CN114455590A - Quartz sand acid elution pure method - Google Patents
Quartz sand acid elution pure method Download PDFInfo
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- CN114455590A CN114455590A CN202210304099.9A CN202210304099A CN114455590A CN 114455590 A CN114455590 A CN 114455590A CN 202210304099 A CN202210304099 A CN 202210304099A CN 114455590 A CN114455590 A CN 114455590A
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
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Abstract
A quartz sand acid elution pure method, put the quartz sand after desliming into acid liquor composed of many organic acids to soak, stir while heating, after the temperature reaches 80 degrees, the quartz sand is heated in compound acid liquor, the iron-removing effect is obviously higher than the effect of using a single acid liquor; for quartz products which have high requirements on iron content and silicon content, a floatation method is continuously used after the quartz products are crushed and classified by a jet mill, and the quartz products are continuously classified by cationic collection to form silicon micro powder with different grades.
Description
Technical Field
The invention relates to the technical field of quartz sand purification, in particular to a quartz sand acid elution purification process.
Background
The high-purity and ultra-high-purity quartz sand prepared by mineral separation and purification is widely applied to high-tech fields such as aerospace, laser, optical cable communication, war industry, packaging materials, copper-clad plates, paint coatings and the like.
At present, a magnetic separation method or a flotation method is mainly adopted for purifying and removing iron in quartz sand, and if the iron content in the quartz sand is more than 300PPM and the particle size is coarse with 120 meshes, the iron content can be effectively reduced to 150PPM by the magnetic separation method. Flotation is mainly used for reducing impurities in quartz sand, such as potassium, albite, calcium, magnesium and the like.
However, if the iron content is required to be reduced below 100PPM, or even lower, an acid wash process is used.
The current common pickling method mainly selects inorganic acid to carry out pickling iron removal, such as sulfuric acid, hydrochloric acid, nitric acid or mixed acid thereof.
The inorganic acid has great influence on environmental ecology, has high environmental protection requirement and is difficult to pass environmental evaluation in many places.
In application document No. CN200410044471.9, a process for preparing and purifying quartz sand and quartz powder and its product are disclosed, wherein various quartz raw ores → rough concentration → crushing → primary concentration → roasting → water crushing, and iron removal after dry grinding or wet grinding, characterized in that after water crushing, oxalic acid or citric acid is adopted for acid leaching → dry grinding or wet grinding → high gradient magnetic → magnetic separation → grading → combined process washing → flotation → deionized water washing → special drying → vacuum packaging. The method has the advantages that the oxalic acid or citric acid is selected for acid leaching to purify the quartz sand, so that the content of iron is reduced, the oxalic acid or citric acid belongs to organic acid, the influence on the environment is small, and the requirement on environmental protection can be met, but only the oxalic acid or citric acid is used, and the content of iron in the obtained quartz sand or quartz powder is higher for the application with higher requirement, such as the fields of packaging materials, copper clad plates or aerospace and the like.
Therefore, a more efficient and environment-friendly quartz sand purification method without using inorganic acid is also sought, so that the iron content can be greatly reduced.
Disclosure of Invention
In order to solve the problems, the invention provides a method for deeply purifying quartz sand by using combined organic acid.
Technical scheme
A quartz sand acid elution purification method comprises the following steps:
after being crushed, the mined quartz blocks are cleaned, and then are put into a crusher for crushing;
step 1, crushing: putting the rough quartz sand into a crusher for crushing, sieving with an N-mesh sieve, and continuously crushing the quartz sand on the sieve; the crusher is preferably a ball mill, the medium of the ball mill is ceramic balls, and the lining plate is a high-aluminum lining plate, a rubber lining plate and the like to prevent secondary pollution;
step 2, acid leaching: soaking the sieved quartz sand in acid liquor, wherein the solid-to-liquid ratio of the quartz sand to the acid liquor is 1: 3-5, wherein the acid solution consists of oxalic acid with the concentration of 15-30%, citric acid with the concentration of 0.8-15%, dimethylformamide with the concentration of 0.5-0.9% and hydrogen peroxide with the concentration of 0.5-2%;
step 3, stirring: heating the acid liquor to 50-100 ℃ and stirring for 2-5 hours;
and 4, cleaning: separating quartz sand from acid liquor, and cleaning the quartz sand with purified water or ionized water for 3-5 times until the pH value is neutral; stirring and heating to 50-80 ℃ during first cleaning, and then cleaning without heating;
and 5, separating, namely separating the quartz sand from water to obtain the low-iron quartz sand.
Preferably, the N-mesh sieve in the step 1 is 20-mesh sieve, 120-mesh sieve, 200-mesh sieve or 320-mesh sieve.
Preferably, the acid solution comprises, by weight, 40-60% of oxalic acid, 20-30% of citric acid, 10-20% of dimethylformamide and 5-15% of hydrogen peroxide.
