CN102600988B - 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
- Publication number
- CN102600988B CN102600988B CN 201210060027 CN201210060027A CN102600988B CN 102600988 B CN102600988 B CN 102600988B CN 201210060027 CN201210060027 CN 201210060027 CN 201210060027 A CN201210060027 A CN 201210060027A CN 102600988 B CN102600988 B CN 102600988B
- Authority
- CN
- China
- Prior art keywords
- flotation
- foam
- silicon
- powder
- raw material
- 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.)
- Active
Links
- 238000005188 flotation Methods 0.000 title claims abstract description 95
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000006260 foam Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 31
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000011863 silicon-based powder Substances 0.000 title claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 36
- 239000010703 silicon Substances 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 32
- 238000010306 acid treatment Methods 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000004088 foaming agent Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000005520 cutting process Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 230000005587 bubbling Effects 0.000 claims description 7
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 7
- 239000008158 vegetable oil Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical group OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 4
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 claims description 3
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 239000012991 xanthate Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 2
- 125000004185 ester group Chemical class 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 229910044991 metal oxide Inorganic materials 0.000 description 7
- 150000004706 metal oxides Chemical class 0.000 description 7
- 238000009291 froth flotation Methods 0.000 description 5
- 235000019483 Peanut oil Nutrition 0.000 description 4
- 235000013312 flour Nutrition 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000312 peanut oil Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000008247 solid mixture Substances 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- DIKBFYAXUHHXCS-UHFFFAOYSA-N bromoform Chemical compound BrC(Br)Br DIKBFYAXUHHXCS-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 241001272567 Hominoidea Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229950005228 bromoform Drugs 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- XUIMIQQOPSSXEZ-RNFDNDRNSA-N silicon-32 atom Chemical compound [32Si] XUIMIQQOPSSXEZ-RNFDNDRNSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 description 1
Images
Landscapes
- Silicon Compounds (AREA)
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 surpasses 50% silicon material in silicon chip line cutting process become sawdust and enter slip.The development trend that further attenuate scroll saw is arranged at present, in any case but development, silicon material about 50% becomes sawdust and enters 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 the 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, condensation, dehydration, 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 complexity, 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, by suspending agent and the binding agent in the organic solvent removal waste material, 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 needed bromoform of liquid gravity flotation is very expensive and have toxicity in this process.
Summary of the invention
The technical problem to be solved in the present invention 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 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 battery sheet cutting is as raw material, adds acid in raw material, is 1～3 until the pH of gained reactant liquor value; Filter the back oven dry, get 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 again in the flotation cell of gained is repeated above-mentioned flotation 3～5 times, the solidliquid mixture filtration back of staying in the flotation cell of final gained is dried, get 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 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: raw material (powder that the solar battery sheet cutting produces) is earlier through acid treatment, filtering drying, be made into the certain density aqueous solution with collecting agent and foaming agent again, stir and carry out flotation, foam constantly overflows from flotation cell, till can not overflowing, continues the flotation several times behind the foam nature froth breaking that flotates and (is preferably 4 times, namely 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 and the carborundum purity height of the present invention's acquisition can return use, as raw materials for production, are applicable to suitability for industrialized production.
Description of drawings
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail.
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
In following examples used flotation device as shown in Figure 1, 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 battery sheet cutting is as raw material, this raw material in advance after testing, it is made up of 24% elemental silicon, 40% carborundum and 36% metal oxide.
Annotate: according to " LinBing 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 according to " mensuration of SN/T0256-93 outlet carborundum analytical method-carborundum content ", obtain metal oxide content according to the weight that reduces after the strong acid treatment.
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, with the oven dry of the solid of gained, obtain raw material (being silicon and carborundum hybrid solid) after the 205g acid treatment.
2), select for use vegetable oil (for example being conventional peanut oil) as collecting agent, to select for use lauryl sodium sulfate as foaming agent;
Raw material after 12g collecting agent, 2.5g foaming agent and the 205g acid treatment added be made into the aqueous solution (namely after 0.8L water stirs evenly, 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, connect power supply and begin 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.
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, connect power supply and begin 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 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, get solid; The solid of gained is dried to constant weight in 80 ℃, gets 66.2g to silicon (being that yield is 86.2%), and purity is 92.2%.This purity foundation " LinBing 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 again in the flotation cell of gained is repeated above-mentioned flotation 3 times (process conditions of flotation are the same), with final gained stay solidliquid mixture suction filtration in the flotation cell after, get solid; This solid is dried to constant weight in 80 ℃, gets 108.6g carborundum (being that yield is 84.8%), and 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 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 refers to the weight ratio of raw material after collecting agent and the acid treatment, and the foaming agent consumption refers to the weight ratio of raw material after foaming agent and the acid treatment, and raw material weight concentration refers to 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 battery sheet cutting is as raw material, adds acid in raw material, is 1～3 until the pH of gained reactant liquor value; Filter the back oven dry, get 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 described 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 described collecting agent and the acid treatment, and the weight ratio of raw material is 1～3% after described 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 again in the flotation cell of gained is repeated above-mentioned flotation 3～5 times, the solidliquid mixture filtration back of staying in the flotation cell of final gained is dried, get carborundum.
