CN114620733B - Low-carbon green SiO of superconducting high-strength magnetic coupling quartz ore 2 Fine purification method - Google Patents
Low-carbon green SiO of superconducting high-strength magnetic coupling quartz ore 2 Fine purification method Download PDFInfo
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION 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
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
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- B03C1/0335—Component parts; Auxiliary operations characterised by the magnetic circuit using coils
- B03C1/0337—Component parts; Auxiliary operations characterised by the magnetic circuit using coils superconductive
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Abstract
The invention provides a superconducting high-strength magnetic coupling stoneEnglish ore low-carbon green SiO 2 A fine purification method, which belongs to the high-purity SiO 2 The extraction technical field. The method comprises mixing quartz ore (SiO 2 More than or equal to 90 percent) is dried, crushed and ground to have particle size of 325 to 425 meshes, and quartz raw mineral powder is obtained; then SiO is carried out on Dan Yingyuan mineral powder by utilizing superconducting high gradient magnetic separation equipment 2 The separation and the extraction of the fine particles of weak magnetic substances such as ferric oxide, aluminum oxide and the like are realized, and more than 99 percent of SiO is obtained 2 Coarse fine powder; finally, preparing high-purity SiO by adopting a multistage acid leaching fine purification technology under ultrasonic assistance 2 Thereby realizing high purity SiO 2 High added value recycling of (3). The invention is low-carbon green high-purity SiO 2 The purification process flow is short, the product quality is high, the operation cost is low, the superconductivity is low, and no waste water or waste gas is discharged in the process; siO purified by the process 2 The product grade is stable and is more than or equal to 99.95 percent (up to 99.99 percent), and the high purity SiO is achieved 2 Is a standard of (2).
Description
Technical Field
The invention relates to high purity SiO 2 The extraction technical field, in particular to a low-carbon green SiO of a superconducting high-strength magnetic coupling quartz ore 2 A fine purification method.
Background
Quartz is a silicate mineral with hardness, wear resistance and stable chemical property, and has wide application field. At present, the common quartz ore is mainly applied to the fields of quartz crucible, building industry, quartz glass manufacturing, ceramic industry, foundry industry and the like, and the high-purity quartz has unique physical and chemical characteristics, so that the high-purity quartz plays an increasingly important role in a plurality of high-tech products. The high-purity quartz is mainly applied to high and new technical industries such as electronic electricians, optical fiber communication, aerospace, military industry and the like, and has very important strategic positions. The high-purity quartz has strict requirements on the content of silicon dioxide and the limit of metal elements such as iron, aluminum and the like, so that the method has very important significance in actively exploring the quartz ore purification processing technology in order to meet the requirements of high-quality quartz products. At present, natural quartz ore is mainly purified by processes of color selection, calcination, water quenching, floatation, magnetic separation, acid washing and the like. The production process is complex, the energy consumption is high, the quartz purity is low, and the application requirement is difficult to meet. Therefore, a simple and efficient high-purity quartz extraction means is the key point of current research.
Disclosure of Invention
The invention aims to solve the technical problem of providing a low-carbon green SiO of a superconducting high-strength magnetic coupling quartz ore 2 The fine purification method has the advantages of simple processing flow, low production cost and high product quality; siO in quartz ore treated by the process 2 The content of the silica sand reaches more than 99.95 percent and reaches the standard of high-purity silica sand.
The method comprises the following steps:
s1: drying quartz ore, crushing and fine grinding;
s2: siO using super-conductive high gradient magnetic separation technology 2 Is separated and extracted;
s3: preparation of high-purity SiO by multistage acid leaching fine purification technology under assistance of ultrasound 2 。
Wherein, siO in quartz ore in S1 2 The content of (2) is more than 90 percent, and the particles are finely ground to the particle size of 325 to 425 meshes.
