CN109319791A - A kind of experiment equipment ultrapure quartz sand and its preparation method and application - Google Patents
A kind of experiment equipment ultrapure quartz sand and its preparation method and application Download PDFInfo
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- CN109319791A CN109319791A CN201811165345.7A CN201811165345A CN109319791A CN 109319791 A CN109319791 A CN 109319791A CN 201811165345 A CN201811165345 A CN 201811165345A CN 109319791 A CN109319791 A CN 109319791A
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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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of experiment equipment ultrapure quartz sands and its preparation method and application, after the present invention carries out purification processes to excessively domestic quartzy silicon mine by processing steps such as selected quartzy silicon mine, " chloroazotic acid " impurity elimination, flotation, high-temperature vacuum processing, ultrasonic wave purifications, the ultrapure quartz sand that can be used for preparing high-precision experiment equipment is obtained.The requirement of present invention combination commercial production scale; special adjustment has been carried out to the process route of laboratory research of the present invention; the process conditions of further perfect microwave treatment production ultrapure quartz sand; it sums up and is suitable for industrial process conditions; in particular for the ultrapure quartz sand raw material sources in China; conscientiously the manufacturing condition for being determined that domestic quartzy silicon mine produces ultrapure quartz sand raw material is provided; mature, reasonable, technical effect is stablized, and provides technical support for large-scale production, the real production cost preparation for reducing ultrapure quartz sand of ultrapure quartz sand.
Description
Technical field
The present invention relates to super pure silica technical field of material, more particularly, to a kind of ultrapure stone of experiment equipment
Sand and its preparation method and application.
Background technique
In recent years with dust PM2.5, CO2, SO2 that manufacturing industry and building industry generate formed haze, greenhouse effects with
Acid rain etc. seriously pollutes environment.And non-renewable disposable traditional fossil energy resource is reduced, and finds the new energy and green
Energy technology becomes current worldwide key subjects.Such as solar energy, it is the first choice of current new energy development, in photovoltaic industry
Ultrapure quartz sand is indispensable.With high-tech development, high-grade all-transparent quartz sand demand is continuously increased, and mineral crystal
But exhausted, the eighties in last century, people get only the substitute of water detection crystalline substance, start to explore the depth that silicon ore replaces crystal
Degree purification research.
The high-grade high-precision experiment equipment of all-transparent is SiO2Single content is up to 99.99% or more extraordinary quartz sand, has
Chemical stabilization, all-transparent, impurity content are low, spectral transmission is wide, heat shock resistance is (when can be repeatedly long under 1420 DEG C of hot environments
Between using indeformable), resistance to x ray irradiation x, ultraviolet light penetrate entirely, devitrification resistance can strong, hardness up to seven grades of Mohs, the coefficient of expansion it is small,
The superior physical chemistry such as resistance to thermal shock is strong, electrical insulating property is good, the resistance to corrosion of nearly all acid in addition to hydrofluoric acid and hot phosphoric acid
Energy.
Currently, the whole world possesses the factory for producing the core technology for the ultrapure quartz sand that SiO2 content reaches 99.99%
Family is very few, and wherein the Unimin Corp. (US) (UNIMIN) in the U.S. and General Electric Co. Limited (GE) have almost monopolized entire ultrapure stone
Sand supplies market.Either foreign enterprise or Chinese Enterprise are all using external import quartz silicon mine mostly as raw material
It carries out purification and prepares Li in ultrapure quartz sand, such as Madagascar, Norway's import quartz silicon mine+、K+、Na2+、Fe2+、Al3+
Etc. alkali metal ion content measureds lower than alkali metal ion in crystal, while gas liquid inclusion content is also one lower than China's quartz silicon mine
The order of magnitude, therefore conveniently can be used as the raw material of substitution crystal by purification.But import resources are expensive, and by the limit of exported country
System and the exchange rate influence, so that ultrapure quartz sand production cost and source are restricted by various aspects.
Although China's quartz silicon ore resources deposit very abundant, cheap, gas-liquid package in domestic quartz silicon mine
Body content is significantly larger than external import quartz silicon mine, and not only alkali metal ion content measured is high in the ultrapure quartz sand prepared, simultaneously
Containing hydroxyl, the fusion point for the quartzy article prepared is reduced, when (1420 degrees Celsius) uses of high-temperature area have not yet been reached
It will appear local collapse, cause the subsequent product of quartz material to be scrapped, or crystallization occur when not up to quartz material is using temperature,
This prepares ultrapure quartz sand to domestic quartzy silicon mine and brings technical difficulty, seriously limits domestic quartzy silicon ore resources
It promotes and applies, and is often only used for preparing the quartz sand product of some low sides, can not be used to prepare quartzy Hessian crucible, quartz
The middle and high end product such as heavy stone used as an anchor, experiment equipment, semiconductor.
