CN106809837A - A kind of recovery method of carborundum - Google Patents
A kind of recovery method of carborundum Download PDFInfo
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- CN106809837A CN106809837A CN201510846216.4A CN201510846216A CN106809837A CN 106809837 A CN106809837 A CN 106809837A CN 201510846216 A CN201510846216 A CN 201510846216A CN 106809837 A CN106809837 A CN 106809837A
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Abstract
It is the recovery method to carborundum in siliceous mortar the invention discloses a kind of recovery method of carborundum, siliceous mortar contains carborundum, silicon, impurity and dispersion liquid；The method for reclaiming wherein carborundum is that the siliceous mortar is filtered tentatively to filter the dispersion liquid, obtains silicon mud；To silicon mud be heated to the dispersion liquid volatilization of residual, deimpurity carborundum/silicon mixture is removed in acquisition；Carborundum/silicon mixture is placed in alkaline solution, so that the alkaline solution dissolves the silicon in the carborundum/silicon mixture；And removal obtains purified carborundum dissolved with the alkaline solution of silicon.The method have the advantages that：1. avoid the dispersion liquid in siliceous mortar from going bad；2. avoid using organic solvent to separate carborundum；3. avoid separating carborundum using high speed centrifugation mode.
Description
Technical field
The invention belongs to a kind of recovery method, particularly a kind of recovery method of carborundum.
Background technology
Current silicon chip is widely used to solar industry and electronic industry, and the making of silicon chip is typically to carry out cutting acquisition to silicon crystal bar.Wherein, silicon crystal bar cutting typically uses oily (such as polyethylene glycol of cutting so that cutting tool is adjoint, PEG) silicon crystal bar is cut and slicing slurry is produced so that the compositions such as the cutting loss of carborundum, silicon, cutting oil and cutting element is generally comprised in the slicing slurry.If directly abandoning slicing slurry, environmental pollution is not only caused, will also cause the waste of raw material.Therefore, the recovery correlation technique of carborundum and silicon in relevant unit's input research and development slicing slurry is had at present.
It is currently known the recovery method of carborundum, typically first addition largely separates auxiliary agents (such as water or organic solvent etc.) to dilute slicing slurry in slicing slurry, slicing slurry is filtered with multistage filtering again, the cutting oil of liquid and water is separated with the carborundum and silicon of solid-state.The solid silicon carbide and silicon obtained after filtering are generally separated using following several ways：
1. separating at high temperature：Because the fusing point of carborundum is 2545 DEG C, the fusing point of silicon is 1412 DEG C, therefore using the two
The different characteristic of fusing point, separating at high temperature is carried out with electric furnace, and carborundum is separated with silicon.
However, this method not only consumes energy greatly, and it is seriously polluted, the limitation of TaiWan, China regulation is limited to again, therefore it is more infeasible.
2. heavy-fluid is separated：It is to insert in organic solvent (such as bromofom) of the proportion between carborundum and the proportion of silicon the carborundum and silicon that heavy-fluid is separated, high speed centrifugation is carried out again, so, proportion will float on liquid level less than the silicon of organic solvent, and proportion will be deposited in organic solvent higher than the carborundum of organic solvent, carborundum is separated with silicon, and then obtain the silicon of recyclable recycling.
However, addition of this method due to organic solvent, the toxicity of the organic solvent will cause problem of environmental pollution, and the low flashing point of the organic solvent also easily causes the danger in processing procedure；Again and, ultracentrifugal equipment price is expensive, will also cause the increased shortcoming of cost recovery.
3. froth flotation：This method is added in carborundum and silicon by by interfacial agent, and interfacial agent forms foam, because the interfacial agent is higher to the compatibility of carborundum, therefore can be by silicon carbide absorption in upper strata, and silicon will be precipitated to lower floor, in this way, just carborundum can be separated with silicon.However, the interfacial agent is identical with organic solvent to have the shortcomings that toxicity and low flashing point, will cause this method that there is danger in environmental pollution and processing procedure.
For these reasons, it is necessary further to improve the recovery method of above-mentioned carborundum.
