CN114620733A - Superconductive high-strength magnetic coupling quartz ore low-carbon green SiO2Method for fine purification - Google Patents
Superconductive high-strength magnetic coupling quartz ore low-carbon green SiO2Method for fine purification Download PDFInfo
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- CN114620733A CN114620733A CN202210227922.0A CN202210227922A CN114620733A CN 114620733 A CN114620733 A CN 114620733A CN 202210227922 A CN202210227922 A CN 202210227922A CN 114620733 A CN114620733 A CN 114620733A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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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
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/025—High gradient magnetic separators
- B03C1/031—Component parts; Auxiliary operations
- B03C1/033—Component parts; Auxiliary operations characterised by the magnetic circuit
- 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 low-carbon green SiO superconducting high-strength magnetic coupling quartz ore2A fine purification method, belongs to high-purity SiO2The technical field of extraction. The method comprises mixing quartz ore (SiO)2Not less than 90 percent), drying, crushing and grinding to 325-425 meshes to obtain quartz raw ore powder; then, SiO is carried out on the quartz raw ore powder by utilizing superconducting high-gradient magnetic separation equipment2The separation and extraction of the method realizes the high-efficiency removal of iron oxide, aluminum oxide and other fine-particle weak magnetic substances to obtain more than 99 percent of SiO2Coarse refined powder; finally, preparing high-purity SiO by adopting a multi-stage acid leaching refining purification technology under the assistance of ultrasound2Thereby realizing high purity SiO2High value-added recycling. The low-carbon green high-purity SiO of the invention2The purification process flow is short, the product quality is high, the operation cost is low, the superconductivity is low, the energy consumption is low, and no wastewater or waste gas is discharged in the process; SiO purified by the process2Grade of productStable more than or equal to 99.95 percent (up to 99.99 percent) and reaches high-purity SiO2Of (3) is calculated.
Description
Technical Field
The invention relates to high-purity SiO2The technical field of extraction, in particular to low-carbon green SiO of superconducting high-strength magnetic coupling quartz ore2A fine purification method.
Background
Quartz is a silicate mineral with hardness, wear resistance and stable chemical properties, and has wide application fields. At present, common quartz ore is mainly applied to the fields of quartz crucible, building industry, quartz glass manufacturing, ceramic industry, casting industry and the like, and high-purity quartz has unique physical and chemical properties, so that the high-purity quartz plays an increasingly important role in many high-tech products. The high-purity quartz is mainly applied to high and new technology industries such as electronics and electricians, optical fiber communication, aerospace, war industry and the like, and has a very important strategic position. The high-purity quartz has strict requirements on the content of silicon dioxide and the limited amount of metal elements such as iron, aluminum and the like, so that the active exploration of a quartz ore purification processing technology has very important significance in order to meet the requirements of high-quality quartz products. At present, natural quartz ore is mainly purified by processes such as color separation, calcination, water quenching, flotation, magnetic separation, acid washing and the like. The production flow is complex, the energy consumption is high, and the purity of the quartz is not high, so that the application requirements are difficult to meet. Therefore, simple and efficient high-purity quartz extraction means are the focus of current research.
Disclosure of Invention
The invention aims to solve the technical problem of providing a low-carbon green SiO superconducting high-strength magnetic coupling quartz ore2The method for fine purification has simple processing flow, low production cost and high product quality; SiO in quartz ore treated by the process2The content of the sodium hydroxide reaches over 99.95 percent, and high purity is achievedStandard for quartz sand.
The method comprises the following steps:
s1: drying, crushing and finely grinding quartz ore;
s2: SiO by using superconductive high-gradient magnetic separation technology2Separation and extraction;
s3: preparation of high-purity SiO by multi-stage acid leaching refining purification technology under assistance of ultrasound2。
Wherein, SiO in quartz ore in S12The content of (A) is more than 90%, and the mixture is finely ground to a particle size of 325-425 meshes.
In S2, during superconducting high-gradient magnetic separation, the magnetic field intensity is 2-5T, the volume filling rate of steel wool is 3-15%, the ore pulp dispersing agent accounts for 1-15 per mill of the mass of quartz ore powder, and the ore pulp concentration is 10-120 kg/m3The flow rate of the ore pulp is 0.1-1.5 m/s.
The steel wool is uniformly wound on the steel mesh or pressed into the sheet-shaped objects which are arranged in the separator at equal intervals, and the interval is 2-10 nm.
The pulp dispersing agent is one or a mixture of more of sodium hexametaphosphate, washing powder, sodium tripolyphosphate, sodium pyrophosphate, sodium thiophosphate and sodium carbonate.
