CN111573680A - Method for removing iron in quartz sand - Google Patents

Method for removing iron in quartz sand Download PDF

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Publication number
CN111573680A
CN111573680A CN202010430825.2A CN202010430825A CN111573680A CN 111573680 A CN111573680 A CN 111573680A CN 202010430825 A CN202010430825 A CN 202010430825A CN 111573680 A CN111573680 A CN 111573680A
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China
Prior art keywords
acid solution
quartz sand
reaction kettle
solid phase
oxalic acid
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Pending
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CN202010430825.2A
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Chinese (zh)
Inventor
张雪梅
汪徐春
程年寿
管成龙
徐鑫强
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Anhui University of Science and Technology
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Anhui University of Science and Technology
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Priority to CN202010430825.2A priority Critical patent/CN111573680A/en
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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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

A method for removing iron in quartz sand comprises the following steps: taking 1t of quartz sand to be treated and a reaction kettle, injecting 200kg of oxalic acid solution into the reaction kettle from the bottom of the reaction kettle by a pump, wherein the mass fraction of the oxalic acid solution is 20%, heating to 60-80 ℃, keeping the temperature for acid leaching for 4-8h, and stirring in the acid leaching process; adding an ethylene diamine tetraacetic acid solution with the concentration of 0.02mol/L into a reaction kettle after acid leaching, keeping the temperature for reaction for 1-2h, and then performing suction filtration to retain a solid phase, wherein the volume ratio of the dosage of the ethylene diamine tetraacetic acid solution to the dosage of the oxalic acid solution is 1: 25-30; and adding water into the obtained solid phase for washing, wherein the amount of the added water is 200kg, stirring for 3-5min, performing suction filtration to retain the solid phase, and repeatedly washing for 3-4 times to obtain the target product.

