CN103496831B - Recycling method of silicon wafer cutting edge material waste water treatment sludge - Google Patents
Recycling method of silicon wafer cutting edge material waste water treatment sludge Download PDFInfo
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- CN103496831B CN103496831B CN201310427494.7A CN201310427494A CN103496831B CN 103496831 B CN103496831 B CN 103496831B CN 201310427494 A CN201310427494 A CN 201310427494A CN 103496831 B CN103496831 B CN 103496831B
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Abstract
The invention discloses a recycling method of silicon wafer cutting edge material waste water treatment sludge, aiming at solving the technical problem that the flocculent precipitating sludge formed due to waste water treatment in the production process of silicon wafer cutting edge material silicon carbide powder is subjected to resource recycling. The recycling method comprises the following steps: mixing silicon wafer cutting edge material waste water treatment sludge with water, then introducing to a hydrocyclone separator for floatation and separation, and performing filter-pressing concentration to light-phase suspension separated from an overflowing port of the hydrocyclone to obtain recycled product calcium silicate; removing impurities of a heavy-phase slurry separated from a bottom flowing port of the hydrocyclone, then dewatering and drying to obtain the silicon wafer cutting edge material silicon carbide powder. Through adopting the method, the water treatment sludge can be recycled, so that not only can the environment pollution be avoided, but also economic benefits can be brought for enterprises, and the recycling of resources can be achieved.
Description
Technical field
The present invention relates to a kind of recoverying and utilizing method of wastewater treatment mud, particularly a kind of recoverying and utilizing method of crystal silicon wafer cutting edge material wastewater treatment mud.
Background technology
Crystal silicon wafer cutting edge material silicon carbide powder in process of production, needs to carry out chemical purification process to raw material, makes product indices reach corresponding requirements.In these treating processess, partially carbonized silicon powder is discharged along with waste water, after the process of dosing flocculation sediment, forms flocculation sediment mud.Solids component in this mud mainly comprises two portions, and a part is cutting blade material silicon carbide powder particle, and another part is the calsil that the silicate ion produced in chemical purification process is formed through flocculation sediment, and other also comprises the uncombined carbon etc. of trace.This mud saltiness is high, can significantly improve soil conductivity, destroys plant nutrient and balances and cause surface water pollution.The mud that flocculation sediment gets off, as a kind of trade waste, needs to deal carefully with, in order to avoid pollute ecotope through flow processs such as strict sterilization cleaning, sanitary landfill and outward transports usually.The manpower financial capacity that this process consumes is a large amount of, adds production and operation cost and the burden on society of enterprise.
A kind of method of resource utilization recovery silicon carbide component from crystalline silicon cutting waste mortar is disclosed in Chinese invention patent specification sheets CN102399618B, the method comprises: in crystalline silicon cutting waste mortar, add leveler, by cyclone separator, the mortar material after homogenate is carried out cyclonic separation; Press filtration separation is carried out to the light phase suspension of being discharged by cyclone separator overflow outlet and obtains filtrate and filter residue; The heavy phase slurry of being discharged by cyclone separator underflow outlet removes cutting liquid and separating agent by mechanical separator, then carries out alkali cleaning, pickling and cleaning, after gained silicon carbide wet material drying, obtains silicon carbide component.
But the mud do not produced because of wastewater treatment in process of production crystal silicon wafer cutting edge material silicon carbide powder in the prior art carries out the method for resource utilization recycling.How this mud is recycled and just seem particularly important, make it be used adequately reasonably, both can avoid polluting ecotope, also can reduce enterprise's production and operation cost simultaneously, reach the object that trade waste resource utilization is recycled, ensure environmental safety and bring economic benefit, realizing economic circulation development.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of recoverying and utilizing method of crystal silicon wafer cutting edge material wastewater treatment mud, and the method can carry out resource utilization recycling to the flocculation sediment mud that crystal silicon wafer cutting edge material silicon carbide powder is formed because of wastewater treatment in process of production.
For solving the problems of the technologies described above, the recoverying and utilizing method of crystal silicon wafer cutting edge material wastewater treatment mud of the present invention comprises the following steps:
(1) mix and blend: crystal silicon wafer cutting edge material wastewater treatment mud and water mixed by the mass ratio of 1:1 ~ 1:1.5 and stirs 2 ~ 4 hours, obtaining mixed slurry;
(2) flotation separation: described mixed slurry is introduced wet cyclone (hydrocyclone), temperature be 20 DEG C ~ 60 DEG C, feeding pressure carries out flotation separation under being the condition of 0.1 ~ 0.3MPa, obtains light phase suspension and heavy phase mortar;
(3) filter press concentration: the calsil in described mixed slurry and uncombined carbon separate through the overflow port of wet cyclone with light phase suspension, by this light phase suspension lead 1-in plate paper blotter press, be carry out filter press concentration under the condition of 10 ~ 20MPa at pressure, be recycled product Calucium Silicate powder;
(4) dehydrate: the silicon carbide in described mixed slurry separates with the underflow opening of heavy phase mortar through wet cyclone, carried out dehydrating process by this heavy phase mortar, removing moisture wherein, obtains crystal silicon wafer cutting edge material silicon carbide powder product.
