CN103896425A - Polycrystalline silicon wastewater treatment device and method - Google Patents
Polycrystalline silicon wastewater treatment device and method Download PDFInfo
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- CN103896425A CN103896425A CN201210588234.3A CN201210588234A CN103896425A CN 103896425 A CN103896425 A CN 103896425A CN 201210588234 A CN201210588234 A CN 201210588234A CN 103896425 A CN103896425 A CN 103896425A
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a polycrystalline silicon wastewater treatment device and a method. The device comprises a ceramic membrane system, wherein the ceramic membrane system comprises a material liquid tank, a supply pump, a circulation pump, a ceramic membrane, a permeate tank and a plurality of connecting pipelines, wherein pressure regulation valves and/or instruments and meters are arranged on the connecting pipelines; a liquid separator is further connected through the pipelines; the liquid separator comprises a separation chamber as well as a fluid storage tank and a flow supply pump connected with the separation chamber; the flow supply pump is arranged between the separation chamber and the fluid storage tank. By adopting the method, the original pollutant treatment is converted into industrial resources which can be recycled, so that the waste is turned into wealth, and very high economic values and environment benefits are achieved.
Description
Technical field
The present invention relates to a kind of method of wastewater treatment, be specifically related to a kind of polysilicon method of wastewater treatment and device, belong to waste water reclamation and utilize field.
Background technology
Elementary silicon is as important photoelectric material, semiconductor material, and the status of its strategic resource is day by day obvious, and its global demand amount also constantly increases.At photoelectricity, in semiconductor industry, elemental silicon body need to be cut into satisfactory silicon chip, polysilicon is mainly to adopt multi-wire saw technology at present, in cutting process, approximately 50% silicon material is infiltrated in the cutting fluid being made up of polyoxyethylene glycol (PEG) cutting fluid and carborundum powder (SiC) abrasive material, make the composition of micro mist in cutting fluid, particle diameter, hardness does not all meet standard, cause cutting ability to decline, can not reuse, therefore in cutting process, need constantly to discharge old cutting fluid, and constantly supplement new cutting fluid, so just produce a large amount of cutting waste liquors.
Cutting waste fluid is the thick suspension of black, and main ingredient and content are: polyoxyethylene glycol (PEG), 40%～50%; Silicon carbide (SiC), 23%～33%; Silicon (Si), 20%～24%; Iron filings (Fe), 2. 5%～3. 0%.Wherein, the raw material of PEG is to extract in oil, repolymerization forms, and molecular structure stabilized is difficult for decomposing, very easily water-soluble, biological oxygen demand (BOD) is low, is difficult for degraded at occurring in nature, and its COD (chemical oxygen demand (COD)) value substantially exceeds wastewater discharge standard, as without special processing, flow into physical environment and will cause huge pollution.SiC and Si are important industrial raw material, all belong to Nonrenewable resources.Produce in SiC raw material process and will consume the huge energy, country now limits this new industrial project.Si is wherein the high-purity silicon powder that cuts, if direct discharge can cause the waste of environmental pollution and silicon materials.
For the processing of this waste water, there are two kinds of thinkings at present: one is to process rear discharge up to standard.Common method has microbial method, advanced oxidation processes etc., for this important waste water containing PEG, and microbial method complex process, processing efficiency is low, and poor processing effect hardly may be up to standard; Advanced oxidation processes treatment effect is better, but working cost is higher, technology controlling and process complexity; Other conventional sewage water treatment method is also difficult to be suitable for; Another kind of thinking is by waste liquid classification recycling, because the PEG in waste water, SiC and Si are important industrial raw material, and wherein 12 yuan of per kilograms of polyoxyethylene glycol (PEG) market price, 24 yuan of per kilograms of SiC market price, 140 yuan of per kilograms of Si market price.Therefore, classification reclaim and utilize silicon cutting waste liquor for economizing on resources, protection of the environment, increase economic efficiency significantly, had comparatively ripe processing recovery technology abroad, domestic this respect technology is also immature, mostly in conceptual phase.