The content of the invention
Shortcoming the invention aims to overcome prior art, there is provided a kind of recovery method of carborundum, to avoid the dispersion liquid in siliceous mortar from going bad；To avoid using organic solvent to separate carborundum；To avoid separating carborundum using high speed centrifugation mode.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
1. a kind of one of recovery method of carborundum, is the recovery method to carborundum in siliceous mortar, and siliceous mortar contains carborundum, silicon, impurity and dispersion liquid；The method and step for reclaiming wherein carborundum is as follows：
1) filter：
By the siliceous mortar filtering comprising carborundum, silicon, impurity and dispersion liquid, the impure carborundum of dispersion liquid/silicon mixture is tentatively filtered；
2) raffinate removal：
Heated to tentatively filtering the impure carborundum of dispersion liquid/silicon mixture, 250 DEG C of temperature ＞ makes the dispersion liquid of residual volatilize, obtain impure carborundum/silicon mixture；
3) pickling impurity removal matter：
In being placed in the leaching of impure carborundum/silicon mixture acid solution or include the acid solution of auxiliary agent, by the impurity in acid leach solution carborundum/silicon mixture, acid solution of the removal dissolved with impurity is refiltered, deimpurity carborundum/silicon mixture is tentatively removed in acquisition；
4) stir
Deimpurity carborundum/silicon mixture will be gone to add pH2.5
Stood in~14 aqueous medium, and after stirring, the carborundum/silicon mixture for obtaining precipitation and the liquid medium for being suspended with silicon isolate the carborundum of precipitation/silicon mixture through filtering, and obtain the carborundum/silicon mixture of initial gross separation silicon；
Liquid medium to being suspended with silicon is filtered, filter liquid medium and obtain silicon, by in silicon addition acid solution, to dissolve the impurity in silicon, after filtering the acid solution dissolved with impurity again, the silicon of purifying is obtained, or carries out electromagnetism high intensity magnetic separation and the silicon of magnetic-particle is coated with to remove, then filter the acid solution to obtain silicon after purification.
5) silicon dissolving：
Deimpurity carborundum/silicon mixture will be gone to be placed in alkaline solution, the silicon in making alkaline solution dissolve the carborundum/silicon mixture obtains alkaline solution and the carborundum precipitation dissolved with silicon；
6) alkali lye removal：
The alkaline solution dissolved with silicon is removed, rinsing carborundum with clear water precipitates, and obtains the carborundum of purifying.
2. the two of a kind of recovery method of carborundum, are the recovery methods to carborundum in siliceous mortar, and siliceous mortar contains carborundum, silicon, impurity and dispersion liquid；The method and step for reclaiming wherein carborundum is as follows：
1) filter：
By the siliceous mortar filtering comprising carborundum, silicon, impurity and dispersion liquid, the impure carborundum of dispersion liquid/silicon mixture is tentatively filtered；
2) raffinate removal：
Heated to tentatively filtering the impure carborundum of dispersion liquid/silicon mixture, 250 DEG C of temperature ＞ makes the dispersion liquid of residual volatilize, obtain impure carborundum/silicon mixture；
3) pickling impurity removal matter：
In being placed in the leaching of impure carborundum/silicon mixture acid solution or include the acid solution of auxiliary agent, by the impurity in acid leach solution carborundum/silicon mixture, acid solution of the removal dissolved with impurity is refiltered, deimpurity carborundum/silicon mixture is tentatively removed in acquisition；
4) stir
Deimpurity carborundum/silicon mixture will be gone to add pH2.5
Stood in~14 aqueous medium, and after stirring, the carborundum/silicon mixture for obtaining precipitation and the liquid medium for being suspended with silicon isolate the carborundum of precipitation/silicon mixture through filtering, and obtain the carborundum/silicon mixture of initial gross separation silicon；
Liquid medium to being suspended with silicon is filtered, filter liquid medium and obtain silicon, by in silicon addition acid solution, to dissolve the impurity in silicon, after filtering the acid solution dissolved with impurity again, the silicon of purifying is obtained, or carries out electromagnetism high intensity magnetic separation and the silicon of magnetic-particle is coated with to remove, then filter the acid solution to obtain silicon after purification.