Gas liquid inclusion content is much higher than chalazie in the quartz sand that the prior art passes through domestic quartzy silicon mine preparation, and
And the gas liquid inclusion content in the quartz sand of domestic mine preparation is rejected not exclusively, which has limited common silicon ores to refine ultrapure stone
Sand substitution crystal prepares high-precision experiment equipment and China and substitutes the bottle that crystal prepares high-precision experiment equipment material with silicon ore
Neck.
Since current technique limits, the quartz sand SiO2 content of domestic quartz silicon mine production can only at most reach 99.96%,
Technology stability is bad, and often internal layer is opaque or contains bubble for the high-precision experiment equipment prepared, and the transparency is not good enough.With
China's high-tech technology development needs, the demand to ultrapure quartz sand will be increasing, therefore, in order to break foreign countries at this
The long-term technical monopoly in field, gives full play to china natural resources advantage, needs to realize domestic ultrapure quartz sand industrialized production.
Summary of the invention
The technical problem to be solved by the present invention is to higher for gas liquid inclusion content in domestic quartz sand in the prior art
It can not be applied to high-grade experiment equipment, a kind of ultrapure quartz sand of ultrapure low alkali metal content is provided.
Another technical problem to be solved by the present invention is that for existing ultrapure quartz sand preparation process can not reject it is domestic
The deficiency of gas liquid inclusion in quartz sand provides and a kind of prepares experiment equipment ultrapure quartz sand using common domestic quartzy silicon mine
Purifying technique, which may be implemented ultrapure quartz sand industrial-scale production, and domestic raw material can be used, at low cost,
Technical effect is stablized.
Another technical problem to be solved by the present invention is that providing the ultrapure quartz sand applied to experiment equipment.
Ultrapure quartz sand partial size of the present invention is 50~80 mesh, SiO in ultrapure quartz sand2Content > 99.999%, alkali
Total metal content < 50mg/kg, gas liquid inclusion content are 90~110mg/kg.
Further, the ultrapure quartz sand partial size is 50~80 mesh, SiO in ultrapure quartz sand2Content be 99.999~
99.9999%, alkali metal total content is 20~32mg/kg.
The ultrapure quartz sand of selection appropriate particle size not only contributes to the purification of quartz sand, and another party can also ensure subsequent product
High-quality.It is difficult to remove the impurity such as gas liquid inclusion in the excessive purification process of partial size while influencing to melt.
The preparation method of experiment equipment ultrapure quartz sand provided by the invention mainly gives reality by the following technical programs
It is existing, specifically include following preparation step:
S1. selected quartzy silicon mine: icp analysis is repeated in the domestic quartzy silicon mines in multiple areas and is compared, is screened, so
Afterwards, it is soaked with low concentration acid solution with clean the surface impurity, then is got express developed with a large amount of deionized waters, obtain quartzy silicon mine crude product；
S2. acidleach: by crude product particle obtained by step S1 through Raymond mill, sieving, " chloroazotic acid " impregnates, and removal metal is miscellaneous
Matter, then rinsed with deionized water to get quartz sand crude product；
S3. flotation: flotation in flotation solvent is added in quartz sand crude product obtained by step S2 and rejects non-quartz sand particle；
S4. magnetic separation: the quartz sand crude product after step S3 flotation is rinsed with deionized water, after drying, then uses magnet separator magnetic
Choosing；
S5. high-temperature vacuum is handled: the step S4 quartz sand particle magneticly elected is placed under high temperature, vacuum condition and is kept the temperature,
Lead to chlorine treatment, superconduction purification after cooling again；
S6. ultrasonication: by quartz sand particle obtained by step S5 by ultrasonication to get ultrapure quartz sand.
Further, alkali metal total content is filtered out in step S1 lower than 220mg/kg, gas liquid inclusion total content is
The quartzy silicon mine of 1600~2000mg/kg.
Preferably, the alkali metal total content is lower than 150mg/kg；Al < 92mg/kg, Ca < 5mg/kg, K in alkali metal <
63mg/kg、Na<43mg/kg。
Further, acid solution described in step S1 is one or more of oxalic acid, hydrochloric acid, phosphoric acid, sulfuric acid, the acid
Solution concentration is 1~10%.
