CN203128312U - Polycrystalline silicon waste water treatment device - Google Patents
Polycrystalline silicon waste water treatment device Download PDFInfo
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- CN203128312U CN203128312U CN2012207440653U CN201220744065U CN203128312U CN 203128312 U CN203128312 U CN 203128312U CN 2012207440653 U CN2012207440653 U CN 2012207440653U CN 201220744065 U CN201220744065 U CN 201220744065U CN 203128312 U CN203128312 U CN 203128312U
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 28
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 86
- 238000000926 separation method Methods 0.000 claims abstract description 50
- 239000000919 ceramic Substances 0.000 claims abstract description 48
- 239000012530 fluid Substances 0.000 claims abstract description 34
- 238000003860 storage Methods 0.000 claims abstract description 6
- 239000012528 membrane Substances 0.000 claims description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229910001868 water Inorganic materials 0.000 claims description 19
- 229920005591 polysilicon Polymers 0.000 claims description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 239000001110 calcium chloride Substances 0.000 claims description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000002699 waste material Substances 0.000 abstract description 29
- 230000008901 benefit Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 5
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 44
- 229910010271 silicon carbide Inorganic materials 0.000 description 41
- 239000002202 Polyethylene glycol Substances 0.000 description 38
- 229920001223 polyethylene glycol Polymers 0.000 description 38
- 239000007787 solid Substances 0.000 description 21
- 239000002245 particle Substances 0.000 description 19
- 238000000034 method Methods 0.000 description 18
- 238000005406 washing Methods 0.000 description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 16
- 238000011084 recovery Methods 0.000 description 15
- 239000012535 impurity Substances 0.000 description 14
- 239000000203 mixture Substances 0.000 description 14
- 229910052710 silicon Inorganic materials 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 230000001276 controlling effect Effects 0.000 description 8
- 238000005520 cutting process Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- 238000004064 recycling Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000002173 cutting fluid Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
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- 238000001556 precipitation Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004590 computer program Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
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- 235000012431 wafers Nutrition 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The utility model discloses a polycrystalline silicon waste water treatment device which comprises a ceramic film system, wherein the ceramic film system comprises a material liquid box, a material supply pump, a circulating pump, a ceramic film, a permeating liquid box and a plurality of connection pipelines, wherein pressure adjustment valves and/or instruments are also arranged on the connection pipelines; the polycrystalline silicon waste water treatment device is also connected with a liquid separator through a pipeline and comprises a separation cavity and a fluid storage tank and a flow supply pump which are connected with the separation cavity; and the flow supply pump is arranged between the separation cavity and the fluid storage box. The polycrystalline silicon waste water treatment device can convert original pollutants into industrial resources and recycle and use the industrial resources; waste is turned into treasures; and the polycrystalline silicon waste water treatment device has extremely high economical value and environmental benefits.
Description
Technical Field
The utility model relates to a wastewater treatment device, concretely relates to polycrystalline silicon wastewater treatment device belongs to waste water recovery and utilization field.
Background
The silicon is used as an important photoelectric material and a semiconductor material, the strategic resource position is increasingly obvious, and the global demand is continuously increased. In the photoelectric and semiconductor industries, a single silicon body needs to be cut into silicon wafers meeting requirements, at present, a multi-wire cutting technology is mainly adopted for polycrystalline silicon, about 50% of silicon materials are mixed into cutting fluid consisting of polyethylene glycol (PEG) cutting fluid and silicon carbide powder (SiC) grinding materials in the cutting process, so that the composition, the particle size and the hardness of micro powder in the cutting fluid do not meet the standard, the cutting performance is reduced, the micro powder cannot be recycled, old cutting fluid needs to be continuously discharged in the cutting process, new cutting fluid needs to be continuously supplemented, and a large amount of cutting waste liquid is generated.
