CN109319789A - A kind of system and application method of commercial recovery silicon material removal metal impurities - Google Patents
A kind of system and application method of commercial recovery silicon material removal metal impurities Download PDFInfo
- Publication number
- CN109319789A CN109319789A CN201811471189.7A CN201811471189A CN109319789A CN 109319789 A CN109319789 A CN 109319789A CN 201811471189 A CN201811471189 A CN 201811471189A CN 109319789 A CN109319789 A CN 109319789A
- Authority
- CN
- China
- Prior art keywords
- silicon material
- metal impurities
- pickling
- removal metal
- poured
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- C01B33/02—Silicon
- C01B33/037—Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of methods of commercial recovery silicon material removal metal impurities, include the following steps, extract: industrial silicon；It is broken: the industrial silicon of extraction being poured into and carries out being crushed to 1~2cm in jaw crusher, then powder processed is carried out with twin rollers or airslide disintegrating mill, obtains powder；Screening: powder is poured into vibrating screen and is sieved, required particle is obtained；Heating stirring pickling: the particle screened being poured into closed reaction kettle and reacted, and being heated to temperature is 50 DEG C, carries out pickling while stirring, and mixing time is 8h, cleaning to neutrality；Then deionized water is filtered by suction filtration machine, is dried using vacuum oven；Content after drying is detected.The utility model has the advantages that effectively reducing production cost, pollution is reduced.
Description
Technical field
The present invention relates to field of polysilicon technology, it particularly relates to a kind of commercial recovery silicon material removal metal impurities dress
It sets.
Background technique
Currently, what polysilicon mostly used is the technique for improveing Siemens technique, power consumption is high, seriously polluted, production cost
It is high.And in contrast, metallurgy method is removed impurity using the various metallurgical technologies such as refining, wet process, vacuum from silicon, not due to silicon
It chemically reacts, so little power consumption, cost is relatively low.It is that one kind is effectively reduced and is produced into that metallurgy method, which prepares solar-grade polysilicon,
Originally, it is specially positioned at the production method of solar-grade polysilicon, can satisfy the rapid development of photovoltaic industry, it has also become is anxious at present
The focus technology that need to be researched and developed.
For the problems in the relevant technologies, currently no effective solution has been proposed.
Summary of the invention
For the problems in the relevant technologies, a kind of method that the present invention proposes commercial recovery silicon material removal metal impurities, with
Overcome above-mentioned technical problem present in existing the relevant technologies.
The technical scheme of the present invention is realized as follows:
A kind of system of commercial recovery silicon material removal metal impurities, including sequentially connected crusher, screening machine, reaction kettle
And compressor, which is characterized in that the crusher includes jaw crusher and air-flow crusher, and the jaw crusher is broken
Silicon material partial size after broken is 1~2cm, and it is 38~160 μm that the airslide disintegrating mill, which obtains smashed silicon material partial size, and described is anti-
The suction filter pump being equipped on the outside of kettle for the liquid after reaction to be extracted and filtered is answered, it is true to be additionally provided with pumping in the reaction kettle
Sky pump and heating wire.
After being crushed silicon material by crusher, sieve material is carried out, completes reaction kettle progress pickling of being allowed for access after sieve is expected, in
With the operation of, deionization etc., then reaction kettle is vacuumized, and the higher silicon material of purity is obtained using heating wire drying operation.
According to an aspect of the present invention, a kind of method of commercial recovery silicon material removal metal impurities is provided.
The method of commercial recovery silicon material removal metal impurities, comprising the following steps:
It extracts: industrial silicon；
It is broken: the industrial silicon of extraction is poured into and carries out being crushed to 1~2cm in jaw crusher, then with twin rollers or
Airslide disintegrating mill carries out powder processed, obtains powder；
Screening: powder is poured into vibrating screen and is sieved, required particle is obtained；
Heating stirring pickling: the particle screened is poured into closed reaction kettle and is reacted, be heated to temperature
It is 50 DEG C, carries out pickling while stirring, and mixing time is 8h, cleaning to neutrality；
Then deionized water is filtered by suction filtration machine, is dried using vacuum oven；
Content after drying is detected.