Preferably, the temperature of the acid solution in the step 4 is heated to 80 to 100 ℃.
Preferably, the stirring time of the step 4 is 2-3 h.
As a further improvement of the method for purifying the quartz sand: when the quartz sand is fine quartz powder with 600 meshes, the method also comprises the following steps:
and 6, grinding and grading the low-iron quartz sand obtained in the step 5 by using a jet mill to obtain silicon micropowder with a certain mesh number, and mixing the silicon micropowder with ionized water according to a weight ratio of 1: 5 to obtain a mixed solution;
step 7, the weight ratio of the ionic water to the ionic water in the previous step is 1200-1500: adding the cationic collector of 1 into the mixed solution, continuously stirring for 1 minute, and then performing flotation for three to five minutes to obtain flotation silica micropowder and residual solution;
and 8, adding ionized water with the weight of more than 30% into the residual liquid obtained in the previous step, repeating the process in the step 7 at least more than once, and sorting out the silicon micro powder with different purity grades.
And 9, putting the obtained silicon micro powder with different grades into ionized water for ultrasonic cleaning, filtering, drying and vacuum packaging.
The cationic collector is an ether amine collector or a fatty amine collector.
The ether amine collector is polyether amine D-400, or polyether amine D-230, or polyether amine D-2000.
The aliphatic amine collecting agent is lauryl amine or stearyl amine.
Advantageous effects
1. Putting the deslimed quartz sand into a composite liquid consisting of oxalic acid, citric acid, dimethyl formamide and hydrogen peroxide for soaking, heating and stirring, and when the temperature reaches 80 ℃, heating the quartz sand in the composite acid liquid, wherein the iron removal effect is obviously higher than that of using a single acid liquid;
2. for quartz products which have high requirements on iron content and silicon content, a floatation method is continuously used after the quartz products are ground and classified by a jet mill, and the silicon micro powder with different grades is continuously formed by classification through cation collection.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments.
All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A quartz sand acid elution purification method comprises the following steps:
step 1, crushing: and (3) putting the rough quartz sand into a crusher for crushing, sieving by using an N-mesh sieve, and returning the quartz sand on the sieve to the crusher for continuous crushing.
And (3) crushing the mined quartz blocks, scrubbing the crushed quartz blocks to form rough quartz sand, and then putting the rough quartz sand into a crusher to be crushed. The crusher is preferably a ball mill, the medium of the ball mill is selected from high-alumina balls or ceramic balls and the like to prevent secondary pollution, and the lining plate in the crusher is selected from a high-alumina lining plate, a rubber lining plate and the like to prevent secondary pollution.
Step 2, acid leaching: soaking the sieved quartz sand in acid liquor, wherein the solid-to-liquid ratio of the quartz sand to the acid liquor is 1: 3-5, wherein the acid solution consists of oxalic acid with the concentration of 15-30%, citric acid with the concentration of 0.8-15%, dimethylformamide with the concentration of 0.5-0.9% and hydrogen peroxide with the concentration of 0.5-2%.
Step 3, stirring: heating the acid liquor and the quartz sand to 80-100 ℃ and stirring for 2-5 hours; preferably 3-4 hours.
The acid liquor is placed in a reaction kettle, quartz sand is added, then the acid liquor is heated and stirred, and oxalic acid and citric acid can reduce ferric oxide of the quartz sand.
Organic acid is selected to combine into composite acid liquid which is more effective than single acid. Dimethylformamide is a colorless, transparent liquid, has strong polarity and low toxicity, and is a good organic solvent. The method is favorable for improving the impurity removal effect of oxalic acid and citric acid, and dimethylformamide can be hydrolyzed to generate formic acid and dimethylamine when the aqueous solution is boiled. The formic acid removes impurities in the quartz sand, and the effect is obvious.
And 4, cleaning: filtering with a centrifuge, separating quartz sand from the acid liquor, and allowing the acid liquor to flow into an acid storage pool for recycling. Putting the separated quartz sand into a washing tank, and mixing according to a solid-liquid ratio of 1: 5, washing with purified water or ionized water for 3-5 times until the pH value is neutral. Stirring and heating to 50-80 ℃ during first cleaning, so that the acid liquor on the surface of the quartz sand can be quickly cleaned, and later cleaning is not required to be heated again to save energy consumption. The water after cleaning is treated and recycled.
And 5, separating, namely separating the quartz sand from water to obtain the low-iron quartz sand.
The ferric oxide of the low-iron quartz sand processed by the steps is reduced to be below 100PPM, so that most market demands can be met, and the low-iron quartz sand can be directly dried, packaged and delivered. For example, meet the standard requirements of photovoltaic glass sand.