5) silicon dissolving：
Deimpurity carborundum/silicon mixture will be gone to be placed in alkaline solution, the silicon in making alkaline solution dissolve the carborundum/silicon mixture obtains alkaline solution and the carborundum precipitation dissolved with silicon；
6) alkali lye removal：
The alkaline solution dissolved with silicon is removed, rinsing carborundum with clear water precipitates, and obtains the carborundum of purifying.
3) acid solution described in the pickling impurity removal matter step of the two of the recovery method of one of above-mentioned recovery method of carborundum or carborundum, is hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid or its mixture；Described auxiliary agent is hydrogen peroxide.
Alkaline solution is NaOH, ammoniacal liquor and/or potassium hydroxide aqueous solution described in the silicon dissolving step of the two of the recovery method of one of above-mentioned recovery method of carborundum or carborundum.
In silicon dissolving step described in the two of the recovery method of one of above-mentioned recovery method of carborundum or carborundum, carbon dioxide is passed through in the alkaline solution dissolved with silicon, or add hydrochloric acid, nitric acid, sulfuric acid or/and hydrofluoric acid aqueous solution, so that the silicon in the alkaline solution precipitates to form silica gel because of acidifying, after the silica gel is separated, silica gel is calcined, silica is obtained.
Present invention beneficial effect compared with the prior art is：
1. the recovery method of carborundum of the present invention, using separation auxiliary agent, therefore need not can reduce power consumption and cost recovery, while so that the dispersion liquid for reclaiming will not produce rotten problem and can directly reclaim and use in filtration step.
2. the recovery method of the carborundum of the present invention, the alkaline solution dissolved with silicon that alkali lye removal step is obtained, acidified acquisition silica gel, or carry out filtering roasting again and just can obtain recovery of silica using.
3. the recovery method of carborundum of the present invention, is stirred by the whipping step, the two is carried out initial gross separation using the particle size and difference of specific gravity of carborundum and silicon, therefore need not use such as supercentrifuge expensive device, it is possible to decrease cost recovery；Also the carborundum and silicon need not be separated using organic solvent.And the silicon that is suspended in the liquid medium is also recyclable, material loss is reduced.
Therefore, the recovery method of the carborundum of the present invention can simultaneously reclaim silicon and dispersion liquid carborundum is reclaimed, therefore can reach lifting recycled in its entirety rate, reduce cost recovery and reduce effect of material waste.
Specific embodiment
Embodiment 1
The recovery method of one of the recovery method of carborundum of the present invention carborundum includes filtration step S1, raffinate removal step S2, pickling impurity removal step
S3, silicon dissolving step S4 and alkali lye removal step S5.
1. filtration step S1
(1) the siliceous mortar comprising carborundum, silicon, impurity and dispersion liquid is filtered, is tentatively filtered the carborundum/silicon mixture of dispersion liquid；
In more detail, siliceous mortar is the cutting waste fluid for cutting silicon crystal bar, therefore siliceous mortar includes the composition of carborundum, silicon and dispersion liquid, and the dispersion liquid is general conventional cutting liquid, such as polyethylene glycol (PEG)
Etc. cutting fluid, the impurity such as other impurity, such as chip of the chip produced by cutting element, typically iron filings or other metals may be also included in siliceous mortar.The present embodiment is that the siliceous mortar is filtered, for example, may be selected to filter siliceous mortar with collecting and filtering apparatus or membrane filter, and dispersion liquid is tentatively filtered, and obtains the preliminary carborundum/silicon mixture for filtering dispersion liquid for including carborundum and silicon composition.The carborundum and silicon composition of dispersion liquid and solid-state due to this filtration step S1 only to the liquid carry out preliminary separation of solid and liquid, therefore, additionally addition need not separate auxiliary agent (such as water), cost recovery can not only be reduced, also so that the dispersion liquid for filtering can be reclaimed directly uses, without worry because separate the addition of auxiliary agent and caused by cut the problem of deterioration of oil.