In S2, the superconducting high-gradient magnetic separation has magnetic field strength of 2-5T, steel wool volume filling rate of 3-15%, pulp dispersing agent accounting for 1-15% of the mass of quartz mineral powder, and pulp concentration of 10-120 kg/m 3 The flow rate of ore pulp is 0.1-1.5 m/s.
The steel wool is uniformly wound on a steel mesh or pressed into sheets to be arranged in the separator at equal intervals, and the interval is 2-10 nm.
The ore pulp dispersing agent is one or a mixture of more of sodium hexametaphosphate, washing powder, sodium tripolyphosphate, sodium pyrophosphate, sodium thiophosphate and sodium carbonate.
S2, performing superconducting high-gradient magnetic separation on the obtained SiO 2 Washing the coarse and fine powder with deionized water to neutrality, and removing SiO 2 Dispersing agent remained on the surface of the coarse and fine powder.
S3 specifically comprises the following steps:
magnetically separating S2 to obtain SiO 2 Carrying out one-stage normal-pressure stirring acid leaching on the coarse refined powder for 4-12 hours under the assistance of ultrasonic waves, filtering, and washing with deionized water to be neutral; then carrying out 2-4 sections of acid leaching under the same ultrasonic and normal pressure stirring conditions; finally, the leached SiO is treated 2 Filtering, washing with deionized water to neutrality, and oven drying to obtain high purity SiO with content up to 99.95% (up to 99.99%) 2 。
The ultrasonic power is 400-4000W.
The acid leaching liquid is one or more mixed acids selected from sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid, nitric acid and citric acid; the temperature of the acid leaching is 30-80 ℃; the stirring speed is 200-250 r/min.
SiO obtained by acid leaching liquid and S2 magnetic separation 2 The liquid-solid ratio (mL/g) of the coarse and fine powder is 3-10:1.
The technical scheme of the invention has the following beneficial effects:
(1) The extraction process of the high-purity quartz has simple processing flow, low production cost and high product quality, and can extract high-purity SiO with the content of more than 99.95 percent 2 And (5) a product.
(2) The superconducting magnetic separation energy consumption is 1/10 of the conventional magnetic separation energy consumption, has the advantages of high efficiency, small occupied area, high efficiency, energy conservation, no secondary pollution, and the like, is favorable for forming a green and high-efficiency resource high-added-value utilization system, optimizes an industrial structure, promotes industrial development, and brings great economic benefit and ecological environmental benefit for enterprises.
(3) For SiO 2 The residual part after extraction can extend the industrial chain, and can also be used for producing building and paving materials such as microcrystalline glass, light heat-insulating flame-retardant foam bricks, water permeable bricks and the likeRealizing the best use of the whole industry.
Drawings
FIG. 1 shows a low-carbon green SiO of a superconducting high-strength magnetic coupling quartz ore according to the present invention 2 A technical scheme of a method for fine purification.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
The invention provides a low-carbon green SiO of a superconducting high-strength magnetic coupling quartz ore 2 A fine purification method.
As shown in fig. 1, the method comprises the steps of:
s1: drying quartz ore, crushing and fine grinding;
s2: siO using super-conductive high gradient magnetic separation technology 2 Is separated and extracted;
s3: preparation of high-purity SiO by multistage acid leaching fine purification technology under assistance of ultrasound 2 。
The following describes specific embodiments.
The superconducting high-strength magnetic coupling refined SiO of the embodiment 2 Comprises the following steps:
step 1: drying quartz ore, crushing and grinding the quartz ore to have particle size of 325-425 meshes to obtain quartz raw ore powder; wherein SiO in the quartz raw ore 2 The content of (2) is more than 90%.