Domestic existing processing recovery technology, as a kind of zero-emission process for photovoltaic wastewater (CN 102557291A), system flow is long, complex process, investment are excessive, is difficult to realize practical implementation; A kind of processing, containing the method (CN 1023722388A) of polyoxyethylene glycol waste water, adopts flocculation sediment, Fendon oxidation technology, and processed waste water need enter waste water treatment plant again and process, and cost of use higher, and and be not suitable for the processing of polysilicon waste water; From silicon chip cutting processing byproduct, reclaim the method (CN101244823A) of silicon carbide, this patented method adopts centrifugal solid-liquid to separate, the silicon carbide in a Recycling of waste liquid, and the silicon that polyoxyethylene glycol and recovery value are higher does not relate to;
Existing recovery technology subject matter is: 1. solid-liquid separation effect is not good, often need through stage trapping, as: centrifugation, sloping plate deposition, filtration, press filtration etc., isolated PEG liquid contains the impurity of part lightweight, needs through the ability reuse of further purifying; 2. SiC and Si sepn process complexity and effect are not good enough, need to use various chemical medicaments or through multiple physical process, lack a kind of simple and effective separation method.
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Summary of the invention
Technical problem to be solved by this invention is to process efficiently reuse technology, can thoroughly solve the not good problem of solid-liquid separation effect, for this reason, provides a kind of polysilicon wastewater treatment equipment and method.
It is as follows that the present invention solves the problems of the technologies described above taked technical scheme:
A kind of polysilicon wastewater treatment equipment, comprising: ceramic membrane system;
Wherein, described ceramic membrane system, comprises feed liquid case, charging pump, recycle pump, ceramic membrane, sees through liquid case and multiple connecting tube, wherein, is also provided with pressure regulator valve door and/or instrument on connecting tube.
Further, preferably, described ceramic membrane be shaped as tubular type multistage bending hollow structure, fenestra is less than 1 μ m.
Further, preferably, described ceramic membrane is by being made up of titanium dioxide and zirconium dioxide material.
Further, preferably, be also connected with liquid trap by pipeline, comprise:
Separate cavity and coupled fluid reservoir, flow supply pump, wherein, described flow supply pump is located at and is separated between cavity and described fluid reservoir.
Further, preferably, the liquid-inlet of described separation cavity is opened in the lower position of described separation cavity.
Further, preferably, described liquid is pure water or calcium chloride or sodium chloride solution.
A kind of polysilicon method of wastewater treatment, comprising:
(1) polysilicon waste liquid is entered after supercharging into ceramic membrane system, carry out solid-liquid separation under 0.20MPa-0.55MPa pressure, isolate polyoxyethylene glycol fluid storage and produce in order to reuse, the solidliquid mixture that sub-department goes out enters step (2);
(2) by clean by pure water rinsing isolated ceramic membrane system solidliquid mixture, comprised: the solid mixture of SiC, Si, Fe and impurity, this solid mixture is added in hydrochloric acid and stirs and clean, isolate the composite grain thing of solid SiC, solid Si and impurity;
(3) described solid SiC and Si composite grain thing are added to fluid separator, control fluid separator flow velocity, make SiC and Si layering, and collect respectively SiC and the Si of layering, solid SiC, the solid Si of part in admixture do not separate with impurity.
Further, preferably, after step (3), also comprise: the Si founding after separating is purified, to obtain solar-grade polysilicon; And/or; SiC after separating is dried rear and carries out micro-powder graded separation, select reuse by size.
Further, preferably, in step (2), 30 DEG C-45 DEG C of the temperature of described hydrochloric acid, concentration 10%-30%, and, in step (2), also to stir 30-90 minute.
Further, preferably, in step (3), described fluid separator flow velocity is 40m/h-60 m/h.
After the present invention has taked such scheme, there is following superiority:
1. former waste liquid is without any processing, and direct weighting separates, and does not need to add any chemical, and isolated PEG purity reaches 99.7%, and process is simple and reliable, once just can complete that PEG separates and through purification process, the PEG rate of recovery reaches 92%;
2. the SiC of novelty and Si fluid separator technology, not only simple to operate, and have good separating effect, the Si rate of recovery to reach as high as 85%, the SiC rate of recovery more than 90%.Because the SiC of separating interface can continue to separate with Si mixture in separating next time, separate in theory number of times more, separation rate is higher.
