CN105621414A - Method for recovering silicon carbide from waste mortar of crystal silicon wire cutting - Google Patents
Method for recovering silicon carbide from waste mortar of crystal silicon wire cutting Download PDFInfo
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- CN105621414A CN105621414A CN201510104470.7A CN201510104470A CN105621414A CN 105621414 A CN105621414 A CN 105621414A CN 201510104470 A CN201510104470 A CN 201510104470A CN 105621414 A CN105621414 A CN 105621414A
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Abstract
The invention provides a method for recovering silicon carbide from waste mortar of crystal silicon wire cutting. The method comprises the following steps: 1) waste mortar stirring; 2) slurry preparation; 3) filter pressing separation; 4) swirl washing: 5) alkali washing; 6) acid pickling; 7) drying, sieving and packing. The silicon carbide recovered according to the method is high in purity and particle size uniformity, and can be directly used for crystal silicon wire cutting.
Description
Technical field
The present invention relates to a kind of method reclaiming carborundum from crystal silicon waste mortar for wire cutting.
Background technology
As the important step of photovoltaic industry chain, producing waste mortar in crystal silicon line cutting process, waste mortar is a kind of grey black thickness solid-liquid mixture, containing carborundum, silica flour, ferrum, Polyethylene Glycol, water impurity etc. Slightly hygroscopicity, not volatile, stable chemical nature, water, difficult combustion can be dissolved in, transport by Treatment of Dangerous Chemical Wastes, sealed type storage.
Waste mortar is a kind of industrial waste, if do not processed, it will produce severe contamination, but, carborundum and Polyethylene Glycol in waste mortar are then the important raw and processed materials in the cutting of crystal silicon line, how to reclaim carborundum and Polyethylene Glycol from waste mortar, are popular research topics in recent years.
But, traditional recovery process, the resource cost amount such as method complexity, soda acid is big, and reclaim, the carborundum that regenerates and Polyethylene Glycol quality do not meet regeneration requirements, it is impossible to being directly used in the cutting of crystal silicon line, and organic efficiency is low, cost is high.
Summary of the invention
For solving above-mentioned Problems existing, it is an object of the invention to provide a kind of method reclaiming carborundum from crystal silicon waste mortar for wire cutting, the carborundum purity reclaim, regenerated is high, epigranular, can be directly used for the cutting of crystal silicon line.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
A kind of method reclaiming carborundum from crystal silicon waste mortar for wire cutting, comprises the steps:
1) waste mortar stirring
Waste mortar is delivered in agitator and stir, step up agitator shaft speed, when in bucket, waste mortar Starch Level center occurs that the vortex of rule and vortex bore the end and the liquid level discrepancy in elevation when 50 ~ 80mm, stop speed-raising, keep stabilization of speed, after the waste mortar solid-liquid dispersing in bucket to be mixed is uniform, stop stirring;
2) slurry preparation
Add water in stirred tank, start stirring, then to supplying step in stirred tank 1) stirring after waste mortar, control stirring temperature in the kettle��70 DEG C, after waste mortar feed in raw material, continuation stirring 30 ~ 40min, obtain slurry;
3) filter pressing separates
By step 2) preparation gained slurry delivers to pressure filter and carries out filter pressing separating treatment, feeding pressure��0.1MPa, obtains filter cake and filtrate, filter cake is sent into mortar stirring tank, it is configured to suspension, filtrate is sent into pressing filtering liquid collecting tank, remain to reclaim the Polyethylene Glycol cutting liquid in filtrate;
4) eddy flow washing
The cyclone water of 10 ~ 14M3 is injected in eddy flow mortar preparing tank, open stirring, by step 3) filter cake preparation suspension be transported in described eddy flow mortar preparing tank, obtain mortar suspension, gained mortar suspension solid content is between 15% ~ 25%, then mortar suspension is carried out six stage countercurrent washings, obtain overflow suspension and underflow suspension, concentration filter pressing is carried out respectively with pressure filter, underflow suspension is after filter pressing, filtrate, as eddy flow the recycled process water, enters eddy flow filter pressing water collecting tank, and filter cake enters slurry commanding tank and is configured to underflow slurry;
5) alkali cleaning
By step 4) in the underflow slurry that obtains deliver to caustic treater alkali liquor and carry out alkali cleaning, wash 4 ~ 6h, the slurry after washing is delivered to alkali cleaning band filter and is rinsed, and controlling washing disposed slurry pH value is 7 ~ 8, obtains filter cake and filtrate;
6) pickling
By step 5) gained filter cake is configured to slurry, delivers to pickling tank acid solution and carries out pickling, washs 4 ~ 6h, and the slurry after washing is delivered to pickling band filter and is rinsed, and controlling washing disposed slurry pH value is 6 ~ 7, obtains filter cake and filtrate;
7) dry, sieve, pack
By step 6) gained filter cake feeding plate centrifuge dehydrate, it is then fed into three steaming drying machines and carries out expansion drying, material after expansion drying is delivered to cyclopneumatic separator and carries out sub-material, deliver to batch mixer again, after stirring 25 ~ 35min, vibrosieve is sieved, and obtains finished product carborundum, packing packaging.