The cutting waste liquid is black viscous suspension, and the main component and content are 40-50% of polyethylene glycol (PEG); 23 to 33 percent of silicon carbide (SiC), 20 to 24 percent of silicon (Si) and 2.5 to 3.0 percent of scrap iron (Fe). The PEG is prepared by extracting PEG from petroleum and polymerizing, has stable molecular structure, is not easy to decompose, is very easy to dissolve in water, has low biological oxygen consumption, is not easy to degrade in nature, has COD (chemical oxygen demand) value greatly exceeding the wastewater discharge standard, and causes huge pollution if the PEG flows into the natural environment without special treatment. SiC and Si are important industrial raw materials and belong to non-renewable resources. Huge energy is consumed in the process of producing the SiC raw material, and the state limits the new industrial project. The Si is high-purity silicon powder cut and ground, and if the silicon powder is directly discharged, environmental pollution and waste of silicon materials are caused.
At present, two ideas exist for the treatment of the wastewater: one is to discharge after the treatment reaches the standard. Common methods comprise a microbiological method, an advanced oxidation method and the like, and for the important PEG-containing wastewater, the microbiological method has the disadvantages of complex process, low treatment efficiency and poor treatment effect, and can hardly reach the standard; the advanced oxidation method has good treatment effect, but has high operation cost and complex process control; other common sewage treatment methods are difficult to be applied; the other idea is to recycle the waste liquid by stages, because PEG, SiC and Si in the waste liquid are important industrial raw materials, wherein the market price of polyethylene glycol (PEG) is 12 yuan per kilogram, the market price of SiC is 24 yuan per kilogram, and the market price of Si is 140 yuan per kilogram. Therefore, the classified recovery and utilization of the silicon cutting waste liquid have important significance for saving resources, protecting the environment and improving economic benefits, relatively mature treatment and recovery technologies exist abroad, the technology in the aspect of China is immature, and most of the technology is in the research stage.
The domestic existing treatment and recovery technology comprises the following steps: a photovoltaic wastewater zero discharge process (CN 102557291A), the system flow is too long, the process is complex, the investment is too large, and the practical application of the project is difficult to realize; a method for treating wastewater containing polyethylene glycol (CN 1023722388A) adopts flocculation precipitation and Fendon oxidation technologies, the treated wastewater needs to enter a wastewater treatment plant for treatment, the use cost is high, and the method is not suitable for the treatment of polysilicon wastewater; the patent device adopts centrifugal solid-liquid separation, only recovers silicon carbide in waste liquid, polyethylene glycol and silicon with higher recovery value are not involved;
the main problems of the existing recovery technology are that: the solid-liquid separation effect is not good, and multi-stage separation is often needed, such as: centrifugal separation, inclined plate precipitation, filtration, filter pressing and the like, wherein the separated PEG liquid contains part of light impurities and can be recycled only by further purification; secondly, the SiC and Si separation process is complex and has poor effect, a plurality of chemical agents are needed to be used or a plurality of physical processes are needed, and a simple and effective separation device is lacked.
Disclosure of Invention
The utility model aims to solve the technical problem that the efficient is treated the retrieval and utilization technique, can thoroughly solve the not good problem of solid-liquid separation effect, for this reason, provide a polycrystalline silicon effluent treatment plant.
The utility model provides a technical scheme as follows that above-mentioned technical problem took:
a polysilicon wastewater treatment device comprises: a ceramic membrane system;
the ceramic membrane system comprises a feed liquid tank, a feed pump, a circulating pump, a ceramic membrane, a permeation liquid tank and a plurality of connecting pipelines, wherein the upper opening of the feed liquid tank is connected with the circulating pump through the connecting pipelines, the lower end of the feed liquid tank is connected with the feed pump, the feed pump is connected with the connecting pipelines between the circulating pump and the upper opening of the feed liquid tank through the connecting pipelines, the circulating pump is connected with the ceramic membrane through the connecting pipelines, the ceramic membrane is connected with the upper opening of the permeation liquid tank through the connecting pipelines, and a pressure regulating valve and/or an instrument are/is further arranged on the connecting pipelines.
Further, preferably, the ceramic membrane has a tubular multi-stage bent hollow structure, and the membrane pores are smaller than 1 μm.
Further, it is preferable that the ceramic membrane is made of titanium dioxide and zirconia frit.
Further, it is preferable that a liquid separator is further connected through the pipe, including:
the device comprises a separation cavity, a fluid storage tank connected with the separation cavity, and a flow supply pump, wherein the flow supply pump is arranged between the separation cavity and the fluid storage tank.
