it warm for 1 hour, turn off the microwave, and let the ore cool naturally. After cooling, the ore is taken out from the microwave heating device, and the quartz ore is crushed to 80-120 mesh by mechanical crushing method, and then ultrasonic acid leaching is performed at 90°C for 2hrs with 2 mol/L HNO 3 . The content of Fe in the obtained sample decreased from 284.876ppm of quartz ore to 2.063ppm, and the removal rate reached 99.28%.

实施例3Example 3

将石英矿石放进微波加热装置中,打开微波,对石英矿石进行加热到800℃,保温1hr,关闭微波,使矿石自然冷却。冷却以后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2mol/L HNO3,在90℃超声酸浸2hrs。所获得的样品Fe的含量从石英原矿的284.876ppm下降至6.823ppm,去除率达到97.61%。Put the quartz ore into the microwave heating device, turn on the microwave, heat the quartz ore to 800°C, keep it warm for 1 hour, turn off the microwave, and let the ore cool naturally. After cooling, take the ore out of the microwave heating device, use mechanical crushing method to crush the quartz ore to 80-120 mesh, and then use 2mol/L HNO 3 , ultrasonic acid leaching at 90°C for 2hrs. The content of Fe in the obtained samples decreased from 284.876ppm of quartz ore to 6.823ppm, and the removal rate reached 97.61%.

实施例4Example 4

将石英矿石放进微波加热装置中,打开微波,对石英矿石进行加热到1000℃,保温1hr,关闭微波,使矿石自然冷却。冷却以后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2mol/L HNO3,在90℃超声酸浸2hrs。所获得的样品Fe的含量从石英原矿的284.876ppm下降至8.410ppm,去除率达到97.05%。Put the quartz ore into the microwave heating device, turn on the microwave, heat the quartz ore to 1000°C, keep it warm for 1 hour, turn off the microwave, and let the ore cool naturally. After cooling, take the ore out of the microwave heating device, use mechanical crushing method to crush the quartz ore to 80-120 mesh, and then use 2mol/L HNO 3 , ultrasonic acid leaching at 90°C for 2hrs. The content of Fe in the obtained samples decreased from 284.876ppm in quartz ore to 8.410ppm, and the removal rate reached 97.05%.

实施例5Example 5

采用微波加热,将矿石加热至400℃,保温30min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2 mol/L HNO3,在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm下降到0.534ppm,去除率为99.836%。Microwave heating is used to heat the ore to 400°C and keep it warm for 30 minutes. After the sample is cooled, the ore is taken out from the microwave heating device, and the quartz ore is crushed to 80-120 mesh by mechanical crushing method, and then, 2 mol/L HNO 3 , Ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the raw quartz ore to 0.534ppm, and the removal rate is 99.836%.

实施例6Example 6

采用微波加热,将矿石加热至400℃,保温45min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2 mol/L HNO3,在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm下降到0.895ppm,去除率为99.725%。Microwave heating is used to heat the ore to 400°C and keep it warm for 45 minutes. After the sample is cooled, the ore is taken out from the microwave heating device, and the quartz ore is crushed to 80-120 mesh by mechanical crushing method, and then, 2 mol/L HNO 3 , Ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the raw quartz ore to 0.895ppm, and the removal rate is 99.725%.

实施例7Example 7

采用微波加热,将矿石加热至400℃,保温60min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2 mol/L HNO3,在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm下降到0.958ppm,去除率为99.705%。Microwave heating was used to heat the ore to 400°C and keep it warm for 60 minutes. After the sample was cooled, the ore was taken out from the microwave heating device, and the quartz ore was crushed to 80-120 mesh by mechanical crushing method, and then, 2 mol/L HNO 3 , Ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the raw quartz ore to 0.958ppm, and the removal rate is 99.705%.

实施例8Example 8

采用微波加热,将矿石加热至400℃,保温600min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2 mol/L HNO3,在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm下降到1.845ppm,去除率为99.432%。Microwave heating is used to heat the ore to 400°C and keep it warm for 600 minutes. After the sample is cooled, the ore is taken out from the microwave heating device, and the quartz ore is crushed to 80-120 mesh by mechanical crushing method, and then, 2 mol/L HNO 3 , Ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the raw quartz ore to 1.845ppm, and the removal rate is 99.432%.