Further, moisture��8% in described waste mortar, silica flour content��7wt%, pH value is 6 ~ 7.
And, described step 3) in carry out five filter pressings by 3 pressure filter being sequentially connected with.
Separately, described step 3) after filter pressing processes, moisture content��60% in filtrate, moisture content��30% in filter cake.
Separately have, described step 4) in by one ~ Pyatyi underflow tank and the first ~ the 6th eddy flow tank realize six stage countercurrents washing, from underflow tank, obtain described underflow suspension, from eddy flow tank, obtain described overflow suspension.
Again, described step 4) in grain diameter >=standard value D94 in bed material suspension.
Further, described step 4) in overfall suspension after filter pressing, filtrate, as eddy flow the recycled process water, enters eddy flow filter pressing water collecting tank, and filter cake is then as pottery fine powder packaging warehouse-in.
And, described step 7) in, moisture content��0.2% after plate centrifuge dehydrate.
Again, described step 7) in screening operation include: start conveying worm and enter first ultrasonic activation sieve and once sieve, carry out regrading again through second ultrasonic activation sieve.
The present invention has the beneficial effects that:
3 pressure filter are set, it is achieved 5 filter pressing separatory of waste mortar slurry are processed, and slurry is through six countercurrent washings, hence it is evident that promote the filter pressing treatment effeciency to waste mortar slurry, promote waste mortar regeneration quality; In regeneration gained carborundum powder, carborundum content >=98%, elemental silicon content��1%, can be directly used for the cutting of crystal silicon line.
Accompanying drawing explanation
Fig. 1 is the process chart of the method reclaiming carborundum from crystal silicon waste mortar for wire cutting described in the embodiment of the present invention.
Detailed description of the invention
Referring to Fig. 1, the method reclaiming carborundum from crystal silicon waste mortar for wire cutting of the present invention, comprise the steps:
1) waste mortar stirring
Waste mortar is delivered in agitator and stir, step up agitator shaft speed, when in bucket, waste mortar Starch Level center occurs that the vortex of rule and vortex bore the end and the liquid level discrepancy in elevation when 50 ~ 80mm, stop speed-raising, keep stabilization of speed, after the waste mortar solid-liquid dispersing in bucket to be mixed is uniform, stop stirring;
2) slurry preparation
Add water in stirred tank, start stirring, then to supplying step in stirred tank 1) stirring after waste mortar, control stirring temperature in the kettle��70 DEG C, after waste mortar feed in raw material, continuation stirring 30 ~ 40min, obtain slurry;
3) filter pressing separates
By step 2) preparation gained slurry delivers to pressure filter and carries out filter pressing separating treatment, feeding pressure��0.1MPa, obtains filter cake and filtrate, filter cake is sent into mortar stirring tank, it is configured to suspension, filtrate is sent into pressing filtering liquid collecting tank, remain to reclaim the Polyethylene Glycol cutting liquid in filtrate;
4) eddy flow washing
The cyclone water of 10 ~ 14M3 is injected in eddy flow mortar preparing tank, open stirring, by step 3) filter cake preparation suspension be transported in described eddy flow mortar preparing tank, obtain mortar suspension, gained mortar suspension solid content is between 15% ~ 25%, then mortar suspension is carried out six stage countercurrent washings, obtain overflow suspension and underflow suspension, concentration filter pressing is carried out respectively with pressure filter, underflow suspension is after filter pressing, filtrate, as eddy flow the recycled process water, enters eddy flow filter pressing water collecting tank, and filter cake enters slurry commanding tank and is configured to underflow slurry;
5) alkali cleaning