Step 2: siO using super-conductive high gradient magnetic separation technology 2 Is separated and extracted;
the magnetic field strength is 2-5T, the volume filling rate of steel wool is 3-15%, one or more of sodium hexametaphosphate, washing powder, sodium tripolyphosphate, sodium pyrophosphate, sodium thiophosphate and sodium carbonate accounts for 1-15% of the quartz mineral powder, and the concentration of ore pulp is 10-120 kg/m 3 Superconducting magnetic separation is carried out under the condition that the flow velocity of ore pulp is 0.1-1.5 m/s, so that high-efficiency removal of fine particle weak magnetic substances such as ferric oxide, aluminum oxide and the like is realized, and more than 99% of SiO is obtained 2 Coarse fine powder; the steel wool is uniformly wound on a steel net or pressed into sheet-like objects at equal intervals (2 to the whole10 nm) are arranged in the separator, thereby increasing the adsorption area of the steel wool surface and the weakly magnetic substance.
Step 3: magnetically separating S2 to obtain SiO 2 Washing the coarse and fine powder with deionized water to neutrality, and removing residual SiO 2 Dispersing agent on the surface of coarse and fine powder. At the ultrasonic power of 400-4000W, the stirring speed of 200-250 r/min, the acid leaching temperature of 30-80 ℃, one or more mixed acids of sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid, nitric acid and citric acid and the SiO obtained after the magnetic separation and concentration in the step S2 2 Carrying out one-stage normal-pressure stirring acid leaching for 4-12 h under the condition that the liquid-solid ratio (mL/g) of the coarse and fine powder is 3-10:1, filtering, and washing with deionized water to be neutral; then 2-4 sections of acid leaching is carried out under the same condition; finally, the leached SiO is treated 2 Filtering, washing with deionized water to neutrality, and oven drying to obtain high purity SiO 2 And (5) a product.
Wherein, the sulfuric acid concentration is (4-12) mol/L, the hydrochloric acid concentration is (5-10) mol/L, the acetic acid concentration is (4-14) mol/L, the phosphoric acid concentration is (6-12) mol/L, the nitric acid concentration is (3-8) mol/L, and the citric acid concentration is (8-12) mol/L.
Finally obtained high purity SiO 2 SiO was measured by chemical analysis 2 The content reaches more than 99.95 percent.
The specific implementation process is as follows:
examples 1 to 7
Drying quartz ore, and crushing the quartz ore to 325 meshes to obtain quartz ore powder; wherein SiO in quartz ore 2 The content of (2) was 95%.
The magnetic field strength is 2T, the volume filling rate of steel wool is 15%, the ratio of sodium hexametaphosphate, washing powder, sodium tripolyphosphate, sodium pyrophosphate, sodium thiophosphate, sodium carbonate and the mixture (the mass ratio of sodium hexametaphosphate to washing powder is 1:1) is 4 per mill, 3 per mill, 6 per mill, 5 per mill, 7 per mill, 8 per mill and 1 per mill of the quartz mineral powder respectively, and the concentration of ore pulp is 10kg/m 3 Superconducting magnetic separation is carried out under the condition that the flow velocity of ore pulp is 1m/s, so that high-efficiency removal of fine particle weakly magnetic substances such as ferric oxide, aluminum oxide and the like is realized, and the obtained SiO is obtained 2 The content of coarse and fine powder is 99.23%, 99.53%, 99.13%, 99.17%, 99.34%, 99.04%, 99.56%, respectivelyThe method comprises the steps of carrying out a first treatment on the surface of the The steel wool is uniformly wound on the steel mesh and is arranged in the separator at equal intervals (2 nm), so that the adsorption area of the surface of the steel wool and the weak magnetic substance is increased.
Magnetically separating the obtained SiO 2 Washing the coarse and fine powder with deionized water to neutrality, and removing residual SiO 2 Dispersing agent on the surface of coarse and fine powder. At the ultrasonic power of 4000W, the stirring speed of 220r/min, the acid leaching temperature of 80 ℃,4mol/L sulfuric acid solution and S2 are magnetically separated and carefully selected to obtain the SiO 2 Carrying out one-stage normal-pressure stirring acid leaching for 12 hours under the condition that the liquid-solid ratio (mL/g) of the coarse and fine powder is 10:1, filtering, and washing with deionized water to be neutral; then carrying out two-stage normal-pressure stirring acid leaching for 12h under the same condition; finally, the leached SiO is treated 2 Filtering, washing with deionized water to neutrality, and oven drying to obtain high purity SiO 2 And (5) a product.