Acid solution used excludes most strong using former corrosivity completely and can generate permanent damage to environment, generate forever simultaneously
Can not far wither away F-1HF acid.
Preferably, acid solution described in step S1 is one or more of hydrochloric acid, phosphoric acid, and the acid solutions are
3%.
Acid concentration is too low, and reaction is slow, and time-consuming, and impurity-eliminating effect is poor；Acid concentration is excessively high volatile, causes cost inclined
Height, while environment is polluted, it on the other hand can corrode container and SiO2；The too low reaction rate of acidleach temperature is slow, reaction is not thorough, temperature
It is volatile to spend peracid, concentration easily reduces, therefore, suitable acidleach concentration and acidleach temperature not only on properties of product influence compared with
Greatly, while also it will affect cost control.
Further, it is 60~120min that the time is embathed described in step S1, and embathing temperature is 80~92 DEG C.
Further, the sieve mesh number that pulverizes and sieves described in step S2 is 50~80 mesh, " chloroazotic acid " and quartzy silicon mine crude product
Granular mass ratio is 1:0.5~4, and soaking time is 10~15h, and soaking temperature is 50~58 DEG C, and thunder used in the Raymond mill covers
Ball is high density quartz ball or high aluminium ball.
The present invention can avoid crushing the new metal impurities of friction introducing using high density quartz ball and high aluminium ball.
Further, flotation solvent described in step S3 is prodan, dodecyl sodium sulfate, pentadecanoic acid, oxidation stone
Wax soap, N- (2- aminoethyl)-lauramide, N, one or more of N- dimethyl lauryl amine.
Further, high-temperature temperature described in step S5 is 800~830 DEG C, keeps the temperature 50~90min；Surpass described in step S6
Sonication power is 27~32kw, and sonication treatment time is 30~90min, is ultrasonically treated 35~55 DEG C of temperature.
Beneficial effects of the present invention:
The present invention controls reaction temperature by rationally designing processing step, by easily neutralize the acid not strong with corrosivity and
Its rational proportion, by reasonable process, the especially industrial microwave use condition found out repeatedly of application, effectively remove
Gas liquid inclusion in quartzy silicon mine is prepared to realize the purification of domestic quartzy silicon mine and can be used for accurate experiment equipment
Material, can effectively avoid local collapse phenomenon in quartz sand experiment equipment preparation process, the experiment equipment precision prepared
Height improves the yield rate of quartz sand preparation.
And quartz sand prepared by the present invention have chemical stabilization, all-transparent, impurity content is low, spectral transmission is wide,
Heat shock resistance (can be under 1420 DEG C of hot environments repeatedly for a long time using indeformable), resistance to x ray irradiation x, ultraviolet light penetrate entirely, resist
Crystallization is strong, hardness reaches seven grades of Mohs, the coefficient of expansion is small, resistance to thermal shock is strong, electrical insulating property is good, resistance to several in addition to hydrofluoric acid and hot phosphoric acid
The superior physical and chemical performances such as the corrosion of all acid.
The present invention prepares the process environmental protection easy to operate of ultrapure quartz sand, process stabilizing, and gained ultrapure quartz sand is pure
Degree can reach 99.999%.The requirement of present invention combination commercial production scale carries out the process route of laboratory research of the present invention
Special adjustment, further perfect domestic quartzy silicon mine prepare the process conditions of ultrapure quartz sand, sum up and be suitable for state
The industrial process conditions of mine are produced, are that the scale of domestic quartzy silicon mine uses, really reduces being produced into for ultrapure quartz sand
Offer technical support is originally provided.Change China be chronically at import, supply not can fully ensure that, material quality be difficult to ensure it is high-end
Quartz material problem of industry status outstanding, cracks engineering challenge, thoroughly abolishes China's high-technology industry related with the world
Develop unfavorable bottleneck, raising China's quartz silicon ore resource pair is value added comprehensively, and Technological Economy and social benefit are double good, and can mention
High China's industry international status.
Specific embodiment
It is explained further and illustrates combined with specific embodiments below, but specific embodiment does not have any form to the present invention
Restriction.Unless otherwise specified, method and apparatus used in embodiment be conventional method in that art and equipment, it is raw materials used
For conventional commercial raw material.Following embodiment is using Heilungkiang quartz silicon mine, Macheng, hubei Province quartz silicon mine as silicon mine raw material, thunder used
It covers ball and uses high density quartz ball.