实施例9Example 9

采用微波加热,将矿石加热至400℃,保温30min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2 mol/L的CH3COOH在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm下降到10.016ppm,Fe的去除率为96.9%。Using microwave heating, heat the ore to 400°C and keep it warm for 30 minutes. After the sample is cooled, take the ore out of the microwave heating device, use mechanical crushing method to crush the quartz ore to 80-120 mesh, and then use 2 mol/L CH 3 COOH ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the raw quartz ore to 10.016ppm, and the removal rate of Fe is 96.9%.

实施例10Example 10

采用微波加热,将矿石加热至400℃,保温30min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用1 mol/L的C2H2O4在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm下降到1.838ppm,Fe的去除率为99.43%。Using microwave heating, heat the ore to 400°C and keep it warm for 30 minutes. After the sample is cooled, take the ore out of the microwave heating device, use mechanical crushing method to crush the quartz ore to 80-120 mesh, and then use 1 mol/L C 2 H 2 O 4 Ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the raw quartz ore to 1.838ppm, and the removal rate of Fe is 99.43%.

实施例11Example 11

采用微波加热,将矿石加热至400℃,保温30min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2mol/L的HCl在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm下降到6.370ppm,Fe的去除率为98.04%。Microwave heating is used to heat the ore to 400°C and keep it warm for 30 minutes. After the sample is cooled, the ore is taken out from the microwave heating device, and the quartz ore is crushed to 80-120 mesh by mechanical crushing method. Then, use 2mol/L HCl in Ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the raw quartz ore to 6.370ppm, and the removal rate of Fe is 98.04%.

实施例12Example 12

采用微波加热,将矿石加热至400℃,保温30min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用1mol/L的H3PO4在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm下降到8.880ppm,Fe的去除率为97.27%。Microwave heating is used to heat the ore to 400°C and keep it warm for 30 minutes. After the sample is cooled, the ore is taken out from the microwave heating device, and the quartz ore is crushed to 80-120 mesh by mechanical crushing method, and then, 1mol/L H 3 PO 4 ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the raw quartz ore to 8.880ppm, and the removal rate of Fe is 97.27%.

实施例13Example 13

采用微波加热,将矿石加热至400℃,保温30min,样品冷却后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用1mol/L的H2SO4在90℃超声酸浸2hrs。酸浸完成以后,将石英砂清洗烘干,获得的石英砂的含Fe量从石英原矿的325ppm下降到5.921ppm,Fe的去除率为98.18%。Using microwave heating, heat the ore to 400°C and keep it warm for 30 minutes. After the sample is cooled, take the ore out of the microwave heating device, use mechanical crushing method to crush the quartz ore to 80-120 mesh, and then use 1mol/L H 2 SO 4 Ultrasonic pickling at 90°C for 2hrs. After the acid leaching is completed, the quartz sand is washed and dried, and the Fe content of the obtained quartz sand drops from 325ppm of the raw quartz ore to 5.921ppm, and the removal rate of Fe is 98.18%.

对比例1Comparative example 1

将石英矿石放进微波加热装置中,打开微波,对石英矿石进行加热到200℃,保温1hr,关闭微波,使矿石自然冷却。冷却以后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2 mol/L HNO3,在90℃超声酸浸2hrs。所获得的样品Fe的含量从石英原矿的284.876ppm下降至24.630ppm,去除率为91.36%。Put the quartz ore into the microwave heating device, turn on the microwave, heat the quartz ore to 200°C, keep it warm for 1 hour, turn off the microwave, and let the ore cool naturally. After cooling, the ore is taken out from the microwave heating device, and the quartz ore is crushed to 80-120 mesh by mechanical crushing method, and then ultrasonic acid leaching is performed at 90°C for 2hrs with 2 mol/L HNO 3 . The content of Fe in the obtained samples decreased from 284.876ppm of quartz ore to 24.630ppm, and the removal rate was 91.36%.

对比例2Comparative example 2

将石英矿石采用机械破碎方法将石英矿破碎至80-120目,然后,用2 mol/L HNO3,在90℃酸浸2hrs。所获得的样品Fe的含量从石英原矿的325ppm下降至51.234ppm,去除率为84.236%。The quartz ore is crushed to 80-120 mesh by mechanical crushing method, and then acid leached with 2 mol/L HNO 3 at 90°C for 2hrs. The content of Fe in the obtained sample decreased from 325ppm of quartz ore to 51.234ppm, and the removal rate was 84.236%.

