CN104150487A - Processing method for purifying high-purity silicon - Google Patents
Processing method for purifying high-purity silicon Download PDFInfo
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- CN104150487A CN104150487A CN201410352717.2A CN201410352717A CN104150487A CN 104150487 A CN104150487 A CN 104150487A CN 201410352717 A CN201410352717 A CN 201410352717A CN 104150487 A CN104150487 A CN 104150487A
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Abstract
The invention relates to a processing method for purifying high-purity silicon and the method is applied in the field of material processing purification. The processing method for purifying high-purity silicon provided by the invention comprises two steps of crushing/cleaning and pickling, wherein quartz stone of which the particle diameter is 1-5cm is reacted and purified by virtue of hydrochloric acid vapor, so that the purity of SiO2 in the purified quartz stone is relatively high. The processing method is simple, the reaction time is shortened and the usage amount of hydrochloric acid is reduced and thus the processing method is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of purification process of high-purity silicon working method, the present invention relates to a kind of purification process of high-purity silicon working method, be applied to China's materials processing purification field.
Background technology
Quartz is a kind of mineral of most study the most common in the earth's crust, and chemical composition is mainly SiO
2, submember is Al
2o
3fe
2o
3, MgO, CaONaCOK
2the compositions such as O, therefore mix SiO at quartzite crystallisation process
2impurity component in addition, has seriously affected the application in our high-end technology.The method of tradition purification quartzite exists salt acid consumption large, and the one week left and right time of reaction needed is the problems such as length consuming time.
Summary of the invention
For the weak point existing in the problems referred to above, the invention provides a kind of purification process of high-purity silicon working method, SiO in the quartzite after purification processes
2purity higher, the method technique is simple, has shortened the reaction times, has reduced hydrochloric acid usage quantity, is applicable to suitability for industrialized production.
The invention provides a kind of purification process of high-purity silicon working method, it is characterized in that, comprise the following steps:
Step 1, crushing washing, first carries out fragmentation by the former mineral material of quartzite after screening, broken after the diameter of material be 1-5 ㎝, by the friction of overturn of the material input material washing machine after fragmentation, injection pure water washs;
Step 2, pickling, pack the material after fragmentation washing into reaction vessel, shut reaction vessel lid, carry out heat treated toward the water vapor that injects 170 degrees Celsius in container, in the time that reaching 120 degrees Celsius, container center temperature stops supplying gas, whole reaction unit is placed under room temperature, in reaction vessel, inject hydrochloric acid soln by pipeline, material in container after broken washing and the mass ratio of hydrochloric acid soln are 100:1, hydrochloric acid soln volatilizees and produces hydrochloric acid vapour in the container of 120 degrees Celsius, with the stifling material of hydrochloric acid vapour four hours, reclaim hydrochloric acid, after reaction finishes, injected 1 st pure water at interval of one hour reacted material is sprayed to washing, carry out altogether 6 washings, take out the material after washing, obtain the HIGH-PURITY SILICON after purifying.
Described a kind of purification process of high-purity silicon working method, is characterized in that, described hydrochloric acid soln massfraction is 36%.
Described a kind of purification process of high-purity silicon working method, is characterized in that, described material washing machine material is cast steel; The reaction vessel material that described pickling is used is PE plastics.
Beneficial effect of the present invention is:
1, the present invention is simple to operate, can effectively remove the elements such as iron in quartzite, aluminium, sodium, titanium, potassium, calcium, and refining effect is good, is applicable to suitability for industrialized production;
2, the present invention uses high temp. salt acid vapour to remove the impurity in quartzite, and reaction process has been accelerated in the use of high temp. salt acid vapour, has shortened the reaction times, has reduced the usage quantity of hydrochloric acid soln simultaneously.
3, the reaction vessel material that pickling of the present invention is used is PE plastics, and this material inorganics composition is extremely low and pollution-free to quartz.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is described in further detail.But example is not as a limitation of the invention.
Embodiment 1
The quartzite of the HIGH-PURITY SILICON after screening is carried out to fragmentation through crusher, 5-10 ㎝, in the material washing machine that the broken input of building stones cast steel is made, repeatedly rub, injection clear water is stirred, remove raw ore dirt settling, the dirty water of draining, carries out several times repeatedly, until quartzite surface inclusion-free, earth is until material washing machine flows out clear water.
The material that fragmentation has been washed packs in the reaction vessel that PE plastics make, by container sealing, the water vapor that injects 170 degrees Celsius carries out heat treated, in the time that reaching 120 degrees Celsius, the temperature at center stops supplying gas, whole reaction unit is placed under room temperature, in reaction vessel, inject hydrochloric acid soln by pipeline, material in container after broken washing and the mass ratio of hydrochloric acid soln are 100:1, hydrochloric acid soln volatilizees and produces hydrochloric acid vapour in the container of 120 degrees Celsius, with the stifling material of hydrochloric acid vapour four hours, reclaim hydrochloric acid, after reaction finishes, injected 1 st pure water at interval of one hour reacted material is sprayed to washing, carry out altogether 6 washings, take out the material after washing, obtain the HIGH-PURITY SILICON after purifying.Known by the HIGH-PURITY SILICON after comparing raw ore diamond stone and purifying, the HIGH-PURITY SILICON after purifying by present method is cleaner, pure white, has proved effectively to remove the impurity in raw ore.