Embodiment 1 prepares ultrapure quartz sand
S1. selected quartzy silicon mine: domestic quartzy silicon mine is subjected to repeatedly icp analysis and is compared, alkali metal total content is filtered out
Lower than 220mg/kg, the silicon mine that gas liquid inclusion total content is 2000mg/kg, the hydrochloric acid for being 1% with concentration is under the conditions of 80 DEG C
Quartzy silicon mine 2h is impregnated, then is got express developed with a large amount of deionized waters, quartzy silicon mine crude product is obtained；
S2. by crude product particle obtained by step S1 through Raymond mill, 50 meshes, under the conditions of 50 DEG C, " chloroazotic acid " acidleach: are crossed
In mass ratio it is that 1:1 impregnates 15h with quartzy silicon mine crude product particle, removes metal impurities, then rinsed to get quartz with deionized water
Sand crude product；
S3. flotation: dodecyl sodium sulfate is added in quartz sand crude product obtained by step S2 and N, N- dimethyl lauryl amine are dense
Degree rejects non-quartz sand particle than flotation in the solvent for 1:1；
S4. magnetic separation: the quartz sand crude product after step S3 flotation is rinsed with deionized water, after drying, then uses magnet separator magnetic
Choosing；
S5. high-temperature vacuum is handled: step S4 being magneticly elected the quartz sand particle come and is placed under 800 DEG C of high temperature, vacuum conditions
90min is kept the temperature, leads to chlorine treatment, superconduction purification after cooling again；
S6. ultrasonication: the ultrasound for being 27kw by power under the conditions of 35 DEG C by quartz sand particle obtained by step S5
Wave handles 90min to get ultrapure quartz sand.
Embodiment 2 prepares ultrapure quartz sand
S1. selected quartzy silicon mine: domestic quartzy silicon mine is subjected to repeatedly icp analysis and is compared, alkali metal total content is filtered out
Lower than 200mg/kg, the silicon mine that gas liquid inclusion total content is 1900mg/kg, the hydrochloric acid for being 2% with concentration is under the conditions of 82 DEG C
Quartzy silicon mine 2h is impregnated, then is got express developed with a large amount of deionized waters, quartzy silicon mine crude product is obtained；
S2. by crude product particle obtained by step S1 through Raymond mill, 60 meshes, under the conditions of 55 DEG C, " chloroazotic acid " acidleach: are crossed
In mass ratio it is that 1:0.5 impregnates 15h with quartzy silicon mine crude product particle, removes metal impurities, then rinsed to get stone with deionized water
Sand crude product；
S3. pentadecanoic acid, oxidized paraffin wax soap, N- (2- aminoethyl)-laurel flotation: is added in quartz sand crude product obtained by step S2
Amide concentration rejects non-quartz sand particle than flotation in the solvent for 1:1:1；
S4. magnetic separation: the quartz sand crude product after step S3 flotation is rinsed with deionized water, after drying, then uses magnet separator magnetic
Choosing；
S5. high-temperature vacuum is handled: step S4 being magneticly elected the quartz sand particle come and is placed under 810 DEG C of high temperature, vacuum conditions
62min is kept the temperature, leads to chlorine treatment, superconduction purification after cooling again；
S6. ultrasonication: the ultrasound for being 30kw by power under the conditions of 38 DEG C by quartz sand particle obtained by step S5
Wave handles 90min to get ultrapure quartz sand.
Embodiment 3 prepares ultrapure quartz sand
S1. selected quartzy silicon mine: domestic quartzy silicon mine is subjected to repeatedly icp analysis and is compared, alkali metal total content is filtered out
Lower than the silicon mine that 150mg/kg, gas liquid inclusion total content are lower than 1800mg/kg, the phosphoric acid for being 3% with concentration is in 85 DEG C of conditions
The quartzy silicon mine 1h of lower immersion, then got express developed with a large amount of deionized waters, obtain quartzy silicon mine crude product；
S2. by crude product particle obtained by step S1 through Raymond mill, 68 meshes, under the conditions of 55 DEG C, " chloroazotic acid " acidleach: are crossed
In mass ratio it is that 2:1 impregnates 12h with quartzy silicon mine crude product particle, removes metal impurities, then rinsed to get quartz with deionized water
Sand crude product；
S3. flotation: dodecyl sodium sulfate is added in quartz sand crude product obtained by step S2 and N, N- dimethyl lauryl amine are dense
Degree rejects non-quartz sand particle than flotation in the solvent for 1:1；
S4. magnetic separation: the quartz sand crude product after step S3 flotation is rinsed with deionized water, after drying, with magnetic separator magnetic separation；
S5. high-temperature vacuum is handled: step S4 being magneticly elected the quartz sand particle come and is placed under 810 DEG C of high temperature, vacuum conditions
75min is kept the temperature, leads to chlorine treatment, superconduction purification after cooling again；
S6. ultrasonication: the ultrasound for being 30kw by power under the conditions of 35 DEG C by quartz sand particle obtained by step S5
Wave handles 58min to get ultrapure quartz sand.
