Method of estimating quality of quartz raw material

FIELD: chemistry.

SUBSTANCE: application: for identification of the purest types of the quartz raw material. Essence of the invention consists in the following: selection of a monomineral sample of quartz, crushing and quartzification of three samples are carried out. Each sample is subjected to irradiation by γ-quanta with a dose of 10±1×106 Gr. In the first sample after irradiation the content of isomorphic structural Al-O centres in quartz is determined. The third sample before irradiation is subjected to temperature processing at 590-650°C for 20-30 min and the complete content of structural Al-O centres in quartz is determined. The third sample before irradiation is activated by SHF fields with power 700-800 W for 3-5 min, and subjected to temperature processing at 590-650°C for 20-30 min and the content of mobile structures of Al-O centres in quartz is determined. After that, an index of quartz washability, C1 - content of isomorphic structural Al-O centres in quartz, C2 -complete content of structural Al-O centres in quartz, C3 - content of mobile structural Al-O centres in quartz are determined, and if a value of washability index is 0.5-1, conclusion about high quality of the quartz raw material is made.

EFFECT: increased accuracy and rapidity, as well as simplification of the process of estimation of the quartz raw material quality.

1 tbl

 

The invention relates to the study of mineral raw materials, in particular, to methods preliminary evaluation of quartz raw materials.

Especially pure quartz is quartz raw materials, suitable for different enrichment technologies, high quality of concentrates that meet the modern requirements to the purity requirements of the domestic industry and relevant international standards. The increased consumption of highly pure quartz caused by the development of high technologies in electronic, chemical, aerospace and other industries. Directions for the use of quartz are determined by the form of occurrence of the various impurities in the quartz. Modern technologies make it possible to almost completely remove the film, mineral and HIV impurities. However, obtaining high-purity quartz concentrates largely determined by the ability to ensure the removal of structural impurities Al, Ti, Ge and others in the process of enrichment of quartz raw materials. Structural elements of impurities in the crystal lattice, as a rule, are formed in the process of crystallization of quartz at the expense of isomorphism - substitution of atoms of the lattice of quartz impurity atoms, and traditional ways of enrichment technologies removed in a very slight degree. While structural elements of impurities and structural defects determine) the ski properties the solubility parameters of polymorphic transformations and other physico-chemical properties of quartz, which, ultimately, determine its adaptability and usage of quartz. Enrichment of quartz structural impurities can occur in the process of technological conversion of quartz raw materials. To a certain extent, this phenomenon is inevitable, as in quartz in large quantities are scattered (or movable) impurities (Crayfish LT Diffuse impurities in the quartz // "Structure and variety of the mineral world". Proceedings of the International mineralogical seminar. Syktyvkar. 2008. S-266). They represent the atoms of different elements captured by defects in the crystal structure. In beneficiation quartz these impurities diffuse in the defective areas of quartz. The result of this diffusion is the interaction of mobile impurities with other structural defects. Thus, high-temperature processing, widely used in purification processes of quartz, facilitates the introduction of mobile elements-impurities into the crystal lattice and makes them available for retrieval (Crayfish LT Mechanisms of isomorphism in quartz // Geochemistry. 2006. No. 10. S-1096). Of the total number implemented using heat treatment, impurities major part (over 95%), and aluminium is the third. Therefore, the evaluation of quartz raw materials at the stage of geological studies on the suitability of obtaining quartz concentrates with the lowest possible content of structural impurities is important.

From the analysis of the prior art there are known various methods preliminary assessment of quality natural quartz raw materials.

There is a method of assessing the quality of quartz, in which the selection of mono fractions of quartz, calcined to a temperature of 350-450°C, remove a range of rentgenolyuminestsentnye calcined quartz in the spectral wavelength range of 350-550 nm and relative intensity of the emission at a wavelength of 360-380 nm to the intensity of rentgenolyuminestsentnye structurepreserving centers in the spectral range 420-500 nm assess the structure defects and quality quartz (RF patent No. 2400736, 2010).

The disadvantage of this method is that rentgenolyuminestsentnye refers to qualitative methods and is not possible with sufficient accuracy to estimate the quantitative structural content of impurity elements. Furthermore, the method does not assess quartz raw materials with a low concentration of impurity atoms (0,n is 0,0000n% microtonalism).

The known method of finding deposits of very pure quartz, namely, that direct the selection of monomineral samples of quartz for exploration the network, measured in samples quantitative spectral method, the impurity concentration of lithium and when their value is less than 0.5 g/t judge the presence of deposits of very pure quartz (RF patent No. 2145105, 2000).