Embodiment 2
The quartzite of the HIGH-PURITY SILICON after screening is carried out to fragmentation through crusher, 5-10 ㎝, in the material washing machine that the broken input of building stones cast steel is made, repeatedly rub, injection clear water is stirred, remove raw ore dirt settling, the dirty water of draining, carries out several times repeatedly, until quartzite surface inclusion-free, earth is until material washing machine flows out clear water.
The material that fragmentation has been washed packs in the reaction vessel that PE plastics make, by container sealing, the water vapor that injects 170 degrees Celsius carries out heat treated, in the time that reaching 120 degrees Celsius, the temperature at center stops supplying gas, whole reaction unit is placed under room temperature, in reaction vessel, inject hydrochloric acid soln by pipeline, material in container after broken washing and the mass ratio of hydrochloric acid soln are 100:1, hydrochloric acid soln volatilizees and produces hydrochloric acid vapour in the container of 120 degrees Celsius, with the stifling material of hydrochloric acid vapour four hours, reclaim hydrochloric acid, after reaction finishes, injected 1 st pure water at interval of one hour reacted material is sprayed to washing, carry out altogether 6 washings, take out the material after washing, obtain the HIGH-PURITY SILICON after purifying.HIGH-PURITY SILICON to raw ore diamond stone and after purifying is carried out respectively impurity content mensuration, the present embodiment Central Plains iron in ore, aluminium, sodium, titanium, potassium, calcium, magnesium element content are respectively 36ppm, 45.6ppm, 22ppm, 8.3ppm, 12ppm, 5.2ppm, 3.5ppm, and in the HIGH-PURITY SILICON after purification, above-mentioned impurity content is reduced to 18ppm, 22.6ppm, 12.7ppm, 3.2ppm, 6.5ppm, 1.2ppm, 2.1ppm.
Claims (3)
1. a purification process of high-purity silicon working method, is characterized in that, comprises the following steps:
Step 1, crushing washing, first carries out fragmentation by former quartzite mineral material, and the material diameter after fragmentation is 1-5 ㎝, and by the friction of overturn of the material input material washing machine after fragmentation, injection pure water washs;
Step 2, pickling, pack the material after fragmentation washing into reaction vessel, shut reaction vessel lid, carry out heat treated toward the water vapor that injects 170 degrees Celsius in container, in the time that reaching 120 degrees Celsius, container center temperature stops supplying gas, whole reaction unit is placed under room temperature, in reaction vessel, inject hydrochloric acid soln by pipeline, material in container after broken washing and the mass ratio of hydrochloric acid soln are 100:1, hydrochloric acid soln volatilizees and produces hydrochloric acid vapour in the container of 120 degrees Celsius, with the stifling material of hydrochloric acid vapour four hours, reclaim hydrochloric acid, after reaction finishes, injected 1 st pure water at interval of one hour reacted material is sprayed to washing, carry out altogether 6 washings, take out the material after washing, obtain the HIGH-PURITY SILICON after purifying.
2. a kind of purification process of high-purity silicon working method according to claim 1, is characterized in that, described hydrochloric acid soln massfraction is 36%.
3. a kind of purification process of high-purity silicon working method according to claim 1, is characterized in that, described material washing machine material is cast steel; The reaction vessel material that described pickling is used is PE plastics.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410352717.2A CN104150487B (en) | 2014-07-22 | 2014-07-22 | A kind of purification process of high-purity silicon processing method |
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| CN201410352717.2A CN104150487B (en) | 2014-07-22 | 2014-07-22 | A kind of purification process of high-purity silicon processing method |
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| CN104150487B CN104150487B (en) | 2016-07-06 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108584962A (en) * | 2018-07-19 | 2018-09-28 | 江苏斯力康科技有限公司 | Acid vapor is purified metals silicon technology and surface equipment for purifying in advance |
| CN111285376A (en) * | 2020-04-15 | 2020-06-16 | 威海圆环先进陶瓷股份有限公司 | Production process for preparing high-purity quartz powder |
| CN113247913A (en) * | 2021-05-24 | 2021-08-13 | 曹永华 | Quartz purification method for cocoa sea area |
-
2014
- 2014-07-22 CN CN201410352717.2A patent/CN104150487B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108584962A (en) * | 2018-07-19 | 2018-09-28 | 江苏斯力康科技有限公司 | Acid vapor is purified metals silicon technology and surface equipment for purifying in advance |
| CN108584962B (en) * | 2018-07-19 | 2020-05-26 | 江苏斯力康科技有限公司 | Acid steam prepurification metallic silicon process and surface purification equipment |
| CN111285376A (en) * | 2020-04-15 | 2020-06-16 | 威海圆环先进陶瓷股份有限公司 | Production process for preparing high-purity quartz powder |
| CN113247913A (en) * | 2021-05-24 | 2021-08-13 | 曹永华 | Quartz purification method for cocoa sea area |
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| CN104150487B (en) | 2016-07-06 |
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