Further, it is preferred that the liquid inlet of the separation chamber opens at a position below the separation chamber.
Further, it is preferable that the liquid is pure water or calcium chloride or a sodium chloride solution.
After the above technical scheme is adopted in the utility model, following superiority has:
firstly, the original waste liquid is directly pressurized and separated without any treatment, no chemicals are added, the purity of the separated PEG reaches 99.7 percent, the process is simple and reliable, the PEG separation and purification process can be completed once, and the PEG recovery rate reaches 92 percent;
the innovative SiC and Si fluid separator technology is simple to operate and has good separation effect, the Si recovery rate can reach 85% at most, and the SiC recovery rate is over 90%. Since the SiC and Si mixture of the separation interface can be continuously separated in the next separation, the separation rate is theoretically higher the more separation times.
The utility model discloses the waste liquid changing waste into valuables that will need to handle has not only realized "zero" emission of pollutant, has very high economic benefits again simultaneously.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
The present invention will be described in detail with reference to the accompanying drawings so that the above advantages of the present invention can be more clearly understood. Wherein,
FIG. 1 is a schematic flow chart of a polysilicon wastewater treatment device according to the present invention;
FIG. 2 is a schematic structural diagram of a ceramic membrane system of the polysilicon wastewater treatment device of the present invention;
FIG. 3 is a schematic structural view of the fluid separator of the polysilicon wastewater treatment apparatus of the present invention.
Detailed Description
The following detailed description will be made with reference to the accompanying drawings and examples, so as to solve the technical problems by applying technical means to the present invention, and to fully understand and implement the technical effects of the present invention. It should be noted that, as long as no conflict is formed, the embodiments and the features in the embodiments of the present invention may be combined with each other, and the technical solutions formed are all within the scope of the present invention.
Additionally, the steps illustrated in the flow charts of the figures may be performed in a computer system such as a set of computer-executable instructions and, although a logical order is illustrated in the flow charts, in some cases, the steps illustrated or described may be performed in an order different than here.
As shown in FIG. 1, the polysilicon wastewater treatment device comprises the following steps:
(1) pressurizing the polycrystalline silicon waste liquid, then feeding the polycrystalline silicon waste liquid into a ceramic membrane system, carrying out solid-liquid separation under the pressure of 0.20MPa-0.55MPa, separating out polyethylene glycol liquid, storing the polyethylene glycol liquid for recycling production, and feeding the solid-liquid mixture subjected to treatment into the step (2);
(2) washing a solid-liquid mixture separated by the ceramic membrane system with pure water to obtain a product comprising: adding the solid mixture of SiC, Si, Fe and impurities into hydrochloric acid, stirring and cleaning to separate out mixed particles of solid SiC, solid Si and impurities;
(3) adding the solid SiC and Si mixed particles into a fluid separator, controlling the flow rate of the fluid separator to layer SiC and Si, respectively collecting the layered SiC and Si, and not separating part of the solid SiC, solid Si and impurities in the mixed state.
Further, it is preferable that, after the step (3), the method further comprises: casting and purifying the separated Si to obtain solar grade polysilicon; and/or; drying the separated SiC, carrying out micro powder grading separation, and selecting and recycling according to the particle size.
Further, it is preferable that the hydrochloric acid has a temperature of 30 to 45 ℃ and a concentration of 10 to 30% in the step (2), and the stirring is performed for 30 to 90 minutes in the step (2).
Further, it is preferable that, in the step (3), the flow rate of the fluid separator is in the range of 40m/h to 60 m/h.