Embodiment 4 prepares ultrapure quartz sand
S1. selected quartzy silicon mine: domestic quartzy silicon mine is subjected to repeatedly icp analysis and is compared, alkali metal total content is filtered out
Lower than the silicon mine that 180mg/kg, gas liquid inclusion total content are lower than 1800mg/kg, the hydrochloric acid for being 3% with concentration is in 90 DEG C of conditions
The quartzy silicon mine 1.5h of lower immersion, then got express developed with a large amount of deionized waters, obtain quartzy silicon mine crude product；
S2. by crude product particle obtained by step S1 through Raymond mill, 72 meshes, under the conditions of 55 DEG C, " chloroazotic acid " acidleach: are crossed
In mass ratio it is that 1:3 impregnates 12h with quartzy silicon mine crude product particle, removes metal impurities, then rinsed to get quartz with deionized water
Sand crude product；
S3. flotation: dodecyl sodium sulfate is added in quartz sand crude product obtained by step S2 and N, N- dimethyl lauryl amine are dense
Degree rejects non-quartz sand particle than flotation in the solvent for 1:0.5；
S4. magnetic separation: the quartz sand crude product after step S3 flotation is rinsed with deionized water, after drying, then uses magnet separator magnetic
Choosing；
S5. high-temperature vacuum is handled: step S4 being magneticly elected the quartz sand particle come and is placed under 810 DEG C of high temperature, vacuum conditions
82min is kept the temperature, leads to chlorine treatment, superconduction purification after cooling again；
S6. ultrasonication: the ultrasound for being 30kw by power under the conditions of 45 DEG C by quartz sand particle obtained by step S5
Wave handles 80min to get ultrapure quartz sand.
Embodiment 5 prepares ultrapure quartz sand
S1. selected quartzy silicon mine: domestic quartzy silicon mine is subjected to repeatedly icp analysis and is compared, alkali metal total content is filtered out
Lower than the silicon mine that 200mg/kg, gas liquid inclusion total content are lower than 1600mg/kg, the hydrochloric acid for being 10% with concentration is in 92 DEG C of conditions
The quartzy silicon mine 1h of lower immersion, then got express developed with a large amount of deionized waters, obtain quartzy silicon mine crude product；
S2. by crude product particle obtained by step S1 through Raymond mill, 80 meshes, under the conditions of 58 DEG C, " chloroazotic acid " acidleach: are crossed
In mass ratio it is that 1:4 impregnates 10h with quartzy silicon mine crude product particle, removes metal impurities, then rinsed to get quartz with deionized water
Sand crude product；
S3. flotation: dodecyl sodium sulfate is added in quartz sand crude product obtained by step S2 and N, N- dimethyl lauryl amine are dense
Degree rejects non-quartz sand particle than flotation in the solvent for 0.5:1；
S4. magnetic separation: the quartz sand crude product after step S3 flotation is rinsed with deionized water, after drying, then uses magnet separator magnetic
Choosing；
S5. high-temperature vacuum is handled: step S4 being magneticly elected the quartz sand particle come and is placed under 830 DEG C of high temperature, vacuum conditions
50min is kept the temperature, leads to chlorine treatment, superconduction purification after cooling again；
S6. ultrasonication: the ultrasound for being 32kw by power under the conditions of 55 DEG C by quartz sand particle obtained by step S5
Wave handles 30min to get ultrapure quartz sand.