3. the waste liquid of need processing is turned waste into wealth in the present invention, has not only realized " zero " discharge of pollutent, has again very high economic benefit simultaneously.
Other features and advantages of the present invention will be set forth in the following description, and, partly from specification sheets, become apparent, or understand by implementing the present invention.Object of the present invention and other advantages can be realized and be obtained by specifically noted structure in write specification sheets, claims and accompanying drawing.
Brief description of the drawings
Below in conjunction with accompanying drawing, the present invention is described in detail, to make above-mentioned advantage of the present invention clearer and more definite.Wherein,
Fig. 1 is the schematic flow sheet of polysilicon method of wastewater treatment of the present invention;
Fig. 2 is the structural representation of the ceramic membrane system of polysilicon wastewater treatment equipment of the present invention;
Fig. 3 is the structural representation of the fluid separator of polysilicon wastewater treatment equipment of the present invention.
Embodiment
Describe embodiments of the present invention in detail below with reference to drawings and Examples, to the present invention, how utilisation technology means solve technical problem whereby, and the implementation procedure of reaching technique effect can fully understand and implement according to this.It should be noted that, only otherwise form conflict, each feature in each embodiment and each embodiment in the present invention can mutually combine, and the technical scheme forming is all within protection scope of the present invention.
In addition, can in the computer system such as one group of computer executable instructions, carry out in the step shown in the schema of accompanying drawing, and, although there is shown logical order in flow process, but in some cases, can carry out shown or described step with the order being different from herein.
As shown in Figure 1, described polysilicon method of wastewater treatment, the present invention carries out according to following step:
(1) polysilicon waste liquid is entered after supercharging into ceramic membrane system, carry out solid-liquid separation under 0.20MPa-0.55MPa pressure, isolate polyoxyethylene glycol fluid storage and produce in order to reuse, the solidliquid mixture that sub-department goes out enters step (2);
(2) by clean by pure water rinsing isolated ceramic membrane system solidliquid mixture, comprised: the solid mixture of SiC, Si, Fe and impurity, this solid mixture is added in hydrochloric acid and stirs and clean, isolate the composite grain thing of solid SiC, solid Si and impurity;
(3) described solid SiC and Si composite grain thing are added to fluid separator, control fluid separator flow velocity, make SiC and Si layering, and collect respectively SiC and the Si of layering, solid SiC, the solid Si of part in admixture do not separate with impurity.
Further, preferably, after step (3), also comprise: the Si founding after separating is purified, to obtain solar-grade polysilicon; And/or; SiC after separating is dried rear and carries out micro-powder graded separation, select reuse by size.
Further, preferably, in step (2), 30 DEG C-45 DEG C of the temperature of described hydrochloric acid, concentration 10%-30%, and, in step (2), also to stir 30-90 minute.
Further, preferably, in step (3), described fluid separator flow velocity is 40m/h-60 m/h.
Wherein, in a more specific embodiment, operate according to step below:
The first step: waste liquid is entered after supercharging into ceramic membrane system, under 0.20MPa-0.55MPa pressure, carry out solid-liquid separation, ceramic membrane system is millipore filtration technology, effectively pore size filter is less than 1 μ m, under pressure-driven, PEG liquid in waste liquid passes through micropore, solid particulate in waste liquid cannot pass through, sepn process is carried out at normal temperatures, do not need to add any chemical agent yet, there is not any phase transformation in whole process, isolated PEG purity liquid reaches 99.7%, reach cutting production requirement completely, can directly store in order to reuse and produce, the PEG rate of recovery is greater than 92%,
Second step: by clean by pure water rinsing isolated ceramic membrane system concentrated mud, obtain the solid of SiC, Si, Fe and minute quantity impurity, this solids is added to 30 DEG C-45 DEG C of temperature, stirring and washing 30-90 minute in the hydrochloric acid of concentration 10%-30%, Fe and a small amount of impurity and hydrochloric acid reaction, be dissolved in hydrochloric acid and be removed, after overpickling, clean by pure water rinsing, gained solid particulate is SiC and Si;
The 3rd step: the composite grain thing obtaining in upper step is added to fluid separator, controlling fluid separator flow velocity is 40m/h-60 m/h, wherein in fluid separator, liquid used is pure water or calcium chloride, sodium chloride solution, due to SiC (SiC 3.2g/cm3s different from Si density, Si 2.4g/cm3), when the liquid in fluid separator is during from bottom to top with certain flow rate, composite grain thing entirety is in suspended state, the little Si of density is suspended in upper strata, the SiC that density is large is suspended in lower floor, at this moment stopping fluid flowing, the composite grain suspending just delaminating deposition gets off, can complete separation, collect respectively SiC, Si, in the middle of fluid separator separating layer, there is the mixture of a small amount of SiC and Si, this part mixture can be collected in addition, in the time of next mixture separation, separate again, can ensure like this SiC and the Si purity collected, simultaneously after separating for several times, separation rate will improve,
The 4th step: the Si founding of collecting is purified, can obtain solar-grade polysilicon, the Si rate of recovery reaches as high as 85%; The 5th step: carry out micro-powder graded separation after SiC is dry, select reuse by size, the rate of recovery is more than 90%.
