CN112916199A - Quartz raw material purification method - Google Patents

Quartz raw material purification method Download PDF

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Publication number
CN112916199A
CN112916199A CN202110158174.0A CN202110158174A CN112916199A CN 112916199 A CN112916199 A CN 112916199A CN 202110158174 A CN202110158174 A CN 202110158174A CN 112916199 A CN112916199 A CN 112916199A
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quartz
flotation
acid solution
magnetic
placer
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杨晓勇
岳迅
孙超
侯琪
曹荆亚
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University of Science and Technology of China USTC
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University of Science and Technology of China USTC
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B9/00General arrangement of separating plant, e.g. flow sheets

Abstract

The invention relates to a quartz raw material purification method, which comprises the following steps: (1) grinding ore; (2) magnetic separation and rough separation; (3) magnetic separation and fine selection; (4) performing flotation and roughing; (5) flotation and fine selection; (6) and acid leaching to obtain final quartz concentrate. By taking the samples of Fengyang county quartzite ores as an example, the optimal magnetic flotation and acid leaching conditions are determined, certain reference can be provided for enterprises in Fengyang county producing high-purity quartz at present, and the utilization rate and the utilization value of Fengyang quartz resources are improved.

Description

Quartz raw material purification method
Technical Field
The invention relates to a quartz raw material purification method, and belongs to the field of mineral processing technologies.
Background
At present, the production processes of Fengyang quartz sand are numerous, and the two production processes are mainly as follows: firstly, wet production, namely crushing a stone wheel for grinding ores, adding water for washing, magnetically separating and hydraulically classifying; the second is dry production, which adopts crushing, desliming, mechanical crushing, magnetic separation and screening. The wet-process quartz sand is washed by water in the production process, so that the impurity content in the wet-process quartz sand is low, the impurity content in the dry-process quartz sand is higher due to the absence of the process in the dry-process production, and in addition, a large amount of mechanical iron is brought in the crushing process in the dry-process production, so that the iron content in the dry-process quartz sand is obviously higher than that in the wet-process quartz sand.
At present, a few Fengyang sand enterprises adopt rod mills, most of quartz sand enterprises have simple production process, original equipment, low yield, unstable product components and granularity, especially the magnetic separation process is too simple, the mechanization degree is not high, like wet production, the permanent magnetic strong magnet is mainly adopted for manual iron removal, and thus the grade and quality of quartz sand are difficult to guarantee. In addition, the over-crushed fine powder generated by wet production is more and can reach 20 percent at most, the waste of mineral resources is great, and the environmental pollution is serious. However, some quartz sand production enterprises adopt a flotation process to process and produce refined quartz sand, but the production scale is small and the yield is not high. The iron content of the quartz sand produced by the flotation method can be generally controlled within 60ppm, but the method has higher requirement on the granularity of the quartz sand (Huhongkun, Zhangming, building materials and decorations, 2016,000,006, 233-.
The problem is summarized as follows: at present, an optimized purification scheme aiming at a Fengyang quartz raw material, such as ore grinding granularity, optimized magnetic separation, flotation conditions and a further purification scheme, is lacked in production enterprises of Fengyang quartz sand so as to achieve the aim of preparing high-purity quartz and further improve the utilization efficiency and economic value of Fengyang high-quality quartz resources.
Disclosure of Invention
The technical problem of the invention is solved: the method overcomes the defects of the prior art, and provides a quartz raw material purification method, wherein a great part of muscovite and plagioclase in quartz sand is dissociated and removed, so that the optimized flotation and acid leaching conditions for purification of Fengyang quartz ore are obtained, and the w (SiO2) of the obtained high-purity quartz sand is up to 99.9% or more; through the research, the characteristics of the Fengyang quartz raw material are combined, and the practical production is combined, so that a theoretical suggestion is provided for the industrial purification process of local enterprises.
The invention is realized by the following technical scheme:
a method for purifying a quartz raw material is characterized by comprising the following steps:
(1) grinding: grinding the quartz rock ore to prepare quartz placer;
(2) magnetic separation and rough separation: roughing the quartz placer obtained in the step (1) by using a magnetic separator, and removing part of magnetic impurities to obtain magnetic separation roughed quartz placer;
(3) magnetic separation and fine selection: selecting the magnetic separation rough separation quartz placer by a magnetic separator, removing magnetic impurities, and obtaining the magnetic separation selected quartz placer;
(4) flotation and roughing: carrying out flotation on the magnetic separation and fine selection quartz sand ore obtained in the step (3) by using a flotation reagent to remove tailings; the flotation reagent comprises a collector and a pH regulator;