Pass through aforesaid method, this crystal silicon wafer cutting edge material wastewater treatment mud obtains resource utilization and recycles process, the product Calucium Silicate powder wherein reclaimed can be applied to the building material industries such as cement, the crystal silicon wafer cutting edge material silicon carbide micro-powder product reclaimed can directly use as finished product or sell, both contaminate environment was avoided, realize resource circulation utilization again, turn waste into wealth, bring economic worth.
In technique scheme, preferably, in step (4), also comprise following removal step to before the drying of described heavy phase slurry dehydration:
A. pickling: add in described heavy phase mortar and be the acid of 2% ~ 10% with solid masses per-cent contained by heavy phase mortar and stir, calsil impurity in heavy phase mortar is fully contacted with added acid, react after 3 ~ 8 hours, carried out 1 ~ 3 concentrated and cleaning that adds water again, removing calsil impurity wherein, and make the pH value of the heavy phase mortar after removing calsil impurity in neutral;
B. de-carbon: the heavy phase mortar after removing calsil impurity is introduced the kiln basin of carbon removing device and the stirring 2 ~ 3 hours that adds water, in kiln basin, pass into the pressurized air of 0.1 ~ 0.3MPa pressure simultaneously, make uncombined carbon impurity in this heavy phase mortar along with bubble floating is to kiln basin surface, scraped off by rotor segment, thus by the uncombined carbon impurity removing in this heavy phase mortar.
The acid added in heavy phase mortar in step a to be concentration be 35% ~ 37% hydrochloric acid or concentration be the sulfuric acid of 95% ~ 98%.
Carbon removing device described in step b refers to de-carbon, impurity removing apparatus disclosed in Chinese utility model patent specification sheets CN 202898044 U, this device comprises by the kiln basin formed at the bottom of columned pond body and cone shape pond, described kiln basin offers overflow groove along position, and at described kiln basin upper edge hole place, rotor segment being installed, its length and this kiln basin upper edge hole diameter match; Air-blowing mechanism is installed bottom described kiln basin.This de-carbon, impurity removing apparatus are in use, mixed mortar is introduced kiln basin, open air-blowing mechanism, air-blowing in kiln basin, mixed slurry is constantly stirred by compressed air and seethes in material pond, and the carbon in slip is seethed with foam form floats up to liquid level, other impurity component in slip is also seethed simultaneously floats up to liquid level, the carbon be mingled with in foam subsequently and impurity are pushed into overflow groove by the rotor segment rotated, and are then flowed away by overflow groove, and then play the effect of de-carbon, removal of impurities.In the recoverying and utilizing method of crystal silicon wafer cutting edge material wastewater treatment mud of the present invention, use this device effectively can remove impurity uncombined carbon in heavy phase mortar, make silicon carbide purity in remaining slurry higher.
By the calsil impurity in heavy phase mortar and uncombined carbon Impurity removal, then after dehydrating, highly purified crystal silicon wafer cutting edge material silicon carbide powder product finally can be obtained by a, b two steps.
For concrete operation step of the present invention and technical process, further detailed description will be made by reference to the accompanying drawings below.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the recoverying and utilizing method of crystal silicon wafer cutting edge material wastewater treatment mud of the present invention.
Embodiment
The process flow sheet of the recoverying and utilizing method of crystal silicon wafer cutting edge material wastewater treatment mud of the present invention as shown in Figure 1, comprises the following steps (involved plant and instrument if no special instructions, is routine instrument device).
First crystal silicon wafer cutting edge material wastewater treatment mud and water mixed by the mass ratio of 1:1 ~ 1:1.5 and stir 2 ~ 4 hours, obtaining mixed slurry.
Then described mixed slurry is introduced wet cyclone and carries out flotation separation, temperature be 20 DEG C ~ 60 DEG C, feeding pressure carries out flotation separation under being the condition of 0.1 ~ 0.3MPa, obtains light phase suspension and heavy phase mortar.
This light phase suspension is pumped into plate and frame(type)filter press by mortar pump, under the filteration and the effect of pushing tow pressure of filter cloth and sheet frame, liquid in the light phase suspension of filtering, Calucium Silicate powder solid is continuous enrichment between filter plate, after enrichment is full, pull open filter plate and unload Calucium Silicate powder solid, thus reach the object of filter press concentration.Press filtration pressure-controlling is at 10-20MPa, and the filter opening aperture of selected filter cloth should be less than Calucium Silicate powder granularity.The recovery product Calucium Silicate powder obtained, can be applicable to the building material industries such as cement.