Description

Method for removing iron in quartz sand
Technical Field
The invention relates to a method for removing iron in quartz sand.
Background
The quartz sand is a non-metal mining industrial raw material, and the reserve volume is very rich. The quartz sand in China is also rich in resources and excellent in quality, and the iron content is about 150ug-1At present, in the face of the development and scientific innovation of the new and advanced economy, the application of the quartz sand is not limited in the traditional field any more, and more relates to the high and new technology industryIn the following description. The fields have higher requirements on the quality of quartz sand raw materials, and SiO2The content is required to be more than 99.9 percent, and the iron content is less than 100ug-1In the process, the quartz sand can be used as high-purity quartz sand for raw materials of ultra-white glass, integrated circuits, communication optical fibers and the like. At present, the iron removal method of the quartz sand comprises the following steps: the method comprises the steps of pickling, magnetic separation, flotation, heavy medium ore dressing, ultrasonic method and the like, wherein the iron removal efficiency of quartz sand by the ultrasonic method is 46 percent and can reach 70 percent at most, but the requirement on equipment is too high and is harmful to human bodies.
Disclosure of Invention
The invention aims to solve the technical problem of providing the method for removing the iron in the quartz sand, and compared with methods such as magnetic separation, flotation, dense medium mineral separation, ultrasonic method and the like, the method has the advantages of higher purification efficiency and environmental friendliness.
In order to solve the technical problem, the invention provides a method for removing iron in quartz sand, which comprises the following steps:
(1) taking 1t of quartz sand to be treated and a reaction kettle, injecting 200kg of oxalic acid solution into the reaction kettle from the bottom of the reaction kettle by a pump, wherein the mass fraction of the oxalic acid solution is 20%, heating to 80 ℃, keeping the temperature for acid leaching for 4-8h, and stirring in the acid leaching process;
(2) adding an ethylene diamine tetraacetic acid solution with the concentration of 0.02mol/L into a reaction kettle after acid leaching, keeping the temperature for reaction for 1-2h, and then performing suction filtration to retain a solid phase, wherein the volume ratio of the dosage of the ethylene diamine tetraacetic acid solution to the dosage of the oxalic acid solution is 1: 25;
(3) and (3) adding water into the solid phase obtained in the step (2) for washing, wherein the amount of the added water is 200kg, stirring for 3-5min, performing suction filtration to retain the solid phase, and repeatedly washing for 3-4 times to obtain the target product.
For the sake of simplicity of explanation, the method for removing iron from silica sand according to the present invention is hereinafter simply referred to as the present method.
The method has the advantages that: the method adopts oxalic acid as a leaching agent, reacts with iron or ferric oxide to generate ferrous ions or ferric ions, adopts disodium ethylene diamine tetraacetate as a complexing agent to coordinate with the iron ions to generate a complex with very good water solubility, separates the complex from quartz sand, and chemically purifies the quartz sand.
In order to achieve better effect of the method, the preferred scheme is as follows:
preferably, sodium hydroxide solution is added to the reaction vessel after acid leaching to adjust the pH to 3.
According to the control variable experiment result curve, the iron removal efficiency is the optimal value when the pH value is 3, and the oxalic acid molecule coordination and complexation capability is sharply reduced when the pH value of the solution is increased after the pH value exceeds 3.
Drawings
FIG. 1 is an electron micrograph (. times.100) of a quartz sand raw material before treatment in example four.
FIG. 2 is an electron micrograph (. times.100) of a raw material of quartz sand used in example four.
FIG. 3 is an electron micrograph (. times.300) of the raw quartz sand of example four before treatment.
FIG. 4 is an electron micrograph (. times.300) of a raw material of quartz sand used in example four.
Detailed Description
The first embodiment is as follows:
a method for removing iron in quartz sand comprises the following steps:
(1) taking 1t of quartz sand to be treated and a reaction kettle, injecting 200kg of oxalic acid solution into the reaction kettle from the bottom of the reaction kettle by a pump, wherein the mass fraction of the oxalic acid solution is 20%, heating to 80 ℃, keeping the temperature for acid leaching for 4 hours, and stirring in the acid leaching process;
(2) adding an ethylene diamine tetraacetic acid solution with the concentration of 0.02mol/L into a reaction kettle after acid leaching, keeping the temperature for reaction for 1 hour, and then performing suction filtration to retain a solid phase, wherein the volume ratio of the dosage of the ethylene diamine tetraacetic acid solution to the dosage of the oxalic acid solution is 1: 25;
(3) and (3) adding water into the solid phase obtained in the step (2) for washing, wherein the amount of the added water is 200kg, stirring for 3min, carrying out suction filtration to retain the solid phase, and repeatedly washing for 3 times to obtain the target product.
Example two:
a method for removing iron in quartz sand comprises the following steps:
(1) taking 1t of quartz sand to be treated and a reaction kettle, injecting 200kg of oxalic acid solution into the reaction kettle from the bottom of the reaction kettle by a pump, wherein the mass fraction of the oxalic acid solution is 20%, heating to 70 ℃, keeping the temperature for acid leaching for 6 hours, and stirring in the acid leaching process;
(2) adding an ethylene diamine tetraacetic acid solution with the concentration of 0.02mol/L into a reaction kettle after acid leaching, keeping the temperature for reaction for 1-2h, and then performing suction filtration to retain a solid phase, wherein the volume ratio of the dosage of the ethylene diamine tetraacetic acid solution to the dosage of the oxalic acid solution is 1: 28;
(3) and (3) adding water into the solid phase obtained in the step (2) for washing, wherein the amount of the added water is 200kg, stirring for 4min, carrying out suction filtration to retain the solid phase, and repeatedly washing for 4 times to obtain the target product.
Example three:
a method for removing iron in quartz sand comprises the following steps:
(1) taking 1t of quartz sand to be treated and a reaction kettle, injecting 200kg of oxalic acid solution into the reaction kettle from the bottom of the reaction kettle by a pump, wherein the mass fraction of the oxalic acid solution is 20%, heating to 80 ℃, keeping the temperature for acid leaching for 8 hours, and stirring in the acid leaching process;
(2) adding an ethylene diamine tetraacetic acid solution with the concentration of 0.02mol/L into a reaction kettle after acid leaching, keeping the temperature for reaction for 2 hours, and then performing suction filtration to retain a solid phase, wherein the volume ratio of the dosage of the ethylene diamine tetraacetic acid solution to the dosage of the oxalic acid solution is 1: 25;
(3) and (3) adding water into the solid phase obtained in the step (2) for washing, wherein the amount of the added water is 200kg, stirring for 5min, carrying out suction filtration to retain the solid phase, and repeatedly washing for 4 times to obtain the target product.
Example four:
a method for removing iron in quartz sand comprises the following steps:
(1) taking 1t of quartz sand to be treated and a reaction kettle, injecting 200kg of oxalic acid solution into the reaction kettle from the bottom of the reaction kettle by a pump, wherein the mass fraction of the oxalic acid solution is 20%, heating to 80 ℃, keeping the temperature for acid leaching for 8 hours, and stirring in the acid leaching process;
(2) adding a sodium hydroxide solution into a reaction kettle after acid leaching to adjust the pH value to 3, then adding an ethylene diamine tetraacetic acid solution with the concentration of 0.02mol/L to keep the temperature for reaction for 2 hours, and then performing suction filtration to retain a solid phase, wherein the volume ratio of the amount of the ethylene diamine tetraacetic acid solution to the amount of the oxalic acid solution is 1: 25;
(3) and (3) adding water into the solid phase obtained in the step (2) for washing, wherein the amount of the added water is 200kg, stirring for 5min, carrying out suction filtration to retain the solid phase, and repeatedly washing for 3 times to obtain the target product.
The quartz sand used in the above examples was from the Fengyang quartz sand mine area.
For the quartz sand treated by the method in the fourth embodiment, the removal rate of iron is up to 72.8% through detection, and observation by an electron microscope shows that the surface of the quartz sand particles before treatment is uneven, and has some very small covering substances, and the surface of the treated quartz sand is smooth and flat. Scanning electron micrographs are shown in FIGS. 1-4. Therefore, 1, the iron covering the surface of the quartz sand is completely reacted; 2. the quartz sand rubs against each other during stirring, resulting in a smoother surface than before.