2. the foam flotation method of divided silicon powder according to claim 1 and silicon carbide powder is characterized in that: described 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, it is characterized in that: described collecting agent is ester class nonionic collecting agent.
4. the foam flotation method of divided silicon powder according to claim 3 and silicon carbide powder, it is characterized in that: described 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: described 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, it is characterized in that: in the aqueous solution described step 2), the weight concentration of raw material is 20～35% after the acid treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210060027 CN102600988B (en) | 2012-03-08 | 2012-03-08 | Foam flotation method for separating silicon powder from silicon carbide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210060027 CN102600988B (en) | 2012-03-08 | 2012-03-08 | Foam flotation method for separating silicon powder from silicon carbide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102600988A CN102600988A (en) | 2012-07-25 |
| CN102600988B true CN102600988B (en) | 2013-08-07 |
Family
ID=46518973
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210060027 Active CN102600988B (en) | 2012-03-08 | 2012-03-08 | Foam flotation method for separating silicon powder from silicon carbide powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102600988B (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103121684B (en) * | 2012-12-07 | 2016-02-24 | 塔里木大学 | A kind of method of Separation and Recovery silicon carbide and silicon from waste mortar for wire cutting |
| CN103623934B (en) * | 2013-11-28 | 2016-02-10 | 安徽苏源光伏科技有限公司 | A kind of silicon carbide purification is separated medicament |
| CN103639062B (en) * | 2013-11-28 | 2016-02-10 | 安徽苏源光伏科技有限公司 | The medicament of separating silicon carbide in a kind of mortar |
| CN103639064B (en) * | 2013-11-28 | 2016-02-10 | 安徽苏源光伏科技有限公司 | A kind of medicament being separated silicon and carborundum in mortar |
| CN103623935B (en) * | 2013-11-28 | 2016-02-10 | 安徽苏源光伏科技有限公司 | A kind of high-purity silicon carbide reclaims flotation agent |
| CN103623937B (en) * | 2013-11-28 | 2016-05-04 | 安徽苏源光伏科技有限公司 | In a kind of mortar, silicon separates medicament and preparation method thereof with carborundum |
| CN103639063B (en) * | 2013-11-28 | 2016-02-10 | 安徽苏源光伏科技有限公司 | A kind of silicon carbide micro-powder reclaims medicament |
| CN103623936B (en) * | 2013-11-28 | 2016-05-04 | 安徽苏源光伏科技有限公司 | A kind of carborundum flotation agent |
| CN103611635B (en) * | 2013-11-28 | 2016-05-04 | 安徽苏源光伏科技有限公司 | The flotation agent of carborundum and preparation method thereof of purifying in a kind of mortar |
| CN106513185B (en) * | 2016-12-12 | 2019-02-05 | 昆明理工大学 | Plasma flotation device |
| 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 |
| CN110775979B (en) * | 2019-12-05 | 2020-09-25 | 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4388080A (en) * | 1982-02-12 | 1983-06-14 | Atlantic Richfield Company | Process for recovery of high purity silicon |
| CN101130237A (en) * | 2007-09-11 | 2008-02-27 | 西安交通大学 | Method for recycling silica powder and carborundum powder from cut waste mortar |
| CN101491888A (en) * | 2009-03-05 | 2009-07-29 | 南昌大学 | Foam flotation method capable of separating silicon powder and carbon silicon powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6838047B2 (en) * | 2001-08-28 | 2005-01-04 | Romain Louis Billiet | MEMS and MEMS components from silicon kerf |
-
2012
- 2012-03-08 CN CN 201210060027 patent/CN102600988B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4388080A (en) * | 1982-02-12 | 1983-06-14 | Atlantic Richfield Company | Process for recovery of high purity silicon |
| CN101130237A (en) * | 2007-09-11 | 2008-02-27 | 西安交通大学 | Method for recycling silica powder and carborundum powder from cut waste mortar |
| CN101491888A (en) * | 2009-03-05 | 2009-07-29 | 南昌大学 | Foam flotation method capable of separating silicon powder and carbon silicon powder |
Non-Patent Citations (4)
| Title |
|---|
| 刑鹏飞等.太阳能级多晶硅切割废料浆的综合回收.《材料导报》.2011,第25卷(第1期),第75页到第79页. |
| 太阳能级多晶硅切割废料浆的综合回收;刑鹏飞等;《材料导报》;20110131;第25卷(第1期);第75页到第79页 * |
| 硅片线锯砂浆中硅粉与碳化硅粉的泡沫浮选分离回收;黄美玲等;《电子元件与材料》;20100430;第29卷(第4期);第74页到第77页 * |
| 黄美玲等.硅片线锯砂浆中硅粉与碳化硅粉的泡沫浮选分离回收.《电子元件与材料》.2010,第29卷(第4期),第74页到第77页. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102600988A (en) | 2012-07-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102600988B (en) | Foam flotation method for separating silicon powder from silicon carbide powder | |