Finally obtained high purity SiO 2 SiO was measured by chemical analysis 2 The contents respectively reach 99.985%, 99.989%, 99.969%, 99.977%, 99.986%, 99.957% and 99.993%.
Examples 8 to 14
Drying quartz ore, and crushing the quartz ore to 400 meshes to obtain quartz ore powder; wherein SiO in quartz ore 2 The content of (2) was 90%.
At a magnetic field strength of 5T, a steel wool volume filling rate of 3%, a sodium hexametaphosphate ratio of 4 per mill of the quartz mineral powder, and a mineral slurry concentration of 40kg/m 3 Superconducting magnetic separation is carried out under the condition that the flow velocity of ore pulp is 0.1m/s, so that high-efficiency removal of fine-particle weakly magnetic substances such as ferric oxide, aluminum oxide and the like is realized, and the obtained SiO is obtained 2 The content of the coarse refined powder is 99.34%; the steel wool pressed into sheets are arranged in the separator at equal intervals (10 nm), so that the adsorption area of the surface of the steel wool and the weak magnetic substance is increased.
Magnetically separating the obtained SiO 2 Washing the coarse and fine powder with deionized water to neutrality, and removing residual SiO 2 Dispersing agent on the surface of coarse and fine powder. At an ultrasonic power of 400W, a stirring speed of 200r/min and an acid leaching temperature of 60 ℃, the pickle liquor was treated with 5mol/L sulfuric acid, 6mol/L hydrochloric acid, 10mol/L acetic acid, 6mol/L phosphoric acid, 3mol/L nitric acid, 8mol/L citric acid, and mixed acid (V (4 mol/L)V (5 mol/L hydrochloric acid solution) =1:2) and S2, and magnetically separating and concentrating the obtained SiO 2 Carrying out one-stage normal-pressure stirring acid leaching for 8 hours under the condition that the liquid-solid ratio (mL/g) of the coarse and fine powder is 3:1, filtering, and washing with deionized water to be neutral; then three-stage normal pressure stirring acid leaching is carried out for 8 hours under the same condition; finally, the leached SiO is treated 2 Filtering, washing with deionized water to neutrality, and oven drying to obtain high purity SiO 2 And (5) a product.
Finally obtained high purity SiO 2 SiO was measured by chemical analysis 2 The contents respectively reach 99.951%, 99.973%, 99.985%, 99.966%, 99.969%, 99.984% and 99.992%.
Example 15
Drying quartz ore, and crushing the quartz ore to obtain quartz ore powder with a particle size of 425 meshes; wherein SiO in quartz ore 2 The content of (2) was 98.5%.
At the magnetic field strength of 4T, the volume filling rate of steel wool of 8 percent, the sodium hexametaphosphate accounts for 4 per mill of the quartz mineral powder, and the pulp concentration is 80kg/m 3 Superconducting magnetic separation is carried out under the condition that the flow velocity of ore pulp is 1.5m/s, so that high-efficiency removal of fine-particle weakly magnetic substances such as ferric oxide, aluminum oxide and the like is realized, and the obtained SiO is obtained 2 The content of coarse and fine powder is 99.21 percent respectively; the steel wool pressed into sheets are arranged in the separator at equal intervals (5 nm), so that the adsorption area of the surface of the steel wool and the weak magnetic substance is increased.