Wherein, as shown in Figures 2 and 3, the present embodiment also discloses a kind of polysilicon wastewater treatment equipment, wherein, the inventive point of the present embodiment is mainly ceramic membrane system and fluid separator, therefore, mainly in Fig. 2 and Fig. 3 example its structure, other parts can adopt existing parts, are not elaborated at this, and these are all that those skilled in the art can know.
As shown in Figure 2, described ceramic membrane system, comprises feed liquid case 11, charging pump 12, recycle pump 13, ceramic membrane 14, sees through liquid case 15 and multiple connecting tube, wherein, is also provided with pressure regulator valve door and/or instrument on connecting tube.
Further, preferably, described ceramic membrane be shaped as tubular type multistage bending hollow structure, fenestra is less than 1 μ m.
Further, preferably, described ceramic membrane is by being made up of titanium dioxide and zirconium dioxide material.
Further, preferably, be also connected with liquid trap by pipeline, comprise:
Further, preferably, the liquid-inlet of described separation cavity is opened in the lower position of described separation cavity, wherein, little density separation thing 34 up, large density separation thing 35 below, below, can exist and not separate mixture completely.
Further, preferably, described liquid is pure water or calcium chloride or sodium chloride solution, more particularly, in described fluid separator, liquid used enters separator from the bottom to top, by regulating flow rate of liquid in fluid separator, be mixture to be separated in suspended state, and fluid separator liquid used is pure water or certain density calcium chloride, sodium chloride solution.
Below in conjunction with two embodiment of accompanying drawing narration, the present invention is described in detail.
One of embodiment 1, treatment process, according to carrying out with following step:
The first step: the waste liquid of collecting is supplied with to ceramic membrane system through fresh feed pump, ON cycle pump, by regulating fresh feed pump late gate, recycle pump late gate and concentrated solution reverse flow valve, controlling ceramic membrane system intake pressure is 0.55MPa, ceramic membrane system outlet pressure is 0.40MPa, it is 0.14 μ m that ceramic membrane system is loaded membrane filtration aperture, under pressure-driven, PEG liquid in waste liquid is by ceramic membrane micropore, solid particulate in waste liquid cannot pass through, the PEG liquid collecting seeing through is stored, after appearing without PEG liquid, collect enriching slurry;
Second step: by clean by pure water rinsing isolated ceramic membrane system enriching slurry, obtain the solid of SiC, Si, Fe and minute quantity impurity, this solids is added to 30 DEG C of temperature, stirring and washing 90 minutes in the hydrochloric acid of concentration 10%, remove Fe and a small amount of impurity, after overpickling, clean by pure water rinsing, gained solid particulate is SiC and Si;
The 3rd step: the composite grain thing obtaining in upper step is added to fluid separator, controlling fluid separator flow velocity is 60 m/h, wherein in fluid separator, liquid used is pure water, when composite grain thing is during all in suspended state, stop fast fluid separator water inlet, mixture rapid subsidence is got off, collect respectively the Si on upper strata and the SiC of lower floor;
The 4th step: the Si founding of collecting is purified, can obtain solar-grade polysilicon;
The 5th step: carry out micro-powder graded separation after SiC is dry, select reuse by size;
Two of embodiment 2, treatment process, according to carrying out with following step:
