CN102600988A - Foam flotation method for separating silicon powder from silicon carbide powder - Google Patents
Foam flotation method for separating silicon powder from silicon carbide powder Download PDFInfo
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- CN102600988A CN102600988A CN2012100600270A CN201210060027A CN102600988A CN 102600988 A CN102600988 A CN 102600988A CN 2012100600270 A CN2012100600270 A CN 2012100600270A CN 201210060027 A CN201210060027 A CN 201210060027A CN 102600988 A CN102600988 A CN 102600988A
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Abstract
The invention discloses a foam flotation method for separating silicon powder from silicon carbide powder. The foam flotation method includes the steps: 1) using powder generated in cutting of a solar cell as raw materials and obtaining raw materials after acid treatment; 2) adding water into collecting agents, foaming agents and the raw materials after acid treatment to prepare water solution, filling the water solution into a flotation tank for flotation, collecting spilling foam and reserving solid-liquid mixture in the flotation tank; 3) performing flotation again after the foam collected in the step 2 naturally disappears and changes into liquid, and drying the finally obtained foam after suction filtration to obtain silicon; and 4) performing flotation for the solid-liquid mixture reserved in the flotation tank in the step 2 again, and filtering and then drying the solid-liquid mixture finally reserved in the flotation tank to obtain silicon carbide.
Description
Technical field
The present invention relates to the froth flotation isolation technics of silicon and carborundum in the powder that the cutting of a kind of solar battery sheet produces.
Background technology
Solar battery sheet generally adopts the steel wire scroll saw to cooperate the cutting of silicon carbide abrasive slurry to produce; The scroll saw silk directly is generally 0.18mm; The kerf width that produces is generally 0.20～0.30mm; And the thickness of current silicon chip of solar cell is 0.18～0.22mm, and this meaning silicon material above 50% in silicon chip line cutting process becomes sawdust entering slip.The development trend that further attenuate scroll saw is arranged at present, in any case but development, silicon material about 50% becomes sawdust entering slip in the photovoltaic industry, therefore extracts to reclaim to equal to open up a kind of new considerable HIGH-PURITY SILICON raw material sources of scale.
In order to reduce the solar cell cost, some researchs have been done in the recycling of scrap wire saw mortar both at home and abroad, following correlation technique patent is to reporting silicon and separating of carborundum:
1, patent CN 101491888 has reported that foam flotation method separates silicon and carborundum in the mortar; Wherein adopting ethanol, methyl alcohol, water, diesel oil, kerosene etc. is solvent, and APES, OPEO, oleic acid, terpinol etc. are surface modifier.Because the physico-chemical property of silicon and carborundum is close, finds suitable surfactant that very big difficulty is arranged, the separating effect of the surfactant of this patent report is general.
2, the processing recovery method of a kind of monocrystalline silicon cutting waste liquor of patent CN 101113029 reports.(1) this waste liquid is handled with watery hydrochloric acid, and mixed into runny compound; (2) Separation of Solid and Liquid is carried out in compound heating, and water and polyethylene glycol steam together, and condensation is dewatered, reclaim polyethylene glycol, separate solid be the thick solid mixture of carborundum and silicon; (3) after should thick solid mixture water carrying out secondary cleaning, obtain the secondary cleaning solid mixture of carborundum and silicon; (4) then use HN0
3The mix acid liquor that+HF forms is handled, and obtains silicon and carborundum.With the pickling meeting silica flour is dissolved in the 4th step, obtain silicate fluoride solution, can not obtain high purity silicon.And this process is complicated, and carborundum is effective for reclaiming, but improper for reclaiming silicon the method.
3, a kind of process of from the waste mortar of monocrystalline silicon cutting or the generation of grinding silicon wafer, extracting high-purity silica flour and carborundum powder of patent CN 100528488 reports; Remove suspending agent and binding agent in the waste material through organic solvent; Solid-state sand material is carried out gas flotation; Obtain the silicon of certain purity, further this silica flour is carried out liquid floatation and gravity separation again, last pickling obtains highly purified silica flour.Reagent such as the needed bromoform of liquid gravity flotation is very expensive and have toxicity in this process.
Summary of the invention
The technical problem that the present invention will solve provides that a kind of toxicity is low, cost is low, the froth flotation separation method of simple and rapid silicon and carborundum.