2. raffinate removal step S2
Carborundum/silicon mixture is heated, 250 DEG C of temperature ＞, the dispersion liquid of residual is volatilized, obtain carborundum/silicon mixture；This carborundum/silicon mixture is placed in acid solution, impurity therein is further dissolved, filtered dissolved with impurity acid solution, obtain removal impurity carborundum/silicon mixture.
In more detail, filtration step S1 only tentatively carries out separation of solid and liquid, and still remaining has part dispersion liquid in carborundum/silicon mixture, therefore the dispersion liquid volatilization of residual is further heated to carborundum/silicon mixture and is removed.Illustrate, this is tentatively gone deimpurity carborundum/silicon mixture to be placed in pyrolysis furnace by the present embodiment selection carries out distillation heating with 250 DEG C of temperatures above, make tentatively to go the dispersion liquid of remaining in deimpurity carborundum/silicon mixture to evaporate into pyrolysis furnace top, collected gaseous state dispersion liquid above the pyrolysis furnace can utilize the differential condensation of boiling point to reclaim and use.Carborundum/silicon mixture just can be obtained after carborundum/silicon mixture heating, this carborundum/silicon mixture is placed in acid solution, further dissolve impurity therein, filter the acid solution dissolved with impurity, deimpurity carborundum/silicon mixture is removed in acquisition.
3. pickling impurity removal step S3
In being placed in the leaching of impure carborundum/silicon mixture acid solution or include the acid solution of auxiliary agent, by the impurity in acid leach solution carborundum/silicon mixture, acid solution of the removal dissolved with impurity is refiltered, deimpurity carborundum/silicon mixture is tentatively removed in acquisition.
In more detail, because carborundum/silicon mixture may still contain foregoing impurity, therefore carborundum/silicon mixture is preferably leaching and is placed in acid solution (such as hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid or its mixture etc.), by the impurity in the acid leach solution carborundum/silicon mixture, after removing the acid solution dissolved with impurity again, the acid solution for example is removed with filter type, just can be obtained and tentatively be removed deimpurity carborundum/silicon mixture, then carry out subsequent step.Wherein, the auxiliary agents such as auxiliary agent, such as hydrogen peroxide preferably have been additionally comprised in the acid solution, to improve dissolved efficiency of the acid solution to the impurity.For example, the present embodiment be selection concentration be 3M sulfuric acid and add concentration for 1wt% hydrogen peroxide as the acid leach solution impurity.
3. silicon dissolving step S4
Deimpurity carborundum/silicon mixture will be gone to be placed in alkaline solution, the silicon in making alkaline solution dissolve the carborundum/silicon mixture obtains the carborundum of the alkaline solution and precipitation dissolved with silicon.
In more detail, due to the still composition containing silicon in carborundum/silicon mixture, therefore, be placed in carborundum/silicon mixture in alkaline solution (such as NaOH (NaOH), ammoniacal liquor (NH4OH), potassium hydroxide (KOH) alkaline solution or its mixture) by the present embodiment, by alkaline solution by the silicon composition dissolution in carborundum/silicon mixture.It using concentration is 2M sodium hydrate aqueous solutions as alkaline solution that the present embodiment is so that the silicon composition in carborundum/silicon mixture will be dissolved in sodium hydroxide solution and form sodium silicate solution.
4. alkali lye removal step S5
The alkaline solution dissolved with silicon is removed, the carborundum of precipitation is rinsed with clear water, obtain the carborundum of purifying.
In more detail, after alkaline solution is by silicon dissolution, then alkaline solution is removed, such as the present embodiment is that selection filters alkaline solution dissolved with silicon with filter type, just can obtain carborundum after purification.Wherein, after filtering the alkaline solution dissolved with silicon, the carborundum is rinsed with clear water, to avoid the residual of the alkaline solution.So far, one of recovery method of carborundum of the invention is just completed.