Comparative example 1 prepares ultrapure quartz sand
S1. selected quartzy silicon mine: Madagascar's quartz silicon mine is subjected to repeatedly icp analysis and is compared, alkali metal is filtered out
Total content lower than 180mg/kg, gas liquid inclusion total content be lower than 1800mg/kg silicon mine, with concentration be 3% hydrofluoric acid in
Quartzy silicon mine is impregnated under the conditions of 80 DEG C, is got express developed with a large amount of deionized waters, is obtained quartzy silicon mine crude product；
S2. water quenching: 1000 DEG C will be heated to after quartzy silicon mine crude product acidleach obtained by step S1, then quickly met into the water
It is cold to burst 10S, obtain crude product particle；
S3. by crude product particle obtained by step S2 through Raymond mill, 68 meshes, under the conditions of 40 DEG C, " chloroazotic acid " acidleach: are crossed
In mass ratio it is that 2:1 impregnates 72h with quartzy silicon mine crude product particle, removes metal impurities, then rinsed to get quartz with deionized water
Sand crude product；
S4. flotation: flotation in dodecyl sodium sulfate solvent is added in quartz sand crude product obtained by step S3 and rejects non-quartz
Sand particle；
S5. magnetic separation: the quartz sand crude product after step S4 flotation is rinsed with deionized water, after drying, then uses magnet separator magnetic
Choosing；
S6. high-temperature vacuum is handled: step S5 is magneticly elected the quartz sand particle come and is placed under high temperature, vacuum condition and is reacted,
Lead to chlorine treatment, superconduction purification after cooling again；
S7. ultrasonication: the ultrasound for being 21kw by power under the conditions of 35 DEG C by quartz sand particle obtained by step S6
Wave handles 58min to get ultrapure quartz sand.
Comparative example 2 prepares ultrapure quartz sand
Step is same as Example 3, the difference is that filtering out alkali metal total content in step S1 is 230~250mg/
Kg, the quartzy silicon mine that gas liquid inclusion total content is 2100~2200mg/kg.
Comparative example 3 prepares ultrapure quartz sand
Step is same as Example 3, the difference is that will be without 40 DEG C of soaking temperature in step S2.
Comparative example 4 prepares ultrapure quartz sand
Step is same as Example 3, the difference is that step S5 high temperature temperature is 600 DEG C, in step S6 at ultrasound
Reason power is 20kw.
Comparative example 5 prepares ultrapure quartz sand
Step is same as Example 3, the difference is that the grinding device Raymond mill in step S1 is stainless using high density
Steel ball substitutes high density quartz ball.
Domestic quartz silicon mine used in the present invention is set forth through present invention process condition gas-liquid packet before and after the processing in table 1~4
Body content and alkali metal content experimental result are wrapped up in, it is as shown in the table for specific testing result.As seen from table, the present invention is by adjusting technique
Parameter and preparation step can effectively improve the purity of ultrapure quartz sand, reduce gaseous impurity and alkaline metal ions in quartz sand
Content, wherein alkali metal total content reduces 60% in the ultrapure quartz sand that the present invention is prepared, and content is well below right
The ultrapure quartz sand of ratio preparation.
The quartzy silicon mine-gas liquid Fluid Inclusion Compositions content (unit: mg/kg) of table 1
Table 2 is the ultrapure quartz sand gas liquid inclusion component content (unit: mg/kg) being prepared
| Sample | CO2 | H2O | O2 | N2 | CH4 | CO | Total amount |
| Embodiment 1 | 9.53 | 83.42 | 0.18 | 0.48 | 0.68 | 1.61 | 95.90 |
| Embodiment 2 | 9.78 | 82.13 | 0.15 | 0.41 | 0.63 | 1.60 | 94.47 |
| Embodiment 3 | 8.95 | 78.81 | 0.11 | 0.33 | 0.59 | 1.49 | 90.28 |
| Embodiment 4 | 9.69 | 79.95 | 0.23 | 0.45 | 0.64 | 1.51 | 92.47 |
| Embodiment 5 | 10.01 | 80.00 | 0.18 | 0.47 | 0.79 | 1.69 | 93.14 |
| Comparative example 1 | 9.31 | 83.58 | 0.17 | 0.44 | 0.73 | 1.55 | 95.78 |
| Comparative example 2 | 21.61 | 108.29 | 0.13 | 3.92 | 0.92 | 5.11 | 139.98 |