Add in described heavy phase mortar and be the acid of 2% ~ 10% with solid masses per-cent contained by heavy phase mortar and stir, calsil impurity in heavy phase mortar is fully contacted with added acid, react after 3 ~ 8 hours, carried out 1 ~ 3 concentrated and cleaning that adds water again, removing calsil impurity wherein, and make the pH value of the heavy phase mortar after removing calsil impurity in neutral.
Heavy phase mortar after removing calsil impurity is introduced the kiln basin of carbon removing device and the stirring 2 ~ 3 hours that adds water, in kiln basin, pass into the pressurized air of 0.1 ~ 0.3MPa pressure simultaneously, make uncombined carbon impurity in heavy phase mortar along with bubble floating is to kiln basin surface, scraped off by rotor segment, thus by the uncombined carbon impurity removing in this heavy phase mortar.
Carried out dehydrating process by heavy phase mortar after removing impurity, removing moisture wherein, obtains crystal silicon wafer cutting edge material silicon carbide powder product.
In the heavy phase mortar solids component adopting aforesaid method to obtain, carborundum content can reach more than 90%, and the recovery utilization rate of crystal silicon wafer cutting edge material wastewater treatment mud can reach 30% ~ 40%.This crystal silicon wafer cutting edge material wastewater treatment mud obtains resource utilization and recycles process, both avoids contaminate environment, and again for enterprise brings economic return, achieves the recycle of resource.
The following examples are only used to describe the present invention in detail, and limit the scope of the invention never in any form.
Embodiment 1: according to the method described above, mixes crystal silicon wafer cutting edge material wastewater treatment mud and water by the mass ratio of 1:1 and stirs 4 hours, obtaining mixed slurry; Then described mixed slurry is introduced wet cyclone, temperature be 50 DEG C, feeding pressure carries out flotation separation under being the condition of 0.2MPa, obtains light phase suspension and heavy phase mortar; By this light phase suspension lead 1-in plate paper blotter press, be carry out filter press concentration under the condition of 15MPa at pressure, be recycled product Calucium Silicate powder; Adding with solid masses per-cent contained by heavy phase mortar in described heavy phase mortar is 5%, concentration is the hydrochloric acid of 37% and stirs, and reacts after 5 hours, then is carried out 3 concentrated and cleanings that add water, removing calsil impurity wherein; Heavy phase mortar after removing calsil impurity is introduced the kiln basin of carbon removing device and the stirring 3 hours that adds water, in kiln basin, pass into the pressurized air of 0.3MPa pressure simultaneously, the uncombined carbon impurity in this heavy phase mortar is removed; Heavy phase mortar after removing impurity is carried out dehydrating process, obtains crystal silicon wafer cutting edge material silicon carbide powder product.In the heavy phase mortar solids component obtained by this method, carborundum content is 95%.
Embodiment 2: crystal silicon wafer cutting edge material wastewater treatment mud is recycled by the method identical with embodiment 1, difference is, the temperature of flotation separation is 50 DEG C, feeding pressure is 0.1MPa, and the hydrochloric acid that to add with solid masses per-cent contained by heavy phase mortar in heavy phase mortar be 3%, concentration is 37% carries out pickling.In the heavy phase mortar solids component obtained by this method, carborundum content is 90%.
The different-effect obtained as can be seen from embodiment 1 and embodiment 2, under separation temperature 50 DEG C, separating pressure 0.2MPa condition, in the solids component of the heavy phase mortar detected, carborundum content is 95%, and separating pressure 0.1MPa condition at the same temperature, the carborundum content of the heavy phase mortar obtained is 90%.Illustrate at separation temperature 50 DEG C, the flotation separation pressure energy that the flotation separation pressure ratio 0.1MPa that 0.2MPa is higher is lower makes the non-silicon carbide materials in mud more be separated by overflow port by flotation separation, thus the heavy phase mortar making underflow opening separate obtains higher silicon carbide contents, is convenient to follow-up silicon carbide hydrochloric acid removal of impurities process to obtain silicon carbide powder; Reduce the consumption (being only 3%) of removal of impurities auxiliary material hydrochloric acid simultaneously, just can reach the object of 5% hydrochloric acid addition removal of impurities under 0.1MPa condition.
In conjunction with the accompanying drawings and embodiments the present invention is described in detail above, but, person of ordinary skill in the field can understand, under the prerequisite not departing from present inventive concept, each design parameter in above-described embodiment can also be changed, form multiple specific embodiment, be common variation range of the present invention, describe in detail no longer one by one at this.