The disadvantage of this method is the use for estimation is insensitive to spectral analysis, the results of which confirmed the data definition content in the same samples of structural aluminum, which complicates the process of assessing the quality of quartz. In addition, a certain spectral analysis of the concentration of Li does not reflect the real picture quality quartz, as Li can be included in the trace mineral inclusions, and not in the structure of quartz, which reduces the accuracy of assessing the quality of quartz raw materials. The method was tested only with regard to the pegmatitic quartz used to obtain heat-resistant and technical glass.

The closest in technical essence and the achieved result is a way of assessing the quality of quartz, based on the use of electron paramagnetic resonance (EPR), which measures the structural content of impurities in the quartz. According to a known method monomineral finely ground sample of quartz heat-treated, irradiated with γ-rays, doses that translates isomorphic titanium and germanium in ramagnano state, register EPR spectrum and determine the concentration of Ge and Ti centers. Then, the sample is subjected to a special heat treatment (thermal annealing), irradiated with γ-quanta, register EPR spectrum and determine the concentration of Al-O-centers in quartz. The content of said structural impurities in quartz determined based on the maximum concentrations of paramagnetic centers, which allows us to estimate the degree of contamination of the quartz isomorphic impurities Ge, Ti and Al, and to identify the most pure quartz raw materials for use in electronic engineering (Crayfish LT and other "New method for assessing the quality of quartz raw materials. Exploration and conservation of mineral resources", 1993, No. 7, p.36-38).

The disadvantage of this method is that it allows one to determine only the total number of isomorphic structural impurities of Al, Ti and Ge, excluding mobile forms in the internal layers of the damper areas, and does not differentiate between impurities on actually isomorphic and moving, which leads to an overestimation of the threshold process and a decrease in the accuracy assessment of the quality of quartz raw materials. In addition, determination of the three isomorphic structural impurities (Al, Ti, and Ge) complicates the evaluation process and increases its duration. A special high-temperature annealing makes the energy-consuming process.

Task offers the alleged invention is to develop a workable and effective way to evaluate the quality of quartz raw materials, permitting at the preliminary stage of assessment to predict quality quartz and directions of use.

The technical result of the proposed method is to improve the accuracy and expressnet, as well as simplifying the process of assessing the quality of quartz raw materials.

This is achieved in that in the method of estimating quartz raw materials, including the selection of monomineral samples of quartz, grinding, heat treatment, irradiation with γ-quanta, the registration of the EPR spectrum and the determination of structural Al-O-centers in quartz, according to the invention, a sample of quartz divided into three samples, each sample is subjected to irradiation with γ-quanta dose of 10±1×10 Gy, while in the first sample after irradiation determine the content isomorphic structural impurities Al-O-centers, a second sample before irradiation is subjected to heat treatment at a temperature of 590-650°C for 20-30 min and determine the full content of structural Al-O-centers, the third sample before irradiation activates the microwave fields with a capacity of 700-800 watts for 3-5 min, subjected to thermal treatment at 590-650°C for 20-30 min and determine the content of the movable structural Al-O-centers, then determine the rate of enrichment of silica in the mineral sample by the ratio R=(C2-C3)/(C2-C1), the de: P the rate of enrichment of quartz, C1content isomorphic structural Al-O-centers in quartz, With2- full content of structural Al-O-centers in quartz, C3- the content of the movable structural Al-O-centers, and when the value of enrichment of 0.5 to 1 judge of the high quality quartz.

The proposed mode of radiation of γ-quanta dose of 10±1×106Gr gives you the opportunity to get in quartz concentration of paramagnetic Al-O-centers, sufficient for reliable reception of it by the EPR method. Mode quartz heat treatment at temperatures not less than 590-650°C ensures the activation of mobile impurities and implementation of significant parts of the crystal structure of quartz. The measured concentration of Al-O-centers in samples of quartz correspond to various States of the mobile impurities in quartz. The concentration of Al-O-centers in the first sample corresponds to finding moving potential impurities in the damper areas, so the value of C1matches the original content is isomorphic to Al accumulated in quartz in natural conditions. The concentration of Al-O-centers With2in the second sample corresponds to the transition of mobile impurities in the active state and the introduction of their crystalline structure of quartz. The concentration of Al-O-centers C3, metering the controls in the third sample, reflects the influence of the microwave field on the process of implementing mobile Al impurities in the crystal structure of quartz. The proposed processing mode quartz raw materials, including activation of quartz microwave fields at low levels of microwave power (700-800 watts) over a short period of time (3-5 min), accelerates the diffusion of the movable structural impurities from the inner layers of the damping zone to the peripheral, which allows us to differentiate structural admixture of aluminum isomorphic, full and sliding forms and determine their number. The process takes place without contact with metal or dielectric elements of the device, which prevents secondary contamination of the quartz impurities. The rate of enrichment of quartz in the main sample, defined by the ratio (C2-C3)/(C2-C1), shows the percentage of activated mobile impurities offset by the impact of the energy field and is not embedded in the crystalline structure of quartz.

