CN106315589A - Method for processing recycling waste silicon material - Google Patents
Method for processing recycling waste silicon material Download PDFInfo
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- CN106315589A CN106315589A CN201510347612.2A CN201510347612A CN106315589A CN 106315589 A CN106315589 A CN 106315589A CN 201510347612 A CN201510347612 A CN 201510347612A CN 106315589 A CN106315589 A CN 106315589A
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Abstract
The present invention discloses a method for processing recycling a waste silicon material, and the method comprises the following steps: putting an impurity-containing waste silicon material into a container, and adding an alkaline solution; after the reaction is completed, adding an acid solution into the silicon material, and controlling temperature, pressure and reaction time; after the reaction is completed, adding the silicon material into a prepared mixed acid solution for soaking; finally using pure water for multiple times of ultrasonic rinse of the silicon material until the pH of the rinsed solution is 7; and drying. The beneficial effects are that: by the method combing high temperature and high pressure with acid washing and alkali washing, a great quantity of silicon nitride, silicon carbide, graphite, organic glue and other impurities in a waste layer silicon material can be thoroughly removed so as to realize the reuse of the waste layer silicon material.
Description
Technical field
This invention relates to the method for the recycling of a kind of waste material, particularly to the processing method of the discarded silicon material recycling in a kind of photovoltaic semiconductors field.
Background technology
Photovoltaic is a kind of photovoltaic effect utilizing solar cell semi-conducting material, and solar radiation can be converted directly into a kind of new power generating system of electric energy.And solar cell semi-conducting material is mainly formed cell piece by polysilicon through processing silicon chip, therefore in photovoltaic semiconductors field, the silicon ingot of polysilicon is split into polylith crystalline substance brick through evolution, a lot of discarded silicon material can be produced in the process, there is a large amount of cavity on this silicon material surface, possibly together with impurity such as more carborundum, silicon nitride, aluminium oxide, ferrum oxide, organic gel as from the foregoing.Organic gel impurity in silicon material is mainly derived from the evolution of silicon ingot, owing to silicon ingot organic gel to be passed through before evolution is fixed on supporting plate, carries out evolution in being arranged on excavation machine again after waiting solidification.After evolution completes, still on some gluing corner being attached to silicon ingot, there is much such impurity on the waste layer silicon material surface therefore obtained after silicon ingot evolution.
Prior art has used the methods such as sandblasting, froth flotation, centrifugation, high-temperature fusion filtration to impurity such as carborundum, silicon nitride or the graphite of removing in silicon material, but these method operating costs are high, it is not easy to produce in batches, and it is the most thorough owing to processing the silicon material remove impurity obtained, typically be difficult to the raw material directly as polycrystalline silicon ingot casting again with, therefore cause greatly waste.
Summary of the invention
The technical problem to be solved in the present invention is to provide the processing method of a kind of discarded silicon material recycling, the method is used to be possible not only to remove and be difficult to the impurity such as the carborundum, the silicon nitride that remove under normal temperature and pressure, can also remove the impurity such as graphite, organic gel, the discarded silicon material after recycling is also used as the raw material of polycrystalline silicon ingot casting and recycles.
Technical scheme: the processing method of a kind of discarded silicon material recycling, it is characterised in that comprise the following steps:
A) the discarded silicon material containing impurity is put in container, add alkaline solution；
B) after question response is complete, then in silicon material, add acid solution, control temperature, pressure and response time；
C), after question response is complete, silicon material is put in the mixed acid solution prepared and soaks；
D) finally using pure water that silicon material is carried out repeated ultrasonic rinsing, to rinsing, the pH value of solution is 7；
E) dry.
Described alkali liquor mass percent concentration is 35%～40%, and alkali cleaning temperature is 40～60 DEG C, and the alkali cleaning time is 20～40min.
In described acid solution, the temperature of reaction controls between 60～80 DEG C, and Stress control is between 1～3MPa, and the time controlled between 2～4 hours.
Described nitration mixture is concentrated sulphuric acid and the mixing of one of which in Fluohydric acid., hydrochloric acid, nitric acid；The weight percent concentration of described various acid is: Fluohydric acid. is 35%～55%, and nitric acid is 68%～98%, and hydrochloric acid is 30%～38%, and concentrated sulphuric acid is more than 90%.
Described container is container high temperature resistant, high pressure resistant, corrosion resistant.
In described said method, the gas that all chemical reactions produce is passed through after exhaust gas processing device processes and discharges, the most specially treated rear discharge of waste liquid of generation.
Adding acid solution in silicon material, control temperature, pressure and response time, its principle is as follows:
Theoretical according to chemical kinetics, the substantial connection of the many factors such as chemical reaction rate and reaction temperature, solvent strength, decomposition pressure, response time.Using and increase reaction temperature, improve decomposition pressure and decompose some difficult materials decomposed under room temperature, normal pressure, such as materials such as carborundum, silicon nitride, organic gel, and the method technique is simple, it is easy to operation.
The present invention selects the hydrogen peroxide use of proper ratio, decreases the loss of silicon material.
Beneficial effect: the present invention uses the method that High Temperature High Pressure and acid, alkali cleaning combine, can remove the most thoroughly discarded silicon material contains a large amount of carborundums, silicon nitride, graphite, the impurity such as organic gel, thus realize the recycling of discarded silicon material.