Further, the partial size for being 38~160 μm by the broken partial size obtained of air-flow all exposes the impurity in silicon material
On silicon material surface, so that the impurity being deposited on grain boundary or at crack is easy to contact with various acid to react, to reach
Remove the purpose of impurity in silicon material.
Further, obtaining the silicon material step that partial size is 38~160 μm includes:
Pure acid is heated to 50 DEG C by liquid-solid ratio for 4:1, is stirred to react 6h in a kettle；
Successively carry out the pickling comparative experiments of chloroazotic acid, nitric acid, HCL, HF, HF+HCL；
Silicon material is cleaned to neutrality with deionized water after reaction；
It filters and dries, sampling carries out metals content impurity detection, is carried out using effect most significantly removal metal process
Purification.
Further, the chloroazotic acid, nitric acid, HCL, HF, HF+HCL pickling time be 5h.
The invention has the benefit that by using the metal impurities in pickling removal industrial silicon, by industrial silicon jaw
Crusher is crushed to 1~2cm, then carries out powder processed with twin rollers or air-flow crusher.Compared with double-roll crusher, air-flow is broken
It is mainly crushed by the impact several times before material, friction, shearing, avoids the contact with metal material to a certain degree,
Reduce the pollution of impurity.In addition, silicon material particle volume size is not only related with pickling effect, but also related with the rate of recovery of silicon material,
Since metal impurities are enriched in grain boundary or silico briquette gap, only silicon material partial size be less than either be equal to grain boundary when
Waiting metal impurities could effectively be removed, but size is smaller, and silicon material is more not easily recycled, when partial size is less than 38 μm, by
It repeatedly to be rinsed in acid cleaning process, so that efficiency reduces, and meticulous silicon material is not easily recycled, and silicon material particle is too small,
Superficial attractive forces enhancing, reactant, which is not easy to leave silicon material surface, to be entered in solution, and easily adsorbs external impurity, therefore, grain
Diameter uses the broken crumbling method effect as industrial silicon of air-flow best at 38~160 μm, and working as in temperature is 50 degrees Celsius
When the middle stirring and pickling time is 5h, the metal effect removed in silicon material is best, when the metal in commercial recovery silicon material is effective
After removal, production cost is effectively reduced, reduces pollution.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is a kind of one of the method flow diagram of commercial recovery silicon material removal metal impurities according to an embodiment of the present invention；
Fig. 2 is the two of the method flow diagram of a kind of commercial recovery silicon material removal metal impurities according to an embodiment of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art's every other embodiment obtained belong to what the present invention protected
Range.
As shown in Figure 1, in the actual production process, the method which removes metal impurities, including it is following
Step:
Step S101 is extracted: industrial silicon；
Step S103, it is broken: the industrial silicon of extraction is poured into and carries out being crushed to 1~2cm in jaw crusher, then with pair
Roller machine or airslide disintegrating mill carry out powder processed, obtain powder；
Screening: step S105 powder is poured into vibrating screen and is sieved, required particle is obtained；
Heating stirring pickling: step S107 the particle screened is poured into closed reaction kettle and is reacted, added
Heat to temperature is 50 DEG C, carries out pickling while stirring, and mixing time is 8h, cleaning to neutrality；
Then step S109, deionized water are filtered by suction filtration machine, are dried using vacuum oven；
Step S1011 detects the content after drying.
In one embodiment, the method for commercial recovery silicon material removal metal impurities, further comprising the steps of:
The partial size for being 38~160 μm by the broken partial size obtained of air-flow, is all exposed to silicon material table for the impurity in silicon material
Face, so that the impurity being deposited on grain boundary or at crack is easy to contact with various acid to react, to reach removal silicon material
The purpose of middle impurity.
In one embodiment, as shown in Fig. 2, the silicon material step that acquirement partial size is 38~160 μm includes:
Pure acid is heated to 50 DEG C by liquid-solid ratio for 4:1, is stirred to react 6h in a kettle by step S201；
Step S203 successively carries out the pickling comparative experiments of chloroazotic acid, nitric acid, HCL, HF, HF+HCL；
Step S205 is after reaction cleaned silicon material to neutrality with deionized water；
Step S207 is filtered and is dried, and sampling carries out metals content impurity detection, most significantly removes metal using effect
Method is purified.