The first step: the waste liquid of collecting is supplied with to ceramic membrane system through fresh feed pump, ON cycle pump, by regulating fresh feed pump late gate, recycle pump late gate and concentrated solution reverse flow valve, controlling ceramic membrane system intake pressure is 0.35MPa, ceramic membrane system outlet pressure is 0.2MPa, it is 0.3 μ m that ceramic membrane system is loaded membrane filtration aperture, under pressure-driven, PEG liquid in waste liquid is by ceramic membrane micropore, solid particulate in waste liquid cannot pass through, the PEG liquid collecting seeing through is stored, after appearing without PEG liquid, collect enriching slurry;
Second step: by clean by pure water rinsing isolated ceramic membrane system enriching slurry, obtain the solid of SiC, Si, Fe and minute quantity impurity, this solids is added to 40 DEG C of temperature, stirring and washing 60 minutes in the hydrochloric acid of concentration 20%, remove Fe and a small amount of impurity, after overpickling, clean by pure water rinsing, gained solid particulate is SiC and Si;
The 3rd step: the composite grain thing obtaining in upper step is added to fluid separator, controlling fluid separator flow velocity is 50 m/h, wherein in fluid separator, liquid used is 20% sodium chloride solution, when composite grain thing is during all in suspended state, stop fast fluid separator water inlet, mixture rapid subsidence is got off, collect respectively the Si on upper strata and the SiC of lower floor;
The 4th step: the Si founding of collecting is purified, can obtain solar-grade polysilicon;
The 5th step: carry out micro-powder graded separation after SiC is dry, select reuse by size;
Three of embodiment 3, treatment process, according to carrying out with following step:
The first step: the waste liquid of collecting is supplied with to ceramic membrane system through fresh feed pump, ON cycle pump, by regulating fresh feed pump late gate, recycle pump late gate and concentrated solution reverse flow valve, controlling ceramic membrane system intake pressure is 0.25MPa, ceramic membrane system outlet pressure is 0.1MPa, it is 0.8 μ m that ceramic membrane system is loaded membrane filtration aperture, under pressure-driven, PEG liquid in waste liquid is by ceramic membrane micropore, solid particulate in waste liquid cannot pass through, the PEG liquid collecting seeing through is stored, after appearing without PEG liquid, collect enriching slurry;
Second step: by clean by pure water rinsing isolated ceramic membrane system enriching slurry, obtain the solid of SiC, Si, Fe and minute quantity impurity, this solids is added to temperature 45 C, stirring and washing 30 minutes in the hydrochloric acid of concentration 30%, remove Fe and a small amount of impurity, after overpickling, clean by pure water rinsing, gained solid particulate is SiC and Si;
The 3rd step: the composite grain thing obtaining in upper step is added to fluid separator, controlling fluid separator flow velocity is 40 m/h, wherein in fluid separator, liquid used is 30% calcium chloride solution, when composite grain thing is during all in suspended state, stop fast fluid separator water inlet, mixture rapid subsidence is got off, collect respectively the Si on upper strata and the SiC of lower floor;
The 4th step: the Si founding of collecting is purified, can obtain solar-grade polysilicon;
The 5th step: carry out micro-powder graded separation after SiC is dry, select reuse by size;
The present invention has following superiority:
Ceramic membrane solid-liquid separation technique, former waste liquid is without any processing, and direct weighting separates, and does not need to add any chemical, and isolated PEG purity reaches 99.7%, and process is simple and reliable, once just can complete that PEG separates and through purification process, the PEG rate of recovery reaches 92%;
2. the SiC of novelty and Si fluid separator technology, not only simple to operate, and have good separating effect, the Si rate of recovery to reach as high as 85%, the SiC rate of recovery more than 90%.Because the SiC of separating interface can continue to separate with Si mixture in separating next time, separate in theory number of times more, separation rate is higher.