SiO is made of 2 Washing the coarse and fine powder with deionized water to neutrality, and removing residual SiO 2 Dispersing agent on the surface of coarse and fine powder. At an ultrasonic power of 2000W, a stirring speed of 250r/min, an acid leaching temperature of 80 ℃, a mixed acid (V (4 mol/L acetic acid): V (6 mol/L hydrochloric acid solution): V (3 mol/L nitric acid solution) =6:3:1) and SiO obtained after magnetic separation and concentration 2 The liquid-solid ratio (mL/g) of the coarse and fine powder is 6:1, carrying out one-stage normal-pressure stirring acid leaching for 4 hours, filtering, and washing with deionized water to be neutral; then four-stage acid leaching is carried out under the same condition, and stirring and acid leaching are carried out for 4 hours at normal pressure; finally, the leached SiO is treated 2 Filtering, washing with deionized water to neutrality, and oven drying to obtain high purity SiO 2 And (5) a product.
Finally obtained high purity SiO 2 Through chemical separationAnalysis of SiO 2 The content reaches 99.989 percent respectively.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (7)
1. Low-carbon green SiO of superconducting high-strength magnetic coupling quartz ore 2 The fine purification method is characterized by comprising the following steps:
s1: drying and crushing quartz ore, finely grinding the quartz ore to the particle size of 325-425 meshes;
s2: siO using super-conductive high gradient magnetic separation technology 2 Is separated and extracted;
s3: preparation of high-purity SiO by multistage acid leaching fine purification technology under assistance of ultrasound 2 ；
In S2, the superconducting high-gradient magnetic separation is carried out, the magnetic field intensity is 2-5T, the steel wool volume filling rate is 3-15%, the ore pulp dispersing agent accounts for 1-15% of the mass of the quartz mineral powder, and the ore pulp concentration is 10-120 kg/m 3 The flow rate of ore pulp is 0.1-1.5 m/s;
the step S3 is specifically as follows:
magnetically separating S2 to obtain SiO 2 Carrying out one-stage normal-pressure stirring acid leaching on the coarse refined powder for 4-12 hours under the assistance of ultrasound, filtering, and washing with deionized water to be neutral; then carrying out 2-4 sections of acid leaching under the same ultrasonic and normal pressure stirring conditions; finally, the leached SiO is treated 2 Filtering, washing with deionized water to neutrality, and oven drying to obtain high purity SiO with content of above 99.95% 2 ；
The pickle liquor is one or more mixed acids of sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid, nitric acid and citric acid;
SiO obtained by magnetic separation of the pickle liquor and S2 2 The liquid-solid ratio of the coarse powder is 3-10:1 mL/g.
2. The superconducting high-strength magnetic coupling quartz ore low-carbon green SiO according to claim 1 2 A fine purification method is characterized in that the SiO in the quartz ore in S1 is 2 The content of (2) is more than 90%.
3. The superconducting high-strength magnetic coupling quartz ore low-carbon green SiO according to claim 1 2 The fine purification method is characterized in that the steel wool is uniformly wound on a steel mesh or pressed into sheets to be arranged in a separator at equal intervals, and the interval is 2-10 nm.
4. The superconducting high-strength magnetic coupling quartz ore low-carbon green SiO according to claim 1 2 The fine purification method is characterized in that the ore pulp dispersing agent is one or a mixture of more of sodium hexametaphosphate, washing powder, sodium tripolyphosphate, sodium pyrophosphate, sodium thiophosphate and sodium carbonate.
5. The superconducting high-strength magnetic coupling quartz ore low-carbon green SiO according to claim 1 2 The fine purification method is characterized in that the SiO obtained after the superconducting high gradient magnetic separation in S2 2 Washing the coarse and fine powder with deionized water to neutrality, and removing SiO 2 Dispersing agent remained on the surface of the coarse and fine powder.
6. The superconducting high-strength magnetic coupling quartz ore low-carbon green SiO according to claim 1 2 The fine purification method is characterized in that the ultrasonic power is 400-4000W.
7. The superconducting high-strength magnetic coupling quartz ore low-carbon green SiO according to claim 1 2 The fine purification method is characterized in that the temperature of the acid leaching is 30-80 ℃; the stirring speed is 200-250 r/min.
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