Detailed description of the invention
In order to make the object, technical solutions and advantages of the present invention clearer, below the preferred embodiments of the present invention are described in detail.
Embodiment 1, the processing method of a kind of discarded silicon material recycling: the discarded silicon material containing impurity is put in container high temperature resistant, high pressure resistant, corrosion resistant, the sodium hydroxide solution adding appropriate 35% reacts, controlling reaction temperature is 40 DEG C, and the response time is 20min；Reaction terminates to add in backward container Fluohydric acid., controls reaction temperature 60 DEG C, pressure 1MPa, 2 hours response time；After question response is complete, silicon material being placed in the mixed acid solution of Fluohydric acid. and concentrated sulphuric acid immersion 20min, wherein the volume ratio of Fluohydric acid. and concentrated sulphuric acid is 1:6, eventually passes the ultrasonic rinsing of pure water, dries, i.e. can obtain can be directly used for the solar energy level silicon material of polycrystalline silicon ingot casting.
Embodiment 2, the processing method of a kind of discarded silicon material recycling: the discarded silicon material containing impurity is put in container high temperature resistant, high pressure resistant, corrosion resistant, the sodium hydroxide solution adding appropriate 40% reacts, controlling reaction temperature is 50 DEG C, and the response time is 30min；Reaction terminates to add in backward container Fluohydric acid., controls reaction temperature 70 DEG C, pressure 2MPa, 3 hours response time；After question response is complete, silicon material being placed in the mixed acid solution of Fluohydric acid. and concentrated sulphuric acid immersion 40min, wherein the volume ratio of Fluohydric acid. and concentrated sulphuric acid is 1:7, eventually passes the ultrasonic rinsing of pure water, dries, i.e. can obtain can be directly used for the solar energy level silicon material of polycrystalline silicon ingot casting.
Embodiment 3, the processing method of a kind of discarded silicon material recycling: the discarded silicon material containing impurity is put in container high temperature resistant, high pressure resistant, corrosion resistant, the sodium hydroxide solution adding appropriate 40% reacts, controlling reaction temperature is 60 DEG C, and the response time is 40min；Reaction terminates to add in backward container Fluohydric acid., controls reaction temperature 80 DEG C, pressure 3MPa, 4 hours response time；After question response is complete, silicon material being placed in the mixed acid solution of Fluohydric acid. and concentrated sulphuric acid immersion 60min, wherein the volume ratio of Fluohydric acid. and concentrated sulphuric acid is 1:8, eventually passes the ultrasonic rinsing of pure water, dries, i.e. can obtain can be directly used for the solar energy level silicon material of polycrystalline silicon ingot casting.
Claims (4)
1. the processing method of a discarded silicon material recycling, it is characterised in that comprise the following steps:
A) the discarded silicon material containing impurity is put in container, add alkaline solution；
B) after question response is complete, then in silicon material, add acid solution, control temperature, pressure and response time；
C), after question response is complete, silicon material is put in the mixed acid solution prepared and soaks；
D) finally using pure water that silicon material is carried out repeated ultrasonic rinsing, to rinsing, the pH value of solution is 7；
E) dry.
The processing method of discarded silicon material recycling the most according to claim 1, it is characterised in that: described alkali liquor mass percent concentration is 35%～40%, and alkali cleaning temperature is 40～60 DEG C, and the alkali cleaning time is 20～40min.
The processing method of discarded silicon material recycling the most according to claim 1, it is characterised in that: in described acid solution, the temperature of reaction controls between 60～80 DEG C, and Stress control is between 1～3MPa, and the time controlled between 2～4 hours.
The processing method of discarded silicon material recycling the most according to claim 1, it is characterised in that: described nitration mixture is concentrated sulphuric acid and the mixing of one of which in Fluohydric acid., hydrochloric acid, nitric acid；The weight percent concentration of described various acid is: Fluohydric acid. is 35%～55%, and nitric acid is 68%～98%, and hydrochloric acid is 30%～38%, and concentrated sulphuric acid is more than 90%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510347612.2A CN106315589A (en) | 2015-06-23 | 2015-06-23 | Method for processing recycling waste silicon material |
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| CN201510347612.2A CN106315589A (en) | 2015-06-23 | 2015-06-23 | Method for processing recycling waste silicon material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109137065A (en) * | 2018-10-24 | 2019-01-04 | 镇江环太硅科技有限公司 | One kind is for the silicon material recovery and treatment method that gives up |
| CN115478322A (en) * | 2022-09-26 | 2022-12-16 | 包头美科硅能源有限公司 | Charging method for remelting ultrathin silicon wafer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757051A (en) * | 2012-04-19 | 2012-10-31 | 镇江环太硅科技有限公司 | Method for performing recovery treatment on waste layer silicon material |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757051A (en) * | 2012-04-19 | 2012-10-31 | 镇江环太硅科技有限公司 | Method for performing recovery treatment on waste layer silicon material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109137065A (en) * | 2018-10-24 | 2019-01-04 | 镇江环太硅科技有限公司 | One kind is for the silicon material recovery and treatment method that gives up |
| CN115478322A (en) * | 2022-09-26 | 2022-12-16 | 包头美科硅能源有限公司 | Charging method for remelting ultrathin silicon wafer |
| CN115478322B (en) * | 2022-09-26 | 2023-11-21 | 包头美科硅能源有限公司 | Charging method for re-returning ultrathin silicon wafer to furnace |
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Application publication date: 20170111 |