(5) flotation and fine selection: performing secondary flotation on the quartz placer obtained in the step (4) after the flotation and rough separation by using a flotation reagent, and removing tailings to obtain flotation and fine-selected quartz placer; the flotation reagent is a collecting agent;
(6) acid leaching: carrying out mixed acid normal-pressure acid leaching on the quartz placer obtained after flotation and concentration in the step (5) for 55-65 minutes, filtering the leached quartz placer, washing the quartz placer to be neutral by water, and drying to obtain final quartz concentrate; the mixed acid solution is a mixture of a sulfuric acid solution, a hydrochloric acid solution and a hydrofluoric acid solution; wherein the sulfuric acid solution: hydrochloric acid solution: the volume ratio of the hydrofluoric acid solution is 2: 2: 3, the mass concentration of the sulfuric acid solution is 28-32%, the mass concentration of the hydrochloric acid solution is 28-32%, the mass concentration of the hydrofluoric acid solution is 28-32%, and the liquid-solid ratio of the mixed acid solution to the quartz sand ore obtained after flotation and concentration in the step (5) is 3 ml/g; controlling the temperature of acid leaching to be 18-22 ℃.
Further, in the step (1), grinding until the fineness is-0.074 mm and accounts for 99.45-100%.
Further, in the step (2), the roughing magnetic field strength is 1.8T-2.0T.
Further, in the step (3), the selected magnetic field intensity is 2.2T-2.4T.
Further, in the step (4), the mass concentration of the ore pulp is 20%, the weight of the dry basis of the quartz sand ore subjected to magnetic separation and concentration is taken as a reference, and the addition amount of the collecting agent is 140-160 g.t-1
Further, in step (4), the pH of the flotation slurry is adjusted to 2-3.
Further, in the step (4), the collecting agent is dodecylamine; the pH regulator is sulfuric acid.
Further, in the step (5), the mass concentration of the ore pulp is 20%, the weight of the dry basis of the quartz sand ore subjected to magnetic separation and concentration is taken as a reference, and the addition amount of the collecting agent is 100-120 g.t-1
Compared with the existing quartz raw material purification method, the method has the characteristics and advantages that:
the quartz raw material selected in the research is a typical quartz raw material in Fengyang county, the research degree is not high, and the research result can provide theoretical guidance for the local actual industrial purification of Fengyang; by taking the samples of Fengyang county quartzite ores as an example, the optimal magnetic flotation and acid leaching conditions are determined, certain reference can be provided for enterprises in Fengyang county producing high-purity quartz at present, the utilization rate and the utilization value of Fengyang quartzite resources are improved, and the waste of quartzite resources is avoided.
Drawings
FIG. 1 is a flow chart of an experiment for purifying a quartz raw material according to the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and the embodiments. The following examples are only for explaining the present invention, the scope of the present invention shall include the full contents of the claims, and the full contents of the claims of the present invention can be fully realized by those skilled in the art through the following examples.
Referring to fig. 1, the method for purifying a quartz raw material according to the present embodiment includes:
(1) grinding: grinding the quartz rock ore until the fineness is-0.074 mm and the ground ore accounts for 99.45% -100%, and preparing quartz sand ore;
(2) magnetic separation and rough separation: roughing the quartz placer obtained in the step (1) by using a magnetic separator, wherein the magnetic field intensity of the roughing is 1.8T-2.0T, and removing partial magnetic impurities to obtain magnetic-separation roughing quartz placer;
(3) magnetic separation and fine selection: selecting the magnetic separation rough separation quartz placer by a magnetic separator, wherein the magnetic field intensity of the selected magnetic separator is 2.2T-2.4T, and removing magnetic impurities to obtain the magnetic separation selected quartz placer;
(4) flotation and roughing: and (4) carrying out flotation on the magnetic separation and fine selection quartz sand ore obtained in the step (3) by using a flotation reagent to remove tailings. The flotation reagent comprises a collector and a pH regulator. The pH of the flotation slurry is adjusted to 2-3. The ore pulp mass concentration is 20%, the weight of a dry basis of the quartz sand ore subjected to magnetic separation and concentration is taken as a reference, and the addition amount of the collecting agent is 140-160 g.t-1. The collecting agent is dodecylamine; the pH regulator is sulfuric acid.
(5) Flotation and fine selection: and (4) carrying out secondary flotation on the quartz placer obtained in the step (4) after the flotation and roughing by using a flotation reagent to remove tailings. Performing chemical analysis on the concentrate after flotation to obtain SiO2The grade reaches 99.26 percent primarily. The flotation reagent is a collector. The ore pulp mass concentration is 20%, the weight of a dry basis of the magnetic separation and concentration quartz sand ore is taken as a reference, and the addition amount of the collecting agent is 100-120 g.t-1. The collector is dodecylamine.
(6) Acid leaching: carrying out mixed acid normal-pressure acid leaching on the quartz placer obtained after flotation and selection in the step (5) for 55-65 minutes; and filtering the leached quartz placer, washing the quartz placer to be neutral by water, and drying the quartz placer to obtain the final quartz concentrate. The mixed acid solution is a mixture of a sulfuric acid solution, a hydrochloric acid solution and a hydrofluoric acid solution; wherein the sulfuric acid solution: hydrochloric acid solution: the volume ratio of the hydrofluoric acid solution is 2: 2: 3, the mass concentration of the sulfuric acid solution is 28-32%, the mass concentration of the hydrochloric acid solution is 28-32%, the mass concentration of the hydrofluoric acid solution is 28-32%, and the liquid-solid ratio of the mixed acid solution to the quartz sand ore obtained after flotation and concentration in the step (5) is 3 ml/g; controlling the temperature of acid leaching to be 18-22 ℃.