In one embodiment, the method comprises the following steps:
the first step is as follows: pressurizing the waste liquid, then introducing the waste liquid into a ceramic membrane system, and performing solid-liquid separation under the pressure of 0.20-0.55 MPa, wherein the ceramic membrane system is a microporous filtration technology, the effective filtration pore diameter is less than 1 mu m, PEG liquid in the waste liquid passes through micropores under the pressure driving, solid particles in the waste liquid cannot pass through the micropores, the separation process is performed at normal temperature without adding any chemical agent, no phase change occurs in the whole process, the purity of the separated PEG liquid reaches 99.7%, the separated PEG liquid completely meets the cutting production requirement, the PEG liquid can be directly stored for reuse production, and the PEG recovery rate is more than 92%;
the second step is that: washing concentrated slurry separated by a ceramic membrane system with pure water to obtain solid of SiC, Si, Fe and a very small amount of impurities, adding the solid into hydrochloric acid with the temperature of 30-45 ℃ and the concentration of 10-30%, stirring and washing for 30-90 minutes, reacting Fe and a small amount of impurities with the hydrochloric acid, dissolving the Fe and the small amount of impurities in the hydrochloric acid to remove the impurities, washing with the pure water after acid washing, and obtaining solid particles of SiC and Si;
the third step: adding the mixed particles obtained in the previous step into a fluid separator, controlling the flow rate of the fluid separator to be 40m/h-60 m/h, wherein the liquid used in the fluid separator is pure water or calcium chloride and sodium chloride solution, and because SiC and Si have different densities (SiC 3.2g/cm3 and Si 2.4g/cm 3), when the liquid in the fluid separator flows from bottom to top at a certain flow rate, the whole mixed particles are in a suspension state, low-density Si is suspended in an upper layer, high-density SiC is suspended in a lower layer, the flow of the fluid is stopped, the suspended mixed particles are separated and settled down in layers, the separation can be completed, SiC and Si are respectively collected, a small amount of mixture of SiC and Si is arranged in the middle of the separation layer of the fluid separator, the mixture can be collected additionally, and the mixture is separated again when the mixture is separated next time, so that the purity of the collected SiC and Si can be ensured, after multiple separation, the separation rate is improved;
the fourth step: the collected Si is cast and purified to obtain solar grade polysilicon, and the highest Si recovery rate can reach 85%; the fifth step: drying SiC, then carrying out micro powder grading separation, selecting and recycling according to the particle size, and the recovery rate is more than 90%.
As shown in fig. 2 and 3, the present embodiment also discloses a polysilicon wastewater treatment apparatus, wherein the utility model of the present embodiment mainly consists of a ceramic membrane system and a fluid separator, and thus, the structure thereof is mainly illustrated in fig. 2 and 3, and other components may be existing components, which will not be described in detail herein, and are known to those skilled in the art.
As shown in fig. 2, the ceramic membrane system includes a feed liquid tank 11, a feed pump 12, a circulation pump 13, a ceramic membrane 14, a permeate liquid tank 15, and a plurality of connection pipes, wherein pressure regulating valves and/or instruments are further disposed on the connection pipes.
Further, preferably, the ceramic membrane has a tubular multi-stage bent hollow structure, and the membrane pores are smaller than 1 μm.
Further, it is preferable that the ceramic membrane is made of titanium dioxide and zirconia frit.
Further, it is preferable that a liquid separator is further connected through the pipe, including:
a separation chamber 31 and a tank 33 connected thereto, a flow feed pump 32 being provided between the separation chamber and the tank.
Further, it is preferred that the liquid inlet of the separation chamber opens at a lower position of the separation chamber, where the low density fraction 34 is above and the high density fraction 35 is below, where there will be an incompletely separated mixture at the lowest.
Further, it is preferable that the liquid is pure water or calcium chloride or sodium chloride solution, more specifically, in the fluid separator, the liquid enters the separator from bottom to top, the mixture to be separated is in a suspension state by adjusting the flow rate of the liquid in the fluid separator, and the liquid used in the fluid separator is pure water or calcium chloride or sodium chloride solution with a certain concentration.
The following describes two embodiments with reference to the drawings, and the present invention is described in detail.