In order to solve the problems of the technologies described above, the present invention provides the foam flotation method of a kind of divided silicon powder and silicon carbide powder, may further comprise the steps:
1), the powder that produces with solar cell sheet cutting is as raw material, in raw material, adds acid, is 1～3 until the pH of gained reactant liquor value; Filter the back oven dry, raw material after the acid treatment;
This raw material is formed (content of impurity is very little, ignores) by silicon, carborundum and metal oxide.The content of silicon is generally 19%～32%, the content of carborundum is generally 40%～48%, and the content of metal oxide is generally 26%～36%, and above-mentioned % is weight %;
2), raw material after collecting agent, foaming agent and the acid treatment added water be made into the aqueous solution, the flotation cell of the aqueous solution being put into flotation device carries out flotation, does not stop flotation until there being foam to overflow, and collects the foam that overflows, and leaves solidliquid mixture in the flotation cell; The weight ratio of raw material is 5～10% after collecting agent and the acid treatment, and the weight ratio of raw material is 1～3% after foaming agent and the acid treatment;
3), treat step 2) the foam nature froth breaking of collecting gained carries out flotation after becoming liquid again, do not stop flotation until there being foam to overflow; The foam that collection is overflowed repeats behind the above-mentioned froth breaking flotation (being to carry out flotation again after the nature froth breaking becomes liquid) 3～5 times, dries behind the foam suction filtration of final gained, obtains silicon;
4), with step 2) solidliquid mixture of staying in the flotation cell of gained carries out flotation, do not stop flotation until there being foam to overflow; The solidliquid mixture of staying once more in the flotation cell of gained is repeated above-mentioned flotation 3～5 times, and the solidliquid mixture filtration back oven dry in the flotation cell of staying with final gained gets carborundum.
Improvement as the foam flotation method of divided silicon powder of the present invention and silicon carbide powder: step 2), 3) and 4) in flotation be: rotating speed is 1600～2000r/min, and the bubbling flow is 80～180m
3/ h.
Further improvement as the foam flotation method of divided silicon powder of the present invention and silicon carbide powder: collecting agent is an ester class nonionic collecting agent, for example is O-isopropyl-N-ethyl thionic carbamate, xanthate or vegetable oil.
Further improvement as the foam flotation method of divided silicon powder of the present invention and silicon carbide powder: foaming agent is lauryl sodium sulfate or neopelex.
Further improvement as the foam flotation method of divided silicon powder of the present invention and silicon carbide powder: in aqueous solution step 2), the weight concentration of raw material is 20～35% after the acid treatment.
Further improvement as the foam flotation method of divided silicon powder of the present invention and silicon carbide powder: the acid in the step 1) is that mass concentration is 5～15% strong acid solution; Strong acid for example is sulfuric acid, hydrochloric acid etc.
Invention process of the present invention is summarized as follows: earlier through acid treatment, filtering drying is made into the certain density aqueous solution with collecting agent and foaming agent to raw material (powder that the solar battery sheet cutting produces) again; Stir and carry out flotation; Foam constantly overflows from flotation cell, and till can not overflowing, the foam nature froth breaking continued flotation several times that flotate (are preferably 4 times; Promptly altogether 5 times), obtain highly purified silicon at last; Lower floor's thing is continued flotation several times (being preferably 4 times), obtain highly purified carborundum at last.
Method of the present invention has following advantage:
(1) the invention provides that a kind of toxicity is low, cost is low, simple and rapid separation method.
(2) silicon of the present invention's acquisition and carborundum purity are high, can return use, as raw materials for production, are applicable to suitability for industrialized production.
Description of drawings
Do further explain below in conjunction with the accompanying drawing specific embodiments of the invention.
Fig. 1 is the structure chart of the froth flotation machine that uses of the present invention;
Left side figure is the right view of froth flotation machine, and right figure is the front view of froth flotation machine.
1 is rotational speed governor, and 2 is agitating device, and 3 is flotation cell, and 4 is pallet, and 5 is motor, and 6 is switch, and 7 is flowmeter.
The specific embodiment
Flotation device used in following examples is as shown in Figure 1, and this flotation device is conventional commercial product, for example can adopt the permanent happy XFD flotation device of producing in Wuhan.
Following % is weight %.
The foam flotation method of embodiment 1, a kind of divided silicon powder and silicon carbide powder may further comprise the steps:
1), the powder that produces with solar cell sheet cutting is as raw material, this raw material is in advance through detecting, it is made up of 24% elemental silicon, 40% carborundum and 36% metal oxide.
Annotate: according to " Lin Ping Xi; Yang Hong etc. the volatilization of elemental silicon and mensuration in the industrial silicon. metallurgical analysis; 2008; 28 (7): the method for the mensuration elementary silicon among the 62-64 " record silicone content, record carborundum content, obtain metal oxide content according to the weight that reduces after the strong acid treatment according to " mensuration of SN/T0256-93 outlet carborundum analytical method-carborundum content ".
Utilize balance to weigh the 320g raw material, in raw material, slowly add hydrochloric acid solution (mass concentration 15%), and measure the pH value at any time, present acidity (being that pH is less than 7) until reactant liquor, and then excessive dripping hydrochloric acid solution (about 10mL), that is, be 2 thereby regulate the pH value.Think that the metal oxide in the raw material has been reacted this moment.