The final quartz concentrate is chemically analyzed to obtain SiO2The content reaches 99.90 percent. Most of magnetic impurities in the quartz sand can be removed through magnetic roughing and magnetic concentration, impurities (including magnetic and non-magnetic impurities) can be further removed through flotation roughing and flotation concentration, metal impurities can be further removed through acid leaching, and the purity of the quartz sand ore is improved.
In the flotation process, the collecting agent is dodecylamine which is an amine collecting agent for floating mica, and fine-grained muscovite mica can be effectively recovered in an acidic medium.
The equipment used in the following examples is shown in attached Table 1:
attached table 1 mineral processing equipment
Figure BDA0002935232240000051
Example 1
Taking a quartz rock sample (N117 degrees 26 '26 degrees, E32 degrees 45' 29 degrees) from Fengyang county, Chuzhou city, Anhui province as an example, the method for gradually purifying the quartz rock sample through the following experimental process to finally obtain the high-purity quartz w (SiO)2) Not less than 99.9% of the product standard. The sample collected sandstone forms sedimentary quartzite through metamorphism, sedimentation and the like, and the ore is in grey white, light purple and the like, and has medium and fine granular metamorphic structure and blocky structure.
(1) Grinding: the raw ore is ground by a CM-01 cone-shaped porcelain grinding machine for 40 minutes with the grinding concentration of 50 percent and the grinding fineness of-0.074 mm; controlling the fineness of the ground ore to be-0.074 mm and accounting for 99.45 percent;
(2) magnetic separation and rough separation: roughing the quartz sand obtained in the step (1) by adopting a wet-type strong magnetic separator (XCSQ-50 x 70, Wuhan prospecting mechanical factory), wherein the magnetic field intensity of roughing is 2.0T, and removing partial magnetic impurities to obtain magnetic separation roughing quartz sand ore;
(3) magnetic separation and fine selection: adopting a wet strong magnetic separator (XCSQ-50 x 70, Wuhan prospecting mechanical plant) to carry out concentration on the magnetic separation rough concentration quartz sand ore, carrying out concentration on the magnetic field intensity for 2.3T, and removing magnetic impurities to obtain magnetic separation concentrated quartz sand ore;
(4) flotation and roughing: the magnetic concentration quartz sand ore is added into a flotation machine (XFD-12, Jilin exploration mechanical plant). Adding sulfuric acid, adjusting the pH value of the slurry to 2.5, and then adding a collecting agent of dodecylamine. The mass concentration of the ore pulp is 20 percent, based on the dry basis weight of the quartz sand ore subjected to magnetic separation and concentration, and the adding amount of the dodecylamine is 160 g/t. Then, carrying out flotation in a flotation machine (XFD-12, Jilin exploration mechanical plant) for 5min to remove tailings;
(5) flotation and fine selection: subjecting the product obtained in step (4)The quartz sand after the rough flotation is added into a flotation machine (XFD-12, Jilin exploration mechanical plant). The collector dodecylamine was then added. The mass concentration of the ore pulp is 20 percent, based on the dry basis weight of the quartz sand ore subjected to magnetic separation and fine selection, the addition amount of the dodecylamine is 100g/t, then the ore pulp is subjected to flotation in a flotation machine (XFD-12, Jilin research mechanical plant), the flotation time is 5min, and tailings are removed. Performing chemical analysis (P61-XRF26s X-ray fluorescence spectrometer melting method rock primary and secondary quantity analysis) on the quartz sand ore obtained after flotation and concentration to obtain SiO2The grade reaches 99.26 percent primarily;
(6) acid leaching: placing the quartz placer obtained after flotation and selection in the step (5) into a container made of polyethylene, and carrying out acid leaching for 60 minutes in mixed acid liquid under normal pressure; and then, filtering the leached quartz placer, washing the quartz placer to be neutral by water, and drying the quartz placer to obtain the final quartz concentrate. The mixed acid solution is a mixture of a sulfuric acid solution, a hydrochloric acid solution and a hydrofluoric acid solution; wherein the sulfuric acid solution: hydrochloric acid solution: the volume ratio of the hydrofluoric acid solution is 2: 2: 3, the mass concentration of the sulfuric acid solution is 30%, the mass concentration of the hydrochloric acid solution is 30%, the mass concentration of the hydrofluoric acid solution is 30%, and the liquid-solid ratio of the mixed acid solution to the quartz placer obtained after flotation and selection in the step (5) is 3 ml/g; the temperature of the acid leaching was controlled at 20 ℃.
The final quartz concentrate was chemically analyzed (P61-XRF26s X-ray fluorescence spectrometer melting method rock primary and secondary quantity analysis) to obtain SiO2The content reaches 99.90 percent.
It should be noted that, according to the above embodiments of the present invention, those skilled in the art can fully implement the full scope of the present invention as defined by the independent claims and the dependent claims, and implement the processes and methods as the above embodiments; and the invention has not been described in detail so as not to obscure the present invention.
The above description is only a part of the embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (8)