Example 1, one of the processing apparatus, was carried out according to the following procedure:
the first step is as follows: supplying the collected waste liquid to a ceramic membrane system through a feed pump, starting a circulating pump, controlling the inlet pressure of the ceramic membrane system to be 0.55MPa, the outlet pressure of the ceramic membrane system to be 0.40MPa, the filter aperture of a filling membrane of the ceramic membrane system to be 0.14 mu m by adjusting a rear valve of the feed pump, a rear valve of the circulating pump and a return valve of concentrated liquid, allowing PEG liquid in the waste liquid to pass through micropores of the ceramic membrane under the driving of pressure, preventing solid particles in the waste liquid from passing through, collecting and storing the penetrated PEG liquid, and collecting concentrated slurry after no PEG liquid is penetrated out;
the second step is that: washing concentrated slurry separated by a ceramic membrane system with pure water to obtain solid of SiC, Si, Fe and a very small amount of impurities, adding the solid into hydrochloric acid with the temperature of 30 ℃ and the concentration of 10%, stirring and washing for 90 minutes to remove Fe and a small amount of impurities, washing with pure water after acid washing, and obtaining solid particles of SiC and Si;
the third step: adding the mixed particulate matters obtained in the previous step into a fluid separator, and controlling the flow speed of the fluid separator to be 60 m/h, wherein the liquid used in the fluid separator is pure water, when the mixed particulate matters are all in a suspension state, rapidly stopping water inlet of the fluid separator, rapidly settling the mixture, and respectively collecting Si on the upper layer and SiC on the lower layer;
the fourth step: casting and purifying the collected Si to obtain solar grade polysilicon;
the fifth step: drying SiC, carrying out micro powder grading separation, and selecting and recycling according to the particle size;
the second example 2 and the second processing device were carried out by the following steps:
the first step is as follows: supplying the collected waste liquid to a ceramic membrane system through a feed pump, starting a circulating pump, controlling the inlet pressure of the ceramic membrane system to be 0.35MPa, the outlet pressure of the ceramic membrane system to be 0.2MPa, the filtering aperture of a filling membrane of the ceramic membrane system to be 0.3 mu m by adjusting a rear valve of the feed pump, a rear valve of the circulating pump and a reflux valve of concentrated liquid, wherein PEG liquid in the waste liquid passes through micropores of the ceramic membrane under the driving of pressure, solid particles in the waste liquid cannot pass through the micropores of the ceramic membrane, collecting and storing the penetrated PEG liquid, and collecting concentrated slurry after no PEG liquid is penetrated out;
the second step is that: washing concentrated slurry separated by a ceramic membrane system with pure water to obtain solid of SiC, Si, Fe and a very small amount of impurities, adding the solid into hydrochloric acid with the temperature of 40 ℃ and the concentration of 20%, stirring and washing for 60 minutes to remove Fe and a small amount of impurities, washing with pure water after acid washing, and obtaining solid particles of SiC and Si;
the third step: adding the mixed particulate matters obtained in the previous step into a fluid separator, and controlling the flow rate of the fluid separator to be 50 m/h, wherein the liquid used in the fluid separator is a 20% sodium chloride solution, when the mixed particulate matters are all in a suspension state, quickly stopping water inlet of the fluid separator, quickly settling the mixture, and respectively collecting the Si on the upper layer and the SiC on the lower layer;
the fourth step: casting and purifying the collected Si to obtain solar grade polysilicon;
the fifth step: drying SiC, carrying out micro powder grading separation, and selecting and recycling according to the particle size;
example 3, the third processing device, was carried out according to the following steps:
the first step is as follows: supplying the collected waste liquid to a ceramic membrane system through a feed pump, starting a circulating pump, controlling the inlet pressure of the ceramic membrane system to be 0.25MPa, the outlet pressure of the ceramic membrane system to be 0.1MPa, the filter aperture of a filling membrane of the ceramic membrane system to be 0.8 mu m by adjusting a rear valve of the feed pump, a rear valve of the circulating pump and a reflux valve of concentrated liquid, wherein PEG liquid in the waste liquid passes through micropores of the ceramic membrane under the driving of pressure, solid particles in the waste liquid cannot pass through the micropores of the ceramic membrane, collecting and storing the penetrated PEG liquid, and collecting concentrated slurry after no PEG liquid is penetrated out;
the second step is that: washing concentrated slurry separated by a ceramic membrane system with pure water to obtain solid of SiC, Si, Fe and a very small amount of impurities, adding the solid into hydrochloric acid with the temperature of 45 ℃ and the concentration of 30%, stirring and washing for 30 minutes to remove Fe and a small amount of impurities, washing with pure water after acid washing, and obtaining solid particles of SiC and Si;