In one embodiment, the chloroazotic acid, nitric acid, HCL, HF, HF+HCL pickling time be 5h.
In conclusion by means of above-mentioned technical proposal of the invention, it is miscellaneous by using the metal in pickling removal industrial silicon
Industrial silicon is crushed to 1~2cm with jaw crusher, then carries out powder processed with twin rollers or air-flow crusher by matter.It is broken with to roller
Broken machine is compared, and air-flow is broken mainly to be crushed by the impact several times before material, friction, shearing, is avoided to a certain degree
Contact with metal material reduces the pollution of impurity.In addition, silicon material particle volume size is not only related with pickling effect, Er Qieyu
The rate of recovery of silicon material is related, since metal impurities are enriched in grain boundary or silico briquette gap, only silicon material partial size be less than or
Metal impurities could be removed effectively when being equal to grain boundary, but size is smaller, and silicon material is more not easily recycled, and works as grain
When diameter is less than 38 μm, due to repeatedly to be rinsed in acid cleaning process, so that efficiency reduces, and meticulous silicon material is not easy back
It receives, silicon material particle is too small, and superficial attractive forces enhancing, reactant, which is not easy to leave silicon material surface, to be entered in solution, and easily absorption is outer
The impurity come, therefore, partial size use the broken crumbling method effect as industrial silicon of air-flow best, and work as at 38~160 μm
When temperature is that the stirring and pickling time is 5h in 50 degrees Celsius, the metal effect removed in silicon material is best.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of method of commercial recovery silicon material removal metal impurities, which comprises the following steps:
It extracts: industrial silicon；
It is broken: the industrial silicon of extraction being poured into and carries out being crushed to 1~2cm in jaw crusher, then with twin rollers or air-flow
Pulverizer carries out powder processed, obtains powder；
Screening: powder is poured into vibrating screen and is sieved, required particle is obtained；
Heating stirring pickling: the particle screened being poured into closed reaction kettle and reacted, and being heated to temperature is 50
DEG C, pickling is carried out while stirring, and mixing time is 8h, cleaning to neutrality；
Then deionized water is filtered by suction filtration machine, is dried using vacuum oven；
Content after drying is detected.
2. the method for commercial recovery silicon material removal metal impurities according to claim 1, which is characterized in that broken by air-flow
The partial size that the partial size of broken acquisition is 38~160 μm, is all exposed to silicon material surface for the impurity in silicon material, so that being deposited on crystal circle
Impurity on face or at crack is easy to contact with various acid to react, to achieve the purpose that remove impurity in silicon material.
3. the method for commercial recovery silicon material removal metal impurities according to claim 2, which is characterized in that obtaining partial size is
38~160 μm of silicon material step includes:
Pure acid is heated to 50 DEG C by liquid-solid ratio for 4:1, is stirred to react 6h in a kettle；
Successively carry out the pickling comparative experiments of chloroazotic acid, nitric acid, HCL, HF, HF+HCL；
Silicon material is cleaned to neutrality with deionized water after reaction；
It filters and dries, sampling carries out metals content impurity detection, is purified using effect most significantly removal metal process.
4. the method for commercial recovery silicon material removal metal impurities according to claim 3, which is characterized in that the chloroazotic acid,
Nitric acid, HCL, HF, HF+HCL pickling time be 5h.