| Comparative example 3 | 24.63 | 96.39 | 0.13 | 5.61 | 0.81 | 6.23 | 133.80 |
| Comparative example 4 | 26.74 | 90.29 | 0.12 | 5.68 | 0.83 | 6.02 | 129.68 |
| Comparative example 5 | 12.65 | 123.17 | 0.14 | 1.51 | 0.95 | 1.72 | 140.14 |
| Level-one crystal | 9.74 | 84.17 | 0.3 | 0.5 | 2.35 | 1.62 | 98.74 |
Impurity content (unit: mg/kg) in each quartzy silicon mine of table 3
Impurity content (unit: mg/kg) in quartz sand after the purification of table 4
| Sample | Al | Fe | Ca | Mg | B | Li | Na | K | Mn | Ni | Cu | Cr |
| Embodiment 1 | 15.85 | 1.11 | 0.49 | 1.05 | 0.36 | 0.24 | 4.24 | 3.68 | 0.24 | 0.03 | 0.27 | <0.04 |
| Embodiment 2 | 15.67 | 1.15 | 0.53 | 1.20 | 0.32 | 0.22 | 5.04 | 3.81 | 0.25 | 0.04 | 0.20 | <0.04 |
| Embodiment 3 | 14.32 | 0.82 | 0.38 | 0.95 | 0.26 | 0.19 | 4.04 | 3.18 | 0.20 | 0.03 | 0.22 | <0.04 |
| Embodiment 4 | 15.43 | 1.11 | 0.42 | 1.21 | 0.33 | 0.21 | 4.32 | 3.41 | 0.30 | 0.04 | 0.23 | <0.04 |
| Embodiment 5 | 15.58 | 1.22 | 0.47 | 1.35 | 0.36 | 0.29 | 4.54 | 3.48 | 0.37 | 0.03 | 0.24 | <0.04 |
| Comparative example 1 | 16.72 | 2.15 | 0.63 | 2.41 | 0.51 | 0.55 | 6.04 | 5.44 | 0.45 | 0.05 | 0.27 | <0.05 |
| Comparative example 2 | 18.76 | 9.24 | 1.13 | 2.38 | 0.73 | 1.14 | 7.20 | 9.69 | 1.11 | 0.18 | 0.38 | <0.05 |
| Comparative example 3 | 17.75 | 10.20 | 1.27 | 2.37 | 0.70 | 1.16 | 7.20 | 10.63 | 1.26 | 0.19 | 0.42 | <0.05 |
| Comparative example 4 | 15.73 | 11.12 | 1.24 | 2.34 | 0.71 | 1.11 | 8.20 | 11.23 | 1.31 | 0.21 | 0.41 | <0.05 |
| Comparative example 5 | 16.04 | 2.19 | 0.68 | 2.01 | 0.53 | 0.57 | 6.09 | 5.42 | 0.49 | 0.08 | 0.27 | <0.05 |
Detailed process equipment and process flow of the invention that the present invention is explained by the above embodiments, but the present invention is not
It is confined to above-mentioned detailed process equipment and process flow, that is, does not mean that the present invention must rely on above-mentioned detailed process equipment and work
Skill process could be implemented.It should be clear to those skilled in the art, any improvement in the present invention, to product of the present invention
The equivalence replacement of each raw material and addition, the selection of concrete mode of auxiliary element etc., all fall within protection scope of the present invention and public affairs
Within the scope of opening.
Claims (10)
1. a kind of experiment equipment ultrapure quartz sand, which is characterized in that the ultrapure quartz sand partial size is 50 ~ 80 mesh, ultrapure stone
SiO in sand2Content>99.999%, alkali metal total content<50mg/kg, gas liquid inclusion content are 90 ~ 110mg/kg.
2. experiment equipment ultrapure quartz sand according to claim 1, the ultrapure quartz sand partial size is 50 ~ 80 mesh, is surpassed
SiO in pure quartz sand2Content is 99.999 ~ 99.9999%, and alkali metal total content is 20 ~ 32mg/kg.
3. a kind of preparation method of experiment equipment ultrapure quartz sand, which comprises the following steps:
S1. selected quartzy silicon mine: icp analysis is repeated in the domestic quartzy silicon mines in multiple areas and is compared, screens, then, uses
Low concentration acid solution embathes surface impurity, then is got express developed with a large amount of deionized waters, obtains quartzy silicon mine crude product；
S2. acidleach: by crude product particle obtained by step S1 through Raymond mill, sieving, " chloroazotic acid " impregnates, and removes metal impurities, then
It is rinsed with deionized water to get quartz sand crude product；
S3. flotation: flotation in flotation solvent is added in quartz sand crude product obtained by step S2 and eliminates non-quartz sand particle；
S4. magnetic separation: step S3 quartz sand crude product is rinsed with deionized water, after drying, then with magnetic separator magnetic separation；
S5. high-temperature vacuum is handled: the step S4 quartz sand particle magneticly elected being placed under high temperature, vacuum condition and is kept the temperature, is cooled down
Lead to chlorine treatment, superconduction purification again afterwards；
S6. ultrasonication: by quartz sand particle obtained by step S5 by ultrasonication to get ultrapure quartz sand.