Several examples of producing photovoltaic low-iron glass sand with 20-120 mesh and acid temperature controlled at boiling are given below to illustrate the pickling effect:
| examples | SiO2(％) | Fe2O3(％) | Al2O3(％) | TiO2(％) |
| Cleaning the crushed raw ore | 99.56 | 0.045 | 0.17 | 0.04 |
| Acid washing for 2 hours | 99.81 | 0.0053 | 0.026 | 0.021 |
| Pickling for 3 hours | 99.92 | 0.0042 | 0.021 | 0.015 |
| Pickling for 4 hours | 99.96 | 0.0033 | 0.019 | 0.011 |
| Pickling for 5 hours | 99.98 | 0.0027 | 0.011 | 0.008 |
The N-mesh sieve in the step 1 is 20-mesh sieve, 120-mesh sieve, 200-mesh sieve and 320-mesh sieve.
Preferably, the acid solution comprises, by weight, 40-60% of oxalic acid, 20-30% of citric acid, 10-20% of dimethylformamide and 5-15% of hydrogen peroxide. In practical application, aiming at different meshes and different purposes of the quartz sand, the weight ratio of each component can be adjusted according to needs.
Preferably, the temperature of the acid solution in the step 4 is heated to 80 to 100 ℃.
Preferably, the stirring time of the step 4 is 2-3 h.
If the glass sand is to be made, the quartz sand after sieving is required to be 20 to 120 meshes.
The quartz has wide application fields, and different fields have different requirements on mesh number. If the rubber is used for industries such as paint and coating, 600 meshes to 2500 meshes are required, if the rubber is used for packaging materials or copper-clad plates, 1000 meshes to 5000 meshes are required, and the rubber requires 1250-; the epoxy floor paint requires 600 meshes and 1250 meshes.
In order to meet the above requirements, it is also necessary to continue the grinding classification of the low-iron quartz sand obtained. The silica sand is ground and classified, usually by a jet mill, while being ground.
The jet mill, the cyclone separator, the dust remover and the induced draft fan form a whole set of crushing system. Compressed air is filtered and dried, and then is injected into a crushing cavity at a high speed through a nozzle, materials at the intersection point of a plurality of high-pressure air flows are repeatedly collided, rubbed and sheared to be crushed, the crushed materials move to a classification area along with ascending air flows under the suction action of a fan, under the action of strong centrifugal force generated by a classification turbine rotating at a high speed, the coarse and fine materials are separated, fine particles meeting the particle size requirement enter a cyclone separator and a dust remover through a classification wheel to be collected, and the coarse particles descend to the crushing area to be continuously crushed.
Instead of using gas flow for polarization, fluid classification may be used.
The fine silica powder obtained after the grinding and classification by the jet mill may contain some impurities, and flotation is performed in order to obtain high-purity fine silica powder.
Flotation also comprises the following steps:
and 6, grinding and grading the low-iron quartz sand obtained in the step 5 by using a jet mill to obtain silicon micropowder with a certain mesh number, and mixing the silicon micropowder with ionized water according to a weight ratio of 1: 5 to obtain a mixed solution.
Step 7, the weight ratio of the ionized water to the ionized water in the previous step is 1200-1500: adding the cationic collector of 1 into the mixed solution, continuously stirring for 1 minute, and then carrying out flotation for three to five minutes to obtain the flotation silica micropowder and the residual solution.
The cationic collector is an ether amine collector or a fatty amine collector.
The ether amine collector is polyether amine D-400, or polyether amine D-230, or polyether amine D-2000.
The aliphatic amine collecting agent is lauryl amine or stearyl amine.
And 8, adding ionized water with the weight of more than 30% into the residual liquid obtained in the previous step, repeating the process in the step 7 at least more than once, and sorting out the silicon micro powder with different purity grades.
And 9, putting the obtained silicon micro powder with different grades into ionized water for ultrasonic cleaning, filtering, drying and vacuum packaging.
The silica sand impurities are not present in elemental form, but are generally present in the form of aluminosilicate minerals, such as feldspar, mica, calcite, etc., metal oxides, such as magnetite, ilmenite, etc. The purity of the crushed quartz sand particles is not uniform.
Example (b): the mesh number of the quartz powder is 600 to 800 meshes, and in the flotation, the step 6 is stirred for one minute, four minutes are carried out for each flotation, and the quartz powder is subjected to flotation five times, so that the quartz powder in the following table is obtained:
| examples | SiO2(％) | Fe2O3(％) | Al2O3(％) | TiO2(％) |
| Before flotation | 99.98 | 0.0027 | 0.011 | 0.008 |
| First flotation | 99.994 | 0.0016 | 0.006 | 0.002 |
| Second flotation | 99.987 | 0.0021 | 0.009 | 0.005 |
| Third flotation | 99.78 | 0.0033 | 0.014 | 0.007 |
| Fourth flotation | 99.67 | 0.0045 | 0.017 | 0.012 |
| Fifth flotation | 99.61 | 0.0065 | 0.023 | 0.019 |
With the increase of the flotation times, the content of impurities in the obtained flotation quartz sand is gradually increased, namely, the quartz sand with different purity grades is separated from the same batch of quartz sand.