SiO obtained after superconducting high-gradient magnetic separation in S22Washing the coarse and fine powder with deionized water to neutrality to remove SiO2Residual dispersing agent on the surface of the coarse powder.
The S3 specifically comprises the following steps:
SiO obtained by magnetic separation of S22Carrying out a section of normal-pressure stirring and acid leaching on the coarse and fine powder for 4-12 h under the assistance of ultrasound, filtering, and washing with deionized water to be neutral; then carrying out 2-4 stages of acid leaching under the same ultrasonic and normal-pressure stirring conditions; finally, the leached SiO is2Filtering, washing with deionized water to neutrality, and oven drying to obtain high purity SiO with content of over 99.95% (up to 99.99%)2。
The ultrasonic power is 400-4000W.
The acid leaching solution is one or more mixed acid of sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid, nitric acid and citric acid; the temperature of acid leaching is 30-80 ℃; the stirring speed is 200-250 r/min.
The SiO obtained by magnetically separating the acid leaching liquid and S22The liquid-solid ratio (mL/g) of the coarse refined 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 the advantages of simple processing flow, low production cost and high product quality, and can extract high-purity SiO with the content of more than 99.95 percent2And (5) producing the 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 efficient resource high-added-value utilization system, optimizes the industrial structure, promotes the industrial development and brings huge economic benefit and ecological environmental protection benefit for enterprises.
(3) For SiO2The rest part after extraction can extend an 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 like, thereby realizing the full use of the whole industry.
Drawings
FIG. 1 shows a low-carbon green SiO crystal of the invention2Technical scheme of the fine purification method.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
The invention provides a low-carbon green SiO superconducting high-strength magnetic coupling quartz ore2A fine purification method.
As shown in fig. 1, the method comprises the steps of:
s1: drying, crushing and finely grinding quartz ore;
s2: SiO by using superconductive high-gradient magnetic separation technology2Separation and extraction;
s3: preparation of high-purity SiO by multi-stage acid leaching refining purification technology under assistance of ultrasound2。
The following description is given with reference to specific examples.
The superconductive high-strength magnetic coupling fine purification SiO of the embodiment2The method of (1), comprising:
step 1: drying quartz ore, crushing and grinding the quartz ore to a particle size of 325-425 meshes to obtain quartz raw ore powder; wherein SiO in the quartz raw ore2The content of (A) is more than 90%.
Step 2: SiO by using superconductive high-gradient magnetic separation technology2Separation and extraction;
under the condition that the magnetic field intensity is 2-5T, the steel wool volume filling rate is 3-15%, the ratio of one or more of sodium hexametaphosphate, washing powder, sodium tripolyphosphate, sodium pyrophosphate, sodium thiophosphate and sodium carbonate is 1-15 per mill of the amount of quartz ore powder, and the concentration of ore pulp is 10-120 kg/m3The ore pulp flow velocity is 0.1-1.5 m/s, the superconducting magnetic separation is carried out, the high-efficiency removal of iron oxide, aluminum oxide and other fine-particle weak magnetic substances is realized, and more than 99 percent of SiO is obtained2Coarse refined powder; the steel wool is uniformly wound on a steel net or pressed into sheet-shaped objects which are arranged in the separator at equal intervals (2-10 nm), so that the adsorption area between the surface of the steel wool and weak magnetic substances is increased.
And step 3: SiO obtained after S2 magnetic separation2Washing the coarse refined powder with deionized water to neutrality to remove residual SiO2Dispersing agent on the surface of the coarse powder. Performing magnetic separation and concentration on one or more of sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid, nitric acid and citric acid and the SiO obtained in the step S2 at an ultrasonic power of 400-4000W and a stirring speed of 200-250 r/min and an acid leaching temperature of 30-80 DEG C2Carrying out primary stirring and acid leaching for 4-12 h under normal pressure under the condition that the liquid-solid ratio (mL/g) of the coarse refined powder is 3-10: 1, filtering, and washing with deionized water to be neutral; then carrying out 2-4 stages of acid leaching under the same condition; finally, the leached SiO is2Filtering, washing with deionized water to neutrality, and drying to obtain high-purity SiO2And (5) producing the product.
Wherein, generally, the concentration of sulfuric acid is (4-12) mol/L, the concentration of hydrochloric acid is (5-10) mol/L, the concentration of acetic acid is (4-14) mol/L, the concentration of phosphoric acid is (6-12) mol/L, the concentration of nitric acid is (3-8) mol/L, and the concentration of citric acid is (8-12) mol/L.