Above-mentioned reacted product is carried out suction filtration,, obtain raw material (being silicon and carborundum hybrid solid) after the 205g acid treatment the oven dry of the solid of gained.
2), select for use vegetable oil (for example being conventional peanut oil), to select for use lauryl sodium sulfate as foaming agent as collecting agent;
Raw material after 12g collecting agent, 2.5g foaming agent and the 205g acid treatment added be made into the aqueous solution (promptly after 0.8L water stirs; The weight concentration of raw material in the aqueous solution is 20.1% after the acid treatment); The flotation cell (flotation cell is fixed on the flotation device) of the aqueous solution being put into flotation device carries out flotation, and energized begins flotation, does not stop flotation until there being foam to overflow powered-down; The rotating speed that flotation device is set is 1800r/min, and the bubbling flow is 100m
3/ h.
The foam that collection is overflowed leaves solidliquid mixture in the flotation cell.Both carry out following processing respectively for this.
3), step 2) after the foam of collecting gained treats its natural froth breaking, carry out flotation again, specific as follows: as to pour in second flotation cell; Energized begins flotation; Do not stop flotation until there being foam to overflow powered-down, the rotating speed that flotation device is set is 1800r/min, and the bubbling flow is 100m
3/ h.
Collected foam is repeated the flotation 3 times (process conditions of flotation are the same) behind the above-mentioned natural froth breaking, behind the foam suction filtration of final flotation gained, solid; The solid of gained is dried to constant weight in 80 ℃, 66.2g to silicon (being that yield is 86.2%), purity is 92.2%.This purity foundation " Lin Ping Xi, Yang Hong etc. the volatilization of elemental silicon and mensuration in the industrial silicon. metallurgical analysis, 2008,28 (7): the method for the mensuration elementary silicon among the 62-64 " detect.
In this step, the residue that remains in the trace in the flotation cell in the floatation process is done discarded the processing.
4), with step 2) the solidliquid mixture in the flotation cell stayed of gained pours second flotation cell into and carries out flotation, do not stop flotation until there being foam to overflow; The rotating speed that flotation device is set is 1800r/min, and the bubbling flow is 100m
3/ h.
The solidliquid mixture of staying once more in the flotation cell of gained is repeated above-mentioned flotation 3 times (process conditions of flotation are the same), with final gained stay the solidliquid mixture suction filtration in the flotation cell after, solid; This solid is dried to constant weight in 80 ℃, 108.6g carborundum (being that yield is 84.8%), purity is 90.3%.This purity detects according to " mensuration of SN/T0256-93 outlet carborundum analytical method-carborundum content ".
Weight concentration, the rotating speed of flotation device and the rotating speed and the bubbling flow homogeneous of the flotation device in bubbling flow (step 2), step 3) and the step 4) of raw material cause in the kind of the kind of the collecting agent among the change embodiment 1 and consumption thereof, foaming agent and consumption thereof, the aqueous solution); All the other steps obtain embodiment 2～embodiment 19 respectively with embodiment 1.
The material composition of embodiment 2～7 is with embodiment 1.
The material composition of embodiment 8～13 is specific as follows: silicon 32%, carborundum 42%, metal oxide 26%.
The material composition of embodiment 14～19 is specific as follows: silicon 19%, carborundum 48%, metal oxide 33%.
The silicon of gained and the purity of carborundum and yield are as shown in table 1.
Table 1
Annotate:
1. O-isopropyl-N-ethyl thionic carbamate, xanthate, vegetable oil as collecting agent in the above-mentioned table 1 be numbered respectively, 2., 3.; Lauryl sodium sulfate, neopelex as foaming agent are numbered a, b respectively.Collector dosage is meant the weight ratio of raw material after collecting agent and the acid treatment, and the foaming agent consumption is meant the weight ratio of raw material after foaming agent and the acid treatment, and raw material weight concentration is meant the weight concentration of aqueous acid medium raw materials treated.
Comparative Examples 1, make the 12g among the embodiment 1 into oleic acid 12g as the vegetable oil of collecting agent (for example being conventional peanut oil), all the other are equal to embodiment 1.
Silicon yield 69.2%, purity are 80.2; Carborundum yield 70.5%, purity 78.2.
Comparative Examples 2, make the 12g among the embodiment 1 into oleic acid 24g as the vegetable oil of collecting agent (for example being conventional peanut oil), all the other are equal to embodiment 1.
Silicon yield 74.8%, purity are 81.3; Carborundum yield 73.9%, purity 78.9.
Comparative Examples 3, make the 12g among the embodiment 1 into OPEO 12g as the vegetable oil of collecting agent (for example being conventional peanut oil), all the other are equal to embodiment 1.