This ultimately provides a more accurate assessment of the quality of quartz raw materials and the reliability of the preliminary assessment quartz. Expressnet and simplification of the evaluation process is achieved by reducing the number of defined elements of impurities in the quartz. The efficiency of the method is provided with the exception of the technological process in comtemplating annealing.

Testing of the proposed method was performed on samples of natural quartz from deposits and occurrences of Karelia: Fenicia-Lampi, Eastern Hitware, Rukavac. Monomineral samples of quartz, selected on a specific object, weighing 200 g crushed to a particle size of 0.5 mm, average and adwareaway 3 sample weighing 2 grams. Each sample is subjected to irradiation with γ-quanta dose of 10±1×106Gr, then register EPR spectrum Al-O-centers, measure the concentration of paramagnetic Al-O-centers and on the basis of their maximum concentrations determine the content of the structural Al-O--centers. The first sample is irradiated with the indicated dose of γ-rays and determine the content isomorphic structural Al-O--centers. A second sample before irradiation with γ-quanta is subjected to thermal processing to 590-650°C for 20-30 min and the EPR method to determine the full content of structural Al-O-centers in quartz. The third sample before irradiation with γ-quanta activate the microwave fields with a capacity of 700-800 watts for 3-5 min, subjected to thermal treatment at 590-650°C for 20-30 min and the EPR method to define the content of the movable structural Al-O-centers. The degree of enrichment of P is determined by the ratio of:

P=(C2-C3)/(C2-C1),where:

C1- the content is isomorphic to the structure of the business Al-O -centres;

C2- full content of structural Al-O-centers

C3- the content of the movable structural Al-O-centers, and when the value of the indicator of the degree of enrichment of 0.5-1.0 judged of high quality quartz.

As the standard of comparison used control - determination of the content of the structural Al-O-centers in natural quartz without activation of the samples microwave fields. Each sample was performed in 10 replicates. The statistically processed data on the content of the structural forms of aluminum and measures of the extent of enrichment of P for quartz of different objects presented in the table.

The table shows that high quality quartz has quartz from fields in Eastern Hitware with the degree of enrichment of P=1.0, with which the mobile form of admixtures of aluminum is fully neutralized and in the process further purification of quartz raw materials will not enter into the crystal lattice of quartz and can be removed traditional enrichment technologies.

Quartz deposits Penkina-Lampi is characterized by the degree of enrichment of P=0,53, in which the mobile form of admixtures of aluminum partially neutralized.

Quartz manifestations Runwalk with the degree of enrichment of P=0,4 is not the source of high-purity quartz raw materials.

Before agemy way of assessing the quality of quartz raw materials increases the efficiency and reliability of the preliminary assessment of enrichment of quartz raw materials and can be used to identify the most pure types of quartz raw materials for applications in electronics, optics, lighting, solar energy and other industries where there are high demands on the purity quartz concentrates.

The method of assessing the quality of quartz raw materials, including the selection of monomineral samples of quartz, grinding, thermal processing, irradiation with γ-quanta, the registration of the EPR spectrum and the determination of structural Al-O-centers in quartz, characterized in that the sample of quartz divided into three samples, each sample is subjected to irradiation with γ-quanta dose of 10±1×106Gr, in the first sample after irradiation to determine the concentration isomorphic structural impurities Al-O-centers, a second sample before irradiation is subjected to thermal treatment at 590-650°C for 20-30 min and determine the full content of structural Al-O-centers in quartz, the third sample before irradiation activates the microwave fields with a capacity of 700-800 watts for 3-5 min, subjected to thermal treatment at 590-650°C for 20-30 min and determine the content of the movable structural Al-O-centers in quartz, then determine the rate of enrichment of silica in the mineral sample by the ratio P=(C2-C3)/(C2-C1), where P is the rate of enrichment of quartz, C1- the content is isomorphic with nocturnia Al-O -centers in quartz, C2- full content of structural Al-O-centers in quartz, C3- the content of the movable structural Al-O-centers, and when the value of 0.5-1 judge of the high quality quartz.



 

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