4. the preparation method of experiment equipment ultrapure quartz sand according to claim 3, which is characterized in that wherein, step
Alkali metal total content is filtered out in S1 lower than 220mg/kg, the quartzy silicon that gas liquid inclusion total content is 1600 ~ 2000mg/kg
Mine.
5. the preparation method of experiment equipment ultrapure quartz sand according to claim 3, which is characterized in that institute in step S1
Stating acid solution is one or more of oxalic acid, hydrochloric acid, phosphoric acid, sulfuric acid, and the acid solutions are 1 ~ 10%.
6. the preparation method of experiment equipment ultrapure quartz sand according to claim 3, which is characterized in that described in step S1
Soaking time is 60 ~ 120min, and soaking temperature is 80 ~ 92 DEG C.
7. the preparation method of experiment equipment ultrapure quartz sand according to claim 3, which is characterized in that described in step S2
The sieve mesh number that pulverizes and sieves be 50 ~ 80 mesh, " chloroazotic acid " and quartzy silicon mine crude product granular mass ratio are 1:0.5 ~ 4, soaking time
For 10 ~ 15h, soaking temperature is 50 ~ 58 DEG C, and it is high density quartz ball or high aluminium ball that thunder used in the Raymond mill, which covers ball,.
8. the preparation method of experiment equipment ultrapure quartz sand according to claim 3, which is characterized in that institute in step S3
State flotation solvent be prodan, dodecyl sodium sulfate, pentadecanoic acid, oxidized paraffin wax soap, N- (2- aminoethyl)-lauramide,
One or more of N, N- dimethyl lauryl amine.
9. the preparation method of experiment equipment ultrapure quartz sand according to claim 3, which is characterized in that described in step S5
High-temperature temperature is 800 ~ 830 DEG C, keeps the temperature 50 ~ 90min；Sonification power described in step S6 is 27 ~ 32kw, when ultrasonic treatment
Between be 30 ~ 90min, be ultrasonically treated 35 ~ 55 DEG C of temperature.
10. as the described in any item ultrapure quartz sands of claim 1 ~ 9 are applied to accurate, high-grade experiment equipment.
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| CN110950346A (en) * | 2019-12-26 | 2020-04-03 | 湖南工业大学 | Process for purifying and preparing ultra-pure quartz sand by fluorine-free and nitric acid-free leaching method and ultra-pure quartz sand |
| CN112010317A (en) * | 2020-09-14 | 2020-12-01 | 昆明理工大学 | Method for purifying quartz sand by microwave-vacuum combined roasting |
| CN114368757A (en) * | 2022-01-21 | 2022-04-19 | 成都光华科技发展有限公司 | Purification method of high-purity quartz sand |
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| CN104071792A (en) * | 2013-03-26 | 2014-10-01 | 南京大学连云港高新技术研究院 | Preparing process of high-purity quartz sand used for quartz steelyard weight production |
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| CN104071792A (en) * | 2013-03-26 | 2014-10-01 | 南京大学连云港高新技术研究院 | Preparing process of high-purity quartz sand used for quartz steelyard weight production |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110950346A (en) * | 2019-12-26 | 2020-04-03 | 湖南工业大学 | Process for purifying and preparing ultra-pure quartz sand by fluorine-free and nitric acid-free leaching method and ultra-pure quartz sand |
| CN110950346B (en) * | 2019-12-26 | 2022-12-02 | 湖南工业大学 | Process for purifying and preparing ultra-pure quartz sand by fluorine-free and nitric acid-free leaching method and ultra-pure quartz sand |
| CN112010317A (en) * | 2020-09-14 | 2020-12-01 | 昆明理工大学 | Method for purifying quartz sand by microwave-vacuum combined roasting |
| CN112010317B (en) * | 2020-09-14 | 2022-06-07 | 昆明理工大学 | Method for purifying quartz sand by microwave-vacuum combined roasting |
| CN114368757A (en) * | 2022-01-21 | 2022-04-19 | 成都光华科技发展有限公司 | Purification method of high-purity quartz sand |
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