Silicon yield 65.7%, purity are 80.1; Carborundum yield 69.1%, purity 78.7.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (6)
1. the foam flotation method of divided silicon powder and silicon carbide powder is characterized in that may further comprise the steps:
1), the powder that produces with solar cell sheet cutting is as raw material, in raw material, adds acid, is 1～3 until the pH of gained reactant liquor value; Filter the back oven dry, raw material after the acid treatment;
2), raw material after collecting agent, foaming agent and the acid treatment added water be made into the aqueous solution, the flotation cell of the said aqueous solution being put into flotation device carries out flotation, does not stop flotation until there being foam to overflow, and collects the foam that overflows, and leaves solidliquid mixture in the flotation cell; The weight ratio of raw material is 5～10% after said collecting agent and the acid treatment, and the weight ratio of raw material is 1～3% after said foaming agent and the acid treatment;
3), treat step 2) the foam nature froth breaking of collecting gained carries out flotation after becoming liquid again, do not stop flotation until there being foam to overflow; The foam that collection is overflowed repeats behind the above-mentioned froth breaking flotation 3～5 times, dries behind the foam suction filtration of final gained, obtains silicon;
4), with step 2) solidliquid mixture of staying in the flotation cell of gained carries out flotation again, do not stop flotation until there being foam to overflow; The solidliquid mixture of staying once more in the flotation cell of gained is repeated above-mentioned flotation 3～5 times, and the solidliquid mixture filtration back oven dry in the flotation cell of staying with final gained gets carborundum.
2. the foam flotation method of divided silicon powder according to claim 1 and silicon carbide powder is characterized in that: said step 2), 3) and 4) in flotation be: rotating speed is 1600～2000r/min, and the bubbling flow is 80～180m
3/ h.
3. the foam flotation method of divided silicon powder according to claim 2 and silicon carbide powder is characterized in that: said collecting agent is an ester class nonionic collecting agent.
4. the foam flotation method of divided silicon powder according to claim 3 and silicon carbide powder is characterized in that: said ester class nonionic collecting agent is O-isopropyl-N-ethyl thionic carbamate, xanthate or vegetable oil.
5. according to the foam flotation method of claim 3 or 4 described divided silicon powders and silicon carbide powder, it is characterized in that: said foaming agent is lauryl sodium sulfate or neopelex.
6. the foam flotation method of divided silicon powder according to claim 5 and silicon carbide powder is characterized in that: in the aqueous solution said step 2), the weight concentration of raw material is 20～35% after the acid treatment.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103121684A (en) * | 2012-12-07 | 2013-05-29 | 塔里木大学 | Method for separating and recovering silicon carbide and silicon from linear cutting waste mortar |
| CN103611635A (en) * | 2013-11-28 | 2014-03-05 | 安徽苏源光伏科技有限公司 | Flotation agent for purifying silicon carbides from mortar and preparing method thereof |
| CN103623937A (en) * | 2013-11-28 | 2014-03-12 | 安徽苏源光伏科技有限公司 | Agent for separating silicon and silicon carbide in mortar and preparation method thereof |
| CN103623934A (en) * | 2013-11-28 | 2014-03-12 | 安徽苏源光伏科技有限公司 | Silicon carbide purification and separation agent and preparation method of silicon carbide purification and separation agent |
| CN103623936A (en) * | 2013-11-28 | 2014-03-12 | 安徽苏源光伏科技有限公司 | Silicon carbide flotation agent and preparation method of silicon carbide flotation agent |
| CN103623935A (en) * | 2013-11-28 | 2014-03-12 | 安徽苏源光伏科技有限公司 | High-purity silicon carbide recovery floatation agent and preparing method thereof |
| CN103639063A (en) * | 2013-11-28 | 2014-03-19 | 安徽苏源光伏科技有限公司 | Silicon carbide micro-powder recycling agent and preparation method thereof |
| CN103639062A (en) * | 2013-11-28 | 2014-03-19 | 安徽苏源光伏科技有限公司 | Medicament for separating silicon carbide from mortar and preparation method thereof |
| CN103639064A (en) * | 2013-11-28 | 2014-03-19 | 安徽苏源光伏科技有限公司 | Medicament for separating silicon and silicon carbide in mortar and preparation method thereof |
| CN106513185A (en) * | 2016-12-12 | 2017-03-22 | 昆明理工大学 | Plasma flotation machine |
| CN109663672A (en) * | 2019-01-15 | 2019-04-23 | 国网山东省电力公司电力科学研究院 | A kind of flotation agent and method for floating for isolating pure silicon from smelting product |
| CN110775979A (en) * | 2019-12-05 | 2020-02-11 | 中国科学院合肥物质科学研究院 | Method for recovering high-purity silicon and silicon carbide from crystalline silicon cutting waste |
| CN111342036A (en) * | 2020-03-25 | 2020-06-26 | 江苏新效新材料科技有限公司 | Method for removing aluminum element from silicon cutting waste residue |
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