Finally obtained high-purity SiO2SiO is measured by chemical analysis2The 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 obtain quartz ore powder with the particle size of 325 meshes; wherein SiO in quartz ore2The content of (B) is 95%.
Under the condition that the magnetic field intensity is 2T, the volume filling rate of steel wool is 15 percent, sodium hexametaphosphate, washing powder, sodium tripolyphosphate, sodium pyrophosphate, sodium thiophosphate, sodium carbonate and a mixture (the mass ratio of the sodium hexametaphosphate to the washing powder is 1: 1) respectively account for 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 ore powder, and the concentration of ore pulp is 10kg/m3The superconductive magnetic separation is carried out under the condition that the flow rate of ore pulp is 1m/s, the high-efficiency removal of iron oxide, aluminum oxide and other fine-particle weak magnetic substances is realized, and the obtained SiO2The content of the coarse refined powder is respectively 99.23%, 99.53%, 99.13%, 99.17%, 99.34%, 99.04% and 99.56%; the steel wool is uniformly wound on the steel mesh and is arranged in the separator at equal intervals (2nm), so that the adsorption area between the surface of the steel wool and weak magnetic substances is increased.
SiO obtained after magnetic separation2Washing the coarse refined powder with deionized water to neutrality to remove residual SiO2Dispersing agent on the surface of the coarse powder. Under the conditions that the ultrasonic power is 4000W, the stirring speed is 220r/min, the acid leaching temperature is 80 ℃, 4mol/L sulfuric acid solution and S2 are subjected to magnetic separation and fine selection to obtain SiO2Carrying out primary stirring and acid leaching for 12h under normal pressure under the condition that the liquid-solid ratio (mL/g) of the coarse refined powder is 10:1, filtering, and washing to be neutral by using deionized water; then carrying out two-stage normal-pressure stirring and acid leaching for 12h under the same condition; finally, the leached SiO is2Filtering, washing with deionized water to neutrality, and drying to obtain high-purity SiO2And (5) producing the product.
Finally obtained high-purity SiO2SiO is measured by chemical analysis2The contents respectively reach 99.985%, 99.989%, 99.969%, 99.977%, 99.986%, 99.957% and 99.993%.
Examples 8 to 14
Mixing quartzDrying the ore, and crushing the ore to the particle size of 400 meshes to obtain quartz ore powder; wherein SiO in quartz ore2The content of (B) is 90%.
Under the condition that the magnetic field intensity is 5T, the volume filling rate of steel wool is 3 percent, the sodium hexametaphosphate accounts for 4 per mill of the quartz ore powder, and the ore pulp concentration is 40kg/m3The ore pulp flow velocity is 0.1m/s to carry out superconducting magnetic separation, thereby realizing the high-efficiency removal of iron oxide, aluminum oxide and other fine-particle weak magnetic substances and obtaining SiO2The content of coarse refined powder is 99.34 percent; the steel wool is pressed into sheets and arranged in the separator at equal intervals (10nm), so that the adsorption area between the surface of the steel wool and weak magnetic substances is increased.
The SiO obtained after magnetic separation2Washing the coarse refined powder with deionized water to neutrality to remove residual SiO2Dispersing agent on the surface of the coarse powder. The ultrasonic power is 400W, the stirring speed is 200r/min, the acid leaching temperature is 60 ℃, the acid leaching solution is respectively subjected to magnetic separation and concentration by using 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 (4mol/L sulfuric acid solution): V (5mol/L hydrochloric acid solution): 1:2) and S2 to obtain SiO2Carrying out a section of stirring and acid leaching under normal pressure for 8 hours under the condition that the liquid-solid ratio (mL/g) of the coarse refined powder is 3:1, filtering, and washing with deionized water to be neutral; then carrying out three-stage normal-pressure stirring and acid leaching for 8h under the same condition; finally, the leached SiO is2Filtering, washing with deionized water to neutrality, and drying to obtain high-purity SiO2And (5) producing the product.
Finally obtained high-purity SiO2SiO is measured by chemical analysis2The contents of the components 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 the particle size of 425 meshes; wherein SiO in quartz ore2The content of (A) was 98.5%.
Under the condition that the magnetic field intensity is 4T, the volume filling rate of steel wool is 8 percent, the sodium hexametaphosphate accounts for 4 per mill of the quartz ore powder, and the ore pulp concentration is 80kg/m3The superconductive magnetic separation is carried out under the condition that the flow velocity of ore pulp is 1.5m/s to realize the fineness of ferric oxide, aluminum oxide and the likeHigh-efficiency removal of granular weak magnetic substances to obtain SiO2The content of coarse refined powder is 99.21 percent respectively; the steel wool is pressed into sheets which are arranged in the separator at equal intervals (5nm), so that the adsorption area between the surface of the steel wool and weak magnetic substances is increased.