Additionally, being separately acidified by the alkaline solution dissolved with silicon, just can produce precipitation and obtain silica gel.For example, the present embodiment is by being passed through carbon dioxide in the alkaline solution dissolved with silicon, or to add acid solution as the aforementioned, makes the silicon in alkaline solution precipitate to form silica gel because of acidifying, just recyclable after silica gel is separated；Or, further silica gel is washed with a kind of solution of electrolyte (such as the electrolyte such as ammonium chloride or sodium chloride) at least, to avoid acid solution from remaining, and by silica gel through filtering to take out after again with 300 DEG C of temperature carry out roasting 2 hours, just can obtain silica.In this way, the silicon that just will can be dissolved in alkaline solution is converted into silica gel or recovery of silica is used, to avoid the waste of material.
Embodiment 2
The two of the recovery method of carborundum of the present invention
The two of the recovery method of carborundum of the present invention include filtration step S1, raffinate removal step S2, pickling impurity removal step S3, whipping step S21, silicon dissolving step S4, alkali lye removal step S5.
1. filtration step S1 is identical with the filtration step S1 described in embodiment 1.
2. raffinate removal step S2 is identical with the raffinate removal step S2 described in embodiment 1.
3. pickling impurity removal step S3 is identical with the pickling impurity removal step S3 described in embodiment 1.
4. whipping step S21
Deimpurity carborundum/silicon mixture will be gone to add pH2.5
Stood in~14 aqueous medium, and after stirring, the carborundum/silicon mixture for obtaining precipitation and the liquid medium for being suspended with silicon isolate the carborundum of precipitation/silicon mixture through filtering, and obtain the carborundum/silicon mixture of initial gross separation silicon.
In more detail, after completing raffinate removal step S2, the carborundum/silicon mixture is placed in after being stirred in the liquid medium and stood, for example, be placed in the carborundum/silicon mixture in the water of pH2.5~14 by the selection of the present embodiment system, and agitator selects the rotating speed of 100~3000rpm to be stirred.Because the proportion of the carborundum is bigger than silicon, and it is same sex electric charge that the carborundum reaches current potential with the boundary of silicon, therefore, carborundum and least a portion of silicon will repel each other with the surface charge of silicon because of carborundum for the same sex after uniform stirring, so that carborundum can be separated faster with silicon, again and, because the proportion of the carborundum is larger, therefore can with the silicon of part precipitation faster and form carborundum/silicon mixture, and most silicon will be suspended in the liquid medium, again after gravitation settler is separated, just can initial gross separation carborundum and silicon.After the carborundum of the precipitation/silicon mixture is taken out, follow-up silicon dissolving step S4 and alkali lye removal step S5 just can be carried out.
And the liquid medium for being suspended with silicon just can obtain silicon after filtering and filtering liquid medium.For example, the present embodiment is after liquid medium is filtered with membrane filter, just obtains silica flour and used for recovery.Wherein, silicon is cleaned with acid solution again, such as the present embodiment is cleaned with the sulfuric acid solution of 20wt%, further to remove by the acid solution impurity (such as iron filings) in silica gel, cannot be by the acid leach solution by silica flour cladding due to that may there is part to have magnetic impurity, therefore, separately carry out electromagnetism high intensity magnetic separation, cannot dissolved impurity by strong magnetic force magnetic acid solution, such as the present embodiment is cannot dissolved impurity with the high-intensity magnetic field magnetic of 2T (Fesla) intensity acid solution, to lift the removal effect of impurity in the silicon, just the silicon of high-purity can be obtained, used for reclaiming silicon.
1. silicon dissolving step S4 is identical with the silicon dissolving step S4 described in embodiment 1.
5. alkali lye removal step S5 is identical with the alkali lye removal step S5 described in embodiment 1.
Although the present invention has utilized above-mentioned preferred embodiment to disclose; but; it is not limited to the present invention, and any to be familiar with this those skilled in the art and do not departing within the spirit and scope of the present invention, carry out various changes with respect to above-described embodiment still belongs to the technology category that the present invention is protected with modification.