5. a kind of system of commercial recovery silicon material removal metal impurities, including sequentially connected crusher, screening machine, reaction kettle and
Compressor, which is characterized in that the crusher includes jaw crusher and air-flow crusher, the jaw crushing crusher machine
Silicon material partial size afterwards is 1~2cm, and it is 38~160 μm that the airslide disintegrating mill, which obtains smashed silicon material partial size, the reaction
It is equipped with the suction filter pump for the liquid after reaction to be extracted and filtered on the outside of kettle, is additionally provided with and vacuumizes in the reaction kettle
Pump and heating wire.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811471189.7A CN109319789A (en) | 2018-12-04 | 2018-12-04 | A kind of system and application method of commercial recovery silicon material removal metal impurities |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811471189.7A CN109319789A (en) | 2018-12-04 | 2018-12-04 | A kind of system and application method of commercial recovery silicon material removal metal impurities |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109319789A true CN109319789A (en) | 2019-02-12 |
Family
ID=65256854
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811471189.7A Withdrawn CN109319789A (en) | 2018-12-04 | 2018-12-04 | A kind of system and application method of commercial recovery silicon material removal metal impurities |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109319789A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111001577A (en) * | 2019-12-09 | 2020-04-14 | 宁晋晶兴电子材料有限公司 | Method for treating silicon scrap |
| CN113070274A (en) * | 2021-03-31 | 2021-07-06 | 江苏美科太阳能科技有限公司 | High-quality single crystal crushed aggregates treatment method |
| CN114570504A (en) * | 2022-04-02 | 2022-06-03 | 芒市永隆铁合金有限公司 | Purification device of metallic silicon and use method thereof |
-
2018
- 2018-12-04 CN CN201811471189.7A patent/CN109319789A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111001577A (en) * | 2019-12-09 | 2020-04-14 | 宁晋晶兴电子材料有限公司 | Method for treating silicon scrap |
| CN113070274A (en) * | 2021-03-31 | 2021-07-06 | 江苏美科太阳能科技有限公司 | High-quality single crystal crushed aggregates treatment method |
| CN114570504A (en) * | 2022-04-02 | 2022-06-03 | 芒市永隆铁合金有限公司 | Purification device of metallic silicon and use method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100579902C (en) | Method for preparing super metallurgy grade silicon | |
| CN109319789A (en) | A kind of system and application method of commercial recovery silicon material removal metal impurities | |
| CN101659413A (en) | Method for preparing ultra-metallurgical grade silicon | |
| CN103131857B (en) | Method for purifying platinum group metal from waste three-way catalyst | |
| CN102757050B (en) | Acid cleaning purification method of metallic silicon | |
| CN104928475B (en) | A kind of recovery method of the aluminium scrap silicon containing rare earth | |
| CN109607612A (en) | Vanadium in a kind of discarded SCR denitration, tungsten, titanium resource recycling method | |
| CN108328619A (en) | A kind of method that industrial silicon hydrometallurgy removes boron | |
| CN104120444B (en) | A kind of technique using mechanical activation reducing process to reclaim metallic lead from waste and old lead bearing glass | |
| CN104073650B (en) | One reclaims zinc technology from tin metallurgy electric furnace dust | |
| CN104294048A (en) | Method for recycling platinum group metals from iron carrier invalid automobile exhaust catalyst | |
| CN108441640B (en) | A kind of method that waste diamond abrasive material resource comprehensive utilization utilizes | |
| CN109384222A (en) | A kind of diamond environmental protection high efficiency extraction system and extracting method | |
| CN103030149B (en) | Method for removing impurities from industrial silicon | |
| CN111268718B (en) | Method for directly preparing mercury oxide from mercury-containing organic sludge | |
| CN111348653B (en) | Method for preparing high-purity silicon, titanium white and high-purity fluoride by using titanium-containing slag and low-purity silicon material | |
| CN112646982A (en) | Non-ferrous smelting waste short-process treatment system and application | |
| CN101955226A (en) | Extraction process for lixiviating vanadium from vanadium ores in alkali liquor by adopting microwave method | |
| CN109437209A (en) | One kind extracting SiO from nature sand2Method | |
| CN205087938U (en) | Retrieve device of tungstic acid in follow waste flue gas denitration catalyst | |
| CN110846512B (en) | Method for leaching manganese from electrolytic manganese anode slag by sulfuric acid curing | |
| CN204939575U (en) | A kind of device reclaiming W and V from waste flue gas denitration catalyst | |
| CN205088291U (en) | Retrieve metal oxide's device in follow waste flue gas denitration catalyst | |
| CN205087939U (en) | Retrieve ti and W's device in follow waste flue gas denitration catalyst | |
| CN111252769A (en) | Preparation method of solar polycrystalline silicon |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190212 |
|
| WW01 | Invention patent application withdrawn after publication |