1. A method for purifying a quartz raw material is characterized by comprising the following steps:
(1) grinding: grinding the quartz rock ore to prepare quartz placer;
(2) magnetic separation and rough separation: roughing the quartz placer obtained in the step (1) by using a magnetic separator, and removing part of magnetic impurities to obtain magnetic separation roughed quartz placer;
(3) magnetic separation and fine selection: selecting the magnetic separation rough separation quartz placer by a magnetic separator, removing magnetic impurities, and obtaining the magnetic separation selected quartz placer;
(4) flotation and roughing: carrying out flotation on the magnetic separation and fine selection quartz sand ore obtained in the step (3) by using a flotation reagent to remove tailings; the flotation reagent comprises a collector and a pH regulator;
(5) flotation and fine selection: performing secondary flotation on the quartz placer obtained in the step (4) after the flotation and rough separation by using a flotation reagent, and removing tailings to obtain flotation and fine-selected quartz placer; the flotation reagent is a collecting agent;
(6) acid leaching: carrying out mixed acid normal-pressure acid leaching on the quartz placer obtained after flotation and concentration in the step (5) for 55-65 minutes, filtering the leached quartz placer, washing the quartz placer to be neutral by water, and drying to obtain final quartz concentrate; the mixed acid solution is a mixture of a sulfuric acid solution, a hydrochloric acid solution and a hydrofluoric acid solution; wherein the sulfuric acid solution: hydrochloric acid solution: the volume ratio of the hydrofluoric acid solution is 2: 2: 3, the mass concentration of the sulfuric acid solution is 28-32%, the mass concentration of the hydrochloric acid solution is 28-32%, the mass concentration of the hydrofluoric acid solution is 28-32%, and the liquid-solid ratio of the mixed acid solution to the quartz sand ore obtained after flotation and concentration in the step (5) is 3 ml/g; controlling the temperature of acid leaching to be 18-22 ℃.
2. The method according to claim 1, wherein in the step (1), the ore is ground to a fineness of-0.074 mm in a range of 99.45% to 100%.
3. The method of claim 1, wherein in step (2), the rougher magnetic field strength is 1.8T to 2.0T.
4. The method of claim 1, wherein in step (3), the concentration magnetic field strength is between 2.2T and 2.4T.
5. The method according to claim 1, characterized in that in the step (4), the ore pulp has a mass concentration of 20%, and the addition amount of the collecting agent is 140-160 g-t based on the dry weight of the quartz sand ore subjected to magnetic separation and concentration-1
6. The method of claim 1, wherein in step (4), the pH of the flotation slurry is adjusted to 2-3.
7. The method of claim 1 wherein in step (4) the collector is dodecylamine; the pH regulator is sulfuric acid.
8. The method according to claim 1, characterized in that in the step (5), the ore pulp has a mass concentration of 20%, and the addition amount of the collecting agent is 100-120 g-t on the basis of the dry weight of the quartz sand ore subjected to magnetic separation and concentration-1
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114904639A (en) * 2022-05-15 2022-08-16 连云港福京石英制品有限公司 Combined quartz sand treatment equipment and method