对比例3Comparative example 3

将石英矿石采用电阻加热到800℃,保温2hrs。采用机械破碎方法将石英矿破碎至80-120目,使用2 mol/L HNO3,在90℃酸浸 2hrs,所获得的样品Fe的含量从石英原矿的325ppm下降至81.126ppm,去除率为75.038%The quartz ore is heated to 800°C by resistance and kept for 2hrs. The quartz ore was crushed to 80-120 mesh by mechanical crushing method, and 2 mol/L HNO 3 was used for acid leaching at 90°C for 2hrs. The content of Fe in the obtained sample dropped from 325ppm of the raw quartz ore to 81.126ppm, and the removal rate was 75.038 %

对比例4Comparative example 4

将石英矿石放进微波加热装置中,打开微波,对石英矿石进行加热到400℃,保温15min,关闭微波,使矿石自然冷却。冷却以后,将矿石从微波加热装置内取出,采用机械破碎方法将石英矿破碎至80-120目,然后,用2mol/L HNO3,在90℃超声酸浸2hrs。所获得的样品Fe的含量从石英原矿的325ppm下降至15.859ppm,去除率95.120%。Put the quartz ore into the microwave heating device, turn on the microwave, heat the quartz ore to 400°C, keep it warm for 15 minutes, turn off the microwave, and let the ore cool naturally. After cooling, take the ore out of the microwave heating device, use mechanical crushing method to crush the quartz ore to 80-120 mesh, and then use 2mol/L HNO 3 , ultrasonic acid leaching at 90°C for 2hrs. The content of Fe in the obtained sample decreased from 325ppm of quartz ore to 15.859ppm, and the removal rate was 95.120%.

综上所述,采用微波对石英矿石在400-1000℃加热,再把矿石制备成石英砂,然后采用超声波辅助酸浸的方法,可以获得超高的Fe的去除率,残余Fe的含量可以降低到非常低的水平。To sum up, using microwaves to heat quartz ore at 400-1000°C, and then preparing the ore into quartz sand, and then using ultrasonic-assisted acid leaching, can obtain a super high removal rate of Fe, and the content of residual Fe can be reduced. to very low levels.

以上所述实施方式仅仅是对本发明的优选实施方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案做出的各种变形和改进,均应落入本发明的权利要求书确定的保护范围内。The above-mentioned embodiments are only descriptions of the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. Variations and improvements should fall within the scope of protection defined by the claims of the present invention.

Claims (4)

1. A method for removing iron and purifying quartz sand by microwave heating and ultrasonic-assisted acid leaching is characterized by comprising the following steps:
(1) Heating quartz ore to a preset temperature by using microwaves, preserving heat for a certain time, and then closing the microwave power to cool the quartz ore to room temperature;
(2) Mechanically crushing the quartz ore subjected to the heating treatment in the step (1) to form quartz sand;
(3) Mixing the quartz sand sample obtained in the step (2) with an acidic solution to form ore pulp, putting the ore pulp into ultrasonic cleaning equipment, carrying out ultrasonic auxiliary acid leaching treatment at room temperature or under a heating condition, turning off the ultrasonic after the acid leaching treatment is finished, and naturally cooling the ore pulp to the room temperature;
(4) Filtering and separating the quartz sand in the step (3) from the ore pulp, washing the quartz sand with deionized water until the pH value is close to neutrality, and then putting the quartz sand into a clean container for drying to obtain a low-iron quartz sand product;
the microwave heating temperature in the step (1) is 400-600 ℃.
2. The method of claim 1, wherein: the quartz ore in the step (1) is a quartz ore with a particle size of more than 1mm and contains a large amount of SiO 2 The heat preservation time of the natural ore of the components is 30-600min.
3. The method of claim 1, wherein: the microwave heating temperature in the step (1) is 400-573 ℃.
4. The method of claim 1, wherein: the acidic solution in the step (3) is HNO 3 、H 2 SO 4 、HCl、HF、H 3 PO 4 、CH 3 COOH、C 2 H 2 O 4 One or a mixture of two or more of them and water.
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