Claims (2)
1. a recoverying and utilizing method for crystal silicon wafer cutting edge material wastewater treatment mud, is characterized in that, comprises the following steps:
(1) mix and blend: crystal silicon wafer cutting edge material wastewater treatment mud and water mixed by the mass ratio of 1:1 ~ 1.5 and stirs 2 ~ 4 hours, obtaining mixed slurry;
(2) flotation separation: described mixed slurry is introduced wet cyclone, temperature be 20 DEG C ~ 60 DEG C, feeding pressure carries out flotation separation under being the condition of 0.1 ~ 0.3MPa, obtains light phase suspension and heavy phase mortar;
(3) filter press concentration: the calsil in described mixed slurry and uncombined carbon separate through the overflow port of wet cyclone with light phase suspension, by this light phase suspension lead 1-in plate paper blotter press, be carry out filter press concentration under the condition of 10 ~ 20MPa at pressure, be recycled product Calucium Silicate powder;
(4) a. pickling: add in described heavy phase mortar and be the acid of 2% ~ 10% with solid masses per-cent contained by heavy phase mortar and stir, calsil impurity in heavy phase mortar is fully contacted with added acid, react after 3 ~ 8 hours, carried out 1 ~ 3 concentrated and cleaning that adds water again, the calsil impurity that removing is wherein residual, and make the pH value of the heavy phase mortar after removing calsil impurity in neutral;
B. de-carbon: the heavy phase mortar of step a gained is introduced the kiln basin of carbon removing device and the stirring 2 ~ 3 hours that adds water, in kiln basin, pass into the pressurized air of 0.1 ~ 0.3MPa pressure simultaneously, make uncombined carbon impurity in this heavy phase mortar along with bubble floating is to kiln basin surface, scraped off by rotor segment, thus by the uncombined carbon impurity removing in this heavy phase mortar;
C. dehydrate: carried out dehydrating process by the heavy phase mortar of step b gained, removing moisture wherein, obtains crystal silicon wafer cutting edge material silicon carbide powder product.
2. the recoverying and utilizing method of crystal silicon wafer cutting edge material wastewater treatment mud according to claim 1, is characterized in that, the acid added in heavy phase mortar in step a to be concentration be 35% ~ 37% hydrochloric acid or concentration be the sulfuric acid of 95% ~ 98%.
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| CN201310427494.7A CN103496831B (en) | 2013-09-18 | 2013-09-18 | Recycling method of silicon wafer cutting edge material waste water treatment sludge |
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| CN201310427494.7A CN103496831B (en) | 2013-09-18 | 2013-09-18 | Recycling method of silicon wafer cutting edge material waste water treatment sludge |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104262379A (en) * | 2014-08-29 | 2015-01-07 | 浙江恒业成有机硅有限公司 | Organic silicon residue slurry treatment device and treatment method |
| CN106542827B (en) * | 2016-10-31 | 2019-02-01 | 河南易成新能源股份有限公司 | The environment-friendly preparation method thereof of silicon carbide ceramics powder |
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| JP4421882B2 (en) * | 2003-12-04 | 2010-02-24 | 日本磁力選鉱株式会社 | Effective utilization of oil-impregnated SiC sludge |
| DE102009054348A1 (en) * | 2009-11-24 | 2011-06-30 | Coenen, Wolfgang, Dipl.-Ing., 28879 | Method and apparatus for treating Si / SiC containing abrasive slurries |
| CN101817526B (en) * | 2010-04-08 | 2012-06-20 | 浙江源盛硅晶材料有限公司 | Method for recovering polyethylene glycol and silicon carbide from silicon crystal cutting waste liquid |
| CN102502643B (en) * | 2011-10-08 | 2013-06-05 | 江苏佳宇资源利用股份有限公司 | Method for realizing resource recycling of silicon powder components in waste mortar from crystalline silicon cutting |
| CN102399618B (en) * | 2011-10-08 | 2013-05-15 | 江苏佳宇资源利用股份有限公司 | Method for resource recovery of silicon carbide component from crystal silicon cutting waste mortar |
| CN102659111B (en) * | 2012-04-28 | 2014-06-25 | 南京远齐环保科技有限公司 | Method for recovering silicon and silicon carbide from silicon wafer cutting waste mortar |
| CN202898044U (en) * | 2012-09-28 | 2013-04-24 | 开封万盛新材料有限公司 | Carbon and impurity removing device |
| CN102951641B (en) * | 2012-11-01 | 2014-05-14 | 临沭山田研磨材有限公司 | Water-saving and environmental protection-type preparation method of silicon carbide micro-powder for silicon wafer wire cutting |
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Address after: Kaifeng City yuwangtai District 475000 Henan Fine Chemical Industry Park Patentee after: HENAN XINDAXIN MATERIALS CO., LTD. Address before: Kaifeng City yuwangtai District 475000 Henan Fine Chemical Industry Park Patentee before: Henan Xindaxin Materials Co., Ltd. |
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