Claims (2)

1. A method for removing iron in quartz sand is characterized by comprising the following steps:
(1) taking 1t of quartz sand to be treated and a reaction kettle, injecting 200kg of oxalic acid solution into the reaction kettle from the bottom of the reaction kettle by a pump, wherein the mass fraction of the oxalic acid solution is 20%, heating to 60-80 ℃, keeping the temperature for acid leaching for 4-8h, and stirring in the acid leaching process;
(2) adding an ethylene diamine tetraacetic acid solution with the concentration of 0.02mol/L into a reaction kettle after acid leaching, keeping the temperature for reaction for 1-2h, and then performing suction filtration to retain a solid phase, wherein the volume ratio of the dosage of the ethylene diamine tetraacetic acid solution to the dosage of the oxalic acid solution is 1: 25-30;
(3) and (3) adding water into the solid phase obtained in the step (2) for washing, wherein the amount of the added water is 200kg, stirring for 3-5min, performing suction filtration to retain the solid phase, and repeatedly washing for 3-4 times to obtain the target product.
2. The method for removing iron from quartz sand according to claim 1, wherein: adding sodium hydroxide solution into the reaction kettle after acid leaching to adjust the pH value to 3.
CN202010430825.2A 2020-05-20 2020-05-20 Method for removing iron in quartz sand Pending CN111573680A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113546907A (en) * 2021-07-28 2021-10-26 韩忠君 Non-acidic pollution-free stone cleaning method

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CN113546907A (en) * 2021-07-28 2021-10-26 韩忠君 Non-acidic pollution-free stone cleaning method

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