3. the waste liquid of need processing is turned waste into wealth in the present invention, has not only realized " zero " discharge of pollutent, has again very high economic benefit simultaneously:
| ? | Market price (unit/kilogram) | Recovery article valency (unit/kilogram) |
| Polyoxyethylene glycol (PEG) | 12 | 12 |
| Silicon carbide (SiC) | 24 | 18 |
| Silicon (Si) | 140 | 140 |
It should be noted that, for aforesaid method embodiment, for simple description, therefore it is all expressed as to a series of combination of actions, but those skilled in the art should know, the application is not subject to the restriction of described sequence of operation, because according to the application, some step can adopt other orders or carry out simultaneously.Secondly, those skilled in the art also should know, the embodiment described in specification sheets all belongs to preferred embodiment, and related action and module might not be that the application is necessary.
Those skilled in the art should understand, the application's embodiment can be provided as method, system or computer program.Therefore, the application can adopt complete hardware implementation example, completely implement software example or the form in conjunction with the embodiment of software and hardware aspect.
Finally it should be noted that: the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although the present invention is had been described in detail with reference to previous embodiment, for a person skilled in the art, its technical scheme that still can record aforementioned each embodiment is modified, or part technical characterictic is wherein equal to replacement.Within the spirit and principles in the present invention all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a polysilicon wastewater treatment equipment, is characterized in that, comprising: ceramic membrane system;
Wherein, described ceramic membrane system, comprises feed liquid case, charging pump, recycle pump, ceramic membrane, sees through liquid case and multiple connecting tube, wherein, is also provided with pressure regulator valve door and/or instrument on connecting tube.
2. polysilicon wastewater treatment equipment according to claim 1, is characterized in that, described ceramic membrane be shaped as tubular type multistage bending hollow structure, fenestra is less than 1 μ m.
3. polysilicon wastewater treatment equipment according to claim 2, is characterized in that, described ceramic membrane is by being made up of titanium dioxide and zirconium dioxide material.
4. polysilicon wastewater treatment equipment according to claim 1, is characterized in that, is also connected with liquid trap by pipeline, comprising:
Separate cavity and coupled fluid reservoir, flow supply pump, wherein, described flow supply pump is located at and is separated between cavity and described fluid reservoir.
5. polysilicon wastewater treatment equipment according to claim 4, is characterized in that, the liquid-inlet of described separation cavity is opened in the lower position of described separation cavity.
6. polysilicon wastewater treatment equipment according to claim 5, is characterized in that, described liquid is pure water or calcium chloride or sodium chloride solution.
7. a polysilicon method of wastewater treatment, is characterized in that, comprising:
(1) polysilicon waste liquid is entered after supercharging into ceramic membrane system, carry out solid-liquid separation under 0.20MPa-0.55MPa pressure, isolate polyoxyethylene glycol fluid storage and produce in order to reuse, the solidliquid mixture that sub-department goes out enters step (2);
(2) by clean by pure water rinsing isolated ceramic membrane system solidliquid mixture, comprised: the solid mixture of SiC, Si, Fe and impurity, this solid mixture is added in hydrochloric acid and stirs and clean, isolate the composite grain thing of solid SiC, solid Si and impurity;
(3) described solid SiC and Si composite grain thing are added to fluid separator, control fluid separator flow velocity, make SiC and Si layering, and collect respectively SiC and the Si of layering, solid SiC, the solid Si of part in admixture do not separate with impurity.
8. polysilicon method of wastewater treatment according to claim 7, is characterized in that, after step (3), also comprises: the Si founding after separating is purified, to obtain solar-grade polysilicon;
And/or; SiC after separating is dried rear and carries out micro-powder graded separation, select reuse by size.
9. polysilicon method of wastewater treatment according to claim 7, is characterized in that, in step (2), and 30 DEG C-45 DEG C of the temperature of described hydrochloric acid, concentration 10%-30%, and, in step (2), also to stir 30-90 minute.
10. polysilicon method of wastewater treatment claimed in claim 7, is characterized in that, in step (3), described fluid separator flow velocity is 40m/h-60 m/h.
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| CN108162216A (en) * | 2017-12-28 | 2018-06-15 | 洛阳阿特斯光伏科技有限公司 | A kind of diamond wire sliced crystal silicon production line and its water system |
| CN113754172A (en) * | 2021-09-28 | 2021-12-07 | 南通友拓新能源科技有限公司 | Polycrystalline silicon wastewater treatment method |
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| CN103896425B (en) | 2015-09-30 |
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