The composition of the quartz sand is complex, and in addition to iron-containing ores, mica/feldspar, clay minerals and the like are frequent. Different capture methods can be selected according to different compositions.
In the prior art, quartz minerals are separated from impurity minerals such as feldspar and mica by flotation and the like for purification, and the impurities contained in quartz sand are generally treated as uniform. However, in practice the distribution of impurities in the silica sand is not uniform.
The invention selects proper collecting agent and proper flotation process to separate the same batch of quartz sand into quartz sand with different purity grades according to the characteristic of quartz sand minerals, thereby being applicable to different fields and improving the application value of the quartz sand.
After the acid washing is finished, the obtained low-iron quartz sand can be subjected to high-temperature calcination and water quenching, then is cleaned and dried by ultrasonic waves, and finally is packaged in vacuum. The high-purity silicon powder obtained in the way has smaller particle size and higher whiteness and purity, and can also effectively prevent the produced quartz product from foaming.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. The quartz sand acid elution purification method is characterized by comprising the following steps of:
step 1, crushing: putting the rough quartz sand into a crusher for crushing, sieving with an N-mesh sieve, and continuously crushing the quartz sand on the sieve; the crusher is preferably a ball mill, the medium of the ball mill is ceramic balls, and the lining plate is a high-aluminum lining plate, a rubber lining plate and the like to prevent secondary pollution;
step 2, acid leaching: soaking the sieved quartz sand in acid liquor, wherein the solid-to-liquid ratio of the quartz sand to the acid liquor is 1: 3-5, wherein the acid solution consists of oxalic acid with the concentration of 15-30%, citric acid with the concentration of 0.8-15%, dimethylformamide with the concentration of 0.5-0.9% and hydrogen peroxide with the concentration of 0.5-2%;
step 3, stirring: heating the acid liquor to 50-100 ℃ and stirring for 2-5 hours;
and 4, cleaning: separating quartz sand from acid liquor, and cleaning the quartz sand with purified water or ionized water for 3-5 times until the pH value is neutral; stirring and heating to 50-80 ℃ during first cleaning, and then cleaning without heating;
and 5, separating, namely separating the quartz sand from water to obtain the low-iron quartz sand.
2. The quartz sand pickling purification method as defined in claim 1, wherein the N-mesh sieves in step 1 are 20-mesh sieves, 120-mesh sieves, 200-mesh sieves and 320-mesh sieves.
3. The quartz sand pickling purification method as defined in claim 1, wherein the acid solution comprises, by weight, 40-60% of oxalic acid, 20-30% of citric acid, 10-20% of dimethylformamide and 5-15% of hydrogen peroxide.
4. The quartz sand pickling purification method as defined in claim 1, wherein the temperature of the acid solution in the step 4 is heated to 80 to 90 degrees.
5. The quartz sand pickling purification method as defined in claim 1, wherein the stirring time in step 4 is 2-3 hours.
6. The quartz sand pickling purification method as claimed in claim 1, wherein when the quartz sand is 600 mesh fine quartz powder, the method further comprises the steps of:
and 6, grinding and grading the low-iron quartz sand obtained in the step 5 by using a jet mill to obtain silicon micropowder with a certain mesh number, and mixing the silicon micropowder with ionized water according to a weight ratio of 1: 5 to obtain a mixed solution;
step 7, the weight ratio of the ionic water to the ionic water in the previous step is 1200-1500: adding the cationic collector of 1 into the mixed solution, continuously stirring for 1 minute, and then performing flotation for three to five minutes to obtain flotation silica micropowder and residual solution;
step 8, adding more than 30% of ionized water by weight into the residual liquid obtained in the previous step, repeating the process of the step 7 at least more than once, and sorting out the silicon micro powder with different purity grades;
and 9, putting the obtained silicon micro powder with different grades into ionized water for ultrasonic cleaning, filtering, drying and vacuum packaging.
7. The quartz sand pickling purification method of claim 6, wherein the cationic collector is an ether amine collector or a fatty amine collector.
8. The quartz sand acid elution purification method as claimed in claim 7, wherein the ether amine collector is polyether amine D-400 or polyether amine D-230 or polyether amine D-2000.
9. The quartz sand acid elution purification process of claim 7, wherein the fatty amine collector is dodecylamine or octadecylamine.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115771897A (en) * | 2022-11-23 | 2023-03-10 | 平远县正远实业有限公司 | Method for purifying quartz sand by continuous acid washing |
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| JPH01224215A (en) * | 1988-03-01 | 1989-09-07 | Nitto Chem Ind Co Ltd | Fine particulate silica slurry and production thereof |
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