Mixing SiO2Washing the coarse refined powder with deionized water to neutrality to remove residual SiO2Dispersing agent on the surface of coarse and fine powder. Under the conditions of ultrasonic power of 2000W, stirring speed of 250r/min, acid leaching temperature of 80 ℃, mixed acid (V (4mol/L acetic acid): V (6mol/L hydrochloric acid solution): V (3mol/L nitric acid solution): 6:3:1) and SiO obtained after magnetic separation and fine selection2The liquid-solid ratio (mL/g) of the crude powder is 6: 1, stirring and acid leaching for 4 hours under normal pressure, filtering, and washing with deionized water to be neutral; then carrying out four-stage acid leaching under the same condition, stirring and acid leaching for 4 hours under normal pressure; finally, the leached SiO is2Filtering, washing with deionized water to neutrality, and drying to obtain high-purity SiO2And (5) producing the product.
Finally obtained high-purity SiO2SiO is measured by chemical analysis2The content respectively reaches 99.989 percent.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. Superconductive high-strength magnetic coupling quartz ore low-carbon green SiO2The fine purification method is characterized by comprising the following steps:
s1: drying, crushing and finely grinding quartz ore;
s2: SiO by using superconductive high-gradient magnetic separation technology2Separation and extraction;
s3: preparation of high-purity SiO by multi-stage acid leaching refining purification technology under assistance of ultrasound2。
2. The superconducting high-strength magnetically-coupled quartz ore low-carbon green SiO product of claim 12Method for fine purificationThe method is characterized in that SiO in the quartz ore in S12The content of (A) is more than 90%, and the mixture is finely ground to a particle size of 325-425 meshes.
3. The superconducting high-strength magnetically-coupled quartz ore low-carbon green SiO product of claim 12The fine purification method is characterized in that in S2, during superconducting high-gradient magnetic separation, 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 per mill of the mass of the quartz ore powder, and the ore pulp concentration is 10-120 kg/m3The flow rate of the ore pulp is 0.1-1.5 m/s.
4. The superconducting high-strength magnetically-coupled quartz ore low-carbon green SiO product of claim 32The fine purification method is characterized in that the steel wool is uniformly wound on a steel net or pressed into sheet-shaped objects which are arranged in a separator at equal intervals, and the intervals are 2-10 nm.
5. The superconducting high-strength magnetically-coupled quartz ore low-carbon green SiO product of claim 32The fine purification method is characterized in that the pulp dispersant is one or a mixture of more of sodium hexametaphosphate, washing powder, sodium tripolyphosphate, sodium pyrophosphate, sodium thiophosphate and sodium carbonate.
6. The superconducting high-strength magnetically-coupled quartz ore low-carbon green SiO product of claim 12The fine purification method is characterized in that the SiO obtained after the superconducting high-gradient magnetic separation in the S2 is adopted2Washing the coarse and fine powder with deionized water to neutrality to remove SiO2Residual dispersing agent on the surface of the coarse powder.
7. The superconducting high-strength magnetically-coupled quartz ore low-carbon green SiO product of claim 12The fine purification method is characterized in that the S3 specifically comprises the following steps:
SiO obtained by magnetic separation of S22Carrying out primary normal-pressure stirring and acid leaching on the coarse and fine powder for 4-12 hours under the assistance of ultrasound, filtering, and washing with deionized water to be neutral; then at the same ultrasoundCarrying out 2-4 sections of acid leaching under the condition of normal pressure stirring; finally, the leached SiO is2Filtering, washing with deionized water to neutrality, and oven drying to obtain high purity SiO with content up to 99.95%2。
8. The superconducting high-strength magnetically-coupled quartz ore low-carbon green SiO of claim 72The fine purification method is characterized in that the ultrasonic power is 400-4000W.
9. The superconducting high-strength magnetic coupling quartz ore low-carbon green SiO2The fine purification method is characterized in that the acid leaching solution is one or more mixed acid of sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid, nitric acid and citric acid; the temperature of acid leaching is 30-80 ℃; the stirring speed is 200-250 r/min.
10. The superconducting high-strength magnetically-coupled quartz ore low-carbon green SiO of claim 72The fine purification method is characterized in that the acid leaching solution and SiO obtained by magnetic separation of S22The liquid-solid ratio of the coarse refined powder is 3-10: 1 mL/g.
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