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CN101254923A (en) * 2008-04-07 2008-09-03 安徽工业大学 Method for preparing high-purity ground quartz
CN106000621A (en) * 2016-06-01 2016-10-12 安徽晶晶石英科技有限公司 Method for purifying quartz sand by compounding chlorination with acid leaching
CN107185708A (en) * 2017-07-14 2017-09-22 长沙有色冶金设计研究院有限公司 A kind of method that high-purity quartz is prepared with mine tailing
CN109046747A (en) * 2018-08-10 2018-12-21 江苏凯达石英股份有限公司 The technique that composite algorithm prepares glass sand
CN109111101A (en) * 2018-11-01 2019-01-01 中钢集团马鞍山矿山研究院有限公司 A kind of purification by mineral method of glass sand
CN110127708A (en) * 2019-05-01 2019-08-16 黄冈师范学院 A kind of SiO2Purity >=99.99% glass sand method of purification
CN111377453A (en) * 2020-03-13 2020-07-07 新沂市磊晶石英材料有限公司 Purification process of superfine high-purity fused quartz powder
CN111874915A (en) * 2020-07-24 2020-11-03 武汉理工大学 Method for preparing high-purity quartz sand by taking vein quartz as raw material

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ATE160098T1 (en) * 1992-08-14 1997-11-15 Materias Primas Monterrey S A METHOD FOR CLEANING QUARTZ SAND AND OTHER MATERIALS
CN101254923A (en) * 2008-04-07 2008-09-03 安徽工业大学 Method for preparing high-purity ground quartz
CN106000621A (en) * 2016-06-01 2016-10-12 安徽晶晶石英科技有限公司 Method for purifying quartz sand by compounding chlorination with acid leaching
CN107185708A (en) * 2017-07-14 2017-09-22 长沙有色冶金设计研究院有限公司 A kind of method that high-purity quartz is prepared with mine tailing
CN109046747A (en) * 2018-08-10 2018-12-21 江苏凯达石英股份有限公司 The technique that composite algorithm prepares glass sand
CN109111101A (en) * 2018-11-01 2019-01-01 中钢集团马鞍山矿山研究院有限公司 A kind of purification by mineral method of glass sand
CN110127708A (en) * 2019-05-01 2019-08-16 黄冈师范学院 A kind of SiO2Purity >=99.99% glass sand method of purification
CN111377453A (en) * 2020-03-13 2020-07-07 新沂市磊晶石英材料有限公司 Purification process of superfine high-purity fused quartz powder
CN111874915A (en) * 2020-07-24 2020-11-03 武汉理工大学 Method for preparing high-purity quartz sand by taking vein quartz as raw material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114904639A (en) * 2022-05-15 2022-08-16 连云港福京石英制品有限公司 Combined quartz sand treatment equipment and method
CN114904639B (en) * 2022-05-15 2023-10-13 连云港福京石英制品有限公司 Combined quartz sand treatment equipment and method

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Application publication date: 20210608