| CN101491888B (en) | Foam flotation method capable of separating silicon powder and carbon silicon powder | |
| CN101623852B (en) | Method separating silicon powder and silicon carbide powder by interface tension | |
| CN101474511B (en) | Process for recovering polyethylene glycol and silicon carbide from silicon wafer wire cutting waste mortar | |
| CN102351184B (en) | Method for recovering silicon carbide, high-purity silicon and dispersion liquid from silicon material linear cutting waste mortar | |
| CN101327622B (en) | Mortar recovery technique for cutting single-crystal and polycrystalline silicon wire | |
| CN102303869B (en) | Method for separating silicon from silicon carbide in silicon wafer wire saw slurry recovery treatment tailing by two-step process | |
| CN110775979B (en) | Method for recovering high-purity silicon and silicon carbide from crystalline silicon cutting waste | |
| CN102173419B (en) | Method for recycling silicon powder from silicon slice cut waste mortar | |
| CN102951641B (en) | Water-saving and environmental protection-type preparation method of silicon carbide micro-powder for silicon wafer wire cutting | |
| CN102730696B (en) | Physical method for recovering cutting liquid, crystal silicon micro-powder and silicon carbide micro-powder from silicon wafer cutting waste mortar | |
| CN102399618B (en) | Method for resource recovery of silicon carbide component from crystal silicon cutting waste mortar | |
| CN101817526B (en) | Method for recovering polyethylene glycol and silicon carbide from silicon crystal cutting waste liquid | |
| CN102502643B (en) | Method for realizing resource recycling of silicon powder components in waste mortar from crystalline silicon cutting | |
| CN103522431B (en) | A kind of silicon chip cutting technique | |
| CN102071092A (en) | Method for recovering and recycling silicon slice cutting waste mortar | |
| CN101850970B (en) | Resource utilization method of silicon wafer cutting and machining mortar at room temperature | |
| CN104176737A (en) | Method for recovering silicon powder from cut mortar waste | |
| CN102659112A (en) | Method for recovering silicon powder from monocrystalline and polycrystalline silicon cutting wastes by utilizing potential adjustment centrifugal process | |
| CN101941699A (en) | Method for reclaiming silicon and silicon carbide from cutting waste materials of monocrystalline silicon and polycrystalline silicon | |
| CN101683981B (en) | Method for recycling waste silicon solution | |
| CN102079520A (en) | Recycling method of silicon carbide | |
| CN102530948A (en) | Method for recycling silicon from filings obtained through silicon wafer cutting | |
| CN102659113B (en) | Method for recovering silicon powder from monocrystalline and polycrystalline silicon linear cutting wastes by utilizing microporous membrane filter process | |
| CN102757856B (en) | Online recovery method for waste mortar produced in silicon wafer cutting |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| ASS | Succession or assignment of patent right |
Owner name: ZHEJIANG UNIVERSITY Effective date: 20130613 Owner name: CCEED INDUSTRIAL EQUIPMENT INSTALLATION CO., LTD. Free format text: FORMER OWNER: ZHEJIANG UNIVERSITY Effective date: 20130613 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Chen Xinzhi Inventor after: Luo Nengzhen Inventor after: Huang Jiamin Inventor after: Xiang Xiangao Inventor after: Xu Yiming Inventor after: Qian Chao Inventor before: Chen Xinzhi Inventor before: Huang Jiamin Inventor before: Qian Chao |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 310027 HANGZHOU, ZHEJIANG PROVINCE TO: 210046 NANJING, JIANGSU PROVINCE Free format text: CORRECT: INVENTOR; FROM: CHEN XINZHI HUANG JIAMIN QIAN CHAO TO: CHEN XINZHI LUO NENGZHEN HUANG JIAMIN XIANG XIANGAO XU YIMING QIAN CHAO |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20130613 Address after: Yaohuamen Yao village in Qixia District of Nanjing City, 210046 new Jiangsu province No. 100 Applicant after: China Construction Industrial Equipment Installation Co., Ltd. Applicant after: Zhejiang University Address before: 310027 Hangzhou, Zhejiang Province, Xihu District, Zhejiang Road, No. 38, No. Applicant before: Zhejiang University |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 210046 Wen Lan Road, Qixia District, Nanjing, Jiangsu Province, No. 6 Co-patentee after: Zhejiang University Patentee after: China Construction Installation Group Co., Ltd. Address before: 210046 No. 100, Yaohua Menyao'an New Village, Qixia District, Nanjing City, Jiangsu Province Co-patentee before: Zhejiang University Patentee before: China Construction Industrial Equipment Installation Co., Ltd. |