the third step: adding the mixed particulate matters obtained in the previous step into a fluid separator, and controlling the flow rate of the fluid separator to be 40m/h, wherein the liquid used in the fluid separator is a 30% calcium chloride solution, when the mixed particulate matters are all in a suspension state, quickly stopping water inlet of the fluid separator, quickly settling the mixture, and respectively collecting the Si on the upper layer and the SiC on the lower layer;
the fourth step: casting and purifying the collected Si to obtain solar grade polysilicon;
the fifth step: drying SiC, carrying out micro powder grading separation, and selecting and recycling according to the particle size;
the utility model discloses there is following superiority:
the ceramic membrane solid-liquid separation technology has the advantages that the original waste liquid is directly subjected to pressure separation without any treatment, no chemicals are added, the purity of the separated PEG reaches 99.7%, the process is simple and reliable, the PEG separation and purification process can be completed at one time, and the PEG recovery rate reaches 92%;
the innovative SiC and Si fluid separator technology is simple to operate and has good separation effect, the Si recovery rate can reach 85% at most, and the SiC recovery rate is over 90%. Since the SiC and Si mixture of the separation interface can be continuously separated in the next separation, the separation rate is theoretically higher the more separation times.
Third the utility model discloses the waste liquid changing waste into valuables that will handle has not only realized "zero" emission of pollutant, has very high economic benefits again simultaneously:
| market price (Yuan/kilogram) | Recycle price (Yuan/kg) | |
| Polyethylene glycol (PEG) | 12 | 12 |
| Silicon carbide (SiC) | 24 | 18 |
| Silicon (Si) | 140 | 140 |
It should be noted that for the sake of simplicity, the above-mentioned embodiments of the apparatus are described as a series of acts or combinations, but those skilled in the art should understand that the present application is not limited by the described order of acts, as some steps may be performed in other orders or simultaneously according to the present application. Further, those skilled in the art should also appreciate that the embodiments described in the specification are preferred embodiments and that the acts and modules referred to are not necessarily required in this application.
As will be appreciated by one skilled in the art, embodiments of the present application may be provided as an apparatus, system, or computer program product. Accordingly, the present application may take the form of an entirely hardware embodiment, an entirely software embodiment or an embodiment combining software and hardware aspects.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A polysilicon wastewater treatment device is characterized by comprising: a ceramic membrane system;
the ceramic membrane system comprises a feed liquid tank, a feed pump, a circulating pump, a ceramic membrane, a permeation liquid tank and a plurality of connecting pipelines, wherein the upper opening of the feed liquid tank is connected with the circulating pump through the connecting pipelines, the lower end of the feed liquid tank is connected with the feed pump, the feed pump is connected with the connecting pipelines between the circulating pump and the upper opening of the feed liquid tank through the connecting pipelines, the circulating pump is connected with the ceramic membrane through the connecting pipelines, the ceramic membrane is connected with the upper opening of the permeation liquid tank through the connecting pipelines, and a pressure regulating valve and/or an instrument are/is further arranged on the connecting pipelines.
2. The polysilicon wastewater treatment device according to claim 1, wherein the ceramic membrane has a tubular multi-section bent hollow structure, and the membrane pores are smaller than 1 μm.
3. The polysilicon wastewater treatment apparatus according to claim 1, wherein a liquid separator is further connected through a pipe, comprising:
the device comprises a separation cavity, a fluid storage tank connected with the separation cavity, and a flow supply pump, wherein the flow supply pump is arranged between the separation cavity and the fluid storage tank.
4. The polysilicon wastewater treatment apparatus according to claim 3, wherein the liquid inlet of the separation chamber opens at a position below the separation chamber.
5. The polysilicon wastewater treatment apparatus according to claim 4, wherein the liquid is pure water or calcium chloride or sodium chloride solution.
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| CN2012207440653U CN203128312U (en) | 2012-12-29 | 2012-12-29 | Polycrystalline silicon waste water treatment device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012207440653U CN203128312U (en) | 2012-12-29 | 2012-12-29 | Polycrystalline silicon waste water treatment device |
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