Claims (5)
1. a kind of recovery method of carborundum, it is characterised in that be the recovery method to carborundum in siliceous mortar, siliceous mortar contains carborundum, silicon, impurity and dispersion liquid；The method and step for reclaiming wherein carborundum is as follows：
1) filter：
By the siliceous mortar filtering comprising carborundum, silicon, impurity and dispersion liquid, the impure carborundum of dispersion liquid/silicon mixture is tentatively filtered；
2) raffinate removal：
Heated to tentatively filtering the impure carborundum of dispersion liquid/silicon mixture, temperature ＞
250 DEG C, the dispersion liquid of residual is volatilized, obtain impure carborundum/silicon mixture；
3) pickling impurity removal matter：
In being placed in the leaching of impure carborundum/silicon mixture acid solution or include the acid solution of auxiliary agent, by acid leach solution carborundum/
Impurity in silicon mixture, refilters acid solution of the removal dissolved with impurity, and deimpurity carborundum/silicon mixture is tentatively removed in acquisition；
4) silicon dissolving：
Deimpurity carborundum/silicon mixture will be gone to be placed in alkaline solution, the silicon in making alkaline solution dissolve the carborundum/silicon mixture obtains alkaline solution and the carborundum precipitation dissolved with silicon；
5) alkali lye removal：
The alkaline solution dissolved with silicon is removed, the carborundum of purifying is obtained.
2. a kind of recovery method of carborundum, it is characterised in that be the recovery method to carborundum in siliceous mortar, siliceous mortar contains carborundum, silicon, impurity and dispersion liquid；The method and step for reclaiming wherein carborundum is as follows：
1) filter：By the siliceous mortar filtering comprising carborundum, silicon, impurity and dispersion liquid, the impure carborundum of dispersion liquid/silicon mixture is tentatively filtered；
2) raffinate removal：
Heated to tentatively filtering the impure carborundum of dispersion liquid/silicon mixture, temperature ＞
250 DEG C, the dispersion liquid of residual is volatilized, obtain impure carborundum/silicon mixture；
3) pickling impurity removal matter：
In being placed in the leaching of impure carborundum/silicon mixture acid solution or include the acid solution of auxiliary agent, by acid leach solution carborundum/
Impurity in silicon mixture, refilters acid solution of the removal dissolved with impurity, and deimpurity carborundum/silicon mixture is tentatively removed in acquisition；
4) stir
To go in the aqueous medium of deimpurity carborundum/silicon mixture addition pH2.5~14, and stood after stirring, carborundum/silicon the mixture for obtaining precipitation and the liquid medium for being suspended with silicon, the carborundum of precipitation/silicon mixture is isolated through filtering, obtains the carborundum/silicon mixture of initial gross separation silicon；
Liquid medium to being suspended with silicon is filtered, filter liquid medium and obtain silicon, by in silicon addition acid solution, to dissolve the impurity in silicon, after filtering the acid solution dissolved with impurity again, the silicon of purifying is obtained, or carries out electromagnetism high intensity magnetic separation and the silicon of magnetic-particle is coated with to remove, then filter the acid solution to obtain silicon after purification；
5) silicon dissolving：
Deimpurity carborundum/silicon mixture will be gone to be placed in alkaline solution, the silicon in making alkaline solution dissolve the carborundum/silicon mixture obtains alkaline solution and the carborundum precipitation dissolved with silicon；6) alkali lye removal：The alkaline solution dissolved with silicon is removed, rinsing carborundum with clear water precipitates, and obtains the carborundum of purifying.
3. the recovery method of the carborundum according to claim 1 or claim 2, it is characterised in that the 3) acid solution described in pickling impurity removal matter step, is hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid or its mixture；Described auxiliary agent is hydrogen peroxide.
4. the recovery method of the carborundum according to claim 1 or claim 2, it is characterised in that alkaline solution described in silicon dissolving step is NaOH, ammoniacal liquor and/or potassium hydroxide aqueous solution.
5. the recovery method of the carborundum according to claim 1 or claim 2, it is characterized in that, silicon dissolving step Hou, carbon dioxide is passed through in the alkaline solution dissolved with silicon, or addition hydrochloric acid, nitric acid, sulfuric acid or/and hydrofluoric acid aqueous solution, so that the silicon in the alkaline solution precipitates to form silica gel because of acidifying, after the silica gel is separated, silica gel is carried out into roast, silica is obtained.
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Application publication date: 20170609 |