By step 4) in the underflow slurry that obtains deliver to caustic treater alkali liquor and carry out alkali cleaning, wash 4 ~ 6h, the slurry after washing is delivered to alkali cleaning band filter and is rinsed, and controlling washing disposed slurry pH value is 7 ~ 8, obtains filter cake and filtrate;
6) pickling
By step 5) gained filter cake is configured to slurry, delivers to pickling tank acid solution and carries out pickling, washs 4 ~ 6h, and the slurry after washing is delivered to pickling band filter and is rinsed, and controlling washing disposed slurry pH value is 6 ~ 7, obtains filter cake and filtrate;
7) dry, sieve, pack
By step 6) gained filter cake feeding plate centrifuge dehydrate, it is then fed into three steaming drying machines and carries out expansion drying, material after expansion drying is delivered to cyclopneumatic separator and carries out sub-material, deliver to batch mixer again, after stirring 25 ~ 35min, vibrosieve is sieved, and obtains finished product carborundum, packing packaging.
Further, moisture��8% in described waste mortar, silica flour content��7wt%, pH value is 6 ~ 7.
And, described step 3) in carry out five filter pressings by 3 pressure filter being sequentially connected with.
Separately, described step 3) after filter pressing processes, moisture content��60% in filtrate, moisture content��30% in filter cake.
Separately have, described step 4) in by one ~ Pyatyi underflow tank and the first ~ the 6th eddy flow tank realize six stage countercurrents washing, from underflow tank, obtain described underflow suspension, from eddy flow tank, obtain described overflow suspension.
Again, described step 4) in grain diameter >=standard value D94 in bed material suspension.
Further, described step 4) in overfall suspension after filter pressing, filtrate, as eddy flow the recycled process water, enters eddy flow filter pressing water collecting tank, and filter cake is then as pottery fine powder packaging warehouse-in.
And, described step 7) in, moisture content��0.2% after plate centrifuge dehydrate.
Again, described step 7) in screening operation include: start conveying worm and enter first ultrasonic activation sieve and once sieve, carry out regrading again through second ultrasonic activation sieve.
The present invention each operation index detection method is as shown in table 1:
It should be noted that above example is only in order to illustrate technical scheme and unrestricted. Although the present invention being described in detail with reference to preferred embodiment, it will be understood by those within the art that, the technical scheme of invention can being modified or equivalent replacement, without deviating from the scope of technical solution of the present invention, it all should be encompassed in scope of the presently claimed invention.
Claims (9)
1. the method reclaiming carborundum from crystal silicon waste mortar for wire cutting, it is characterised in that comprise the steps:
Waste mortar stirs
Waste mortar is delivered in agitator and stir, step up agitator shaft speed, when in bucket, waste mortar Starch Level center occurs that the vortex of rule and vortex bore the end and the liquid level discrepancy in elevation when 50 ~ 80mm, stop speed-raising, keep stabilization of speed, after the waste mortar solid-liquid dispersing in bucket to be mixed is uniform, stop stirring;
Slurry preparation
Add water in stirred tank, start stirring, then to supplying step in stirred tank 1) stirring after waste mortar, control stirring temperature in the kettle��70 DEG C, after waste mortar feed in raw material, continuation stirring 30 ~ 40min, obtain slurry;
Filter pressing separates
By step 2) preparation gained slurry delivers to pressure filter and carries out filter pressing separating treatment, feeding pressure��0.1MPa, obtains filter cake and filtrate, filter cake is sent into mortar stirring tank, it is configured to suspension, filtrate is sent into pressing filtering liquid collecting tank, remain to reclaim the Polyethylene Glycol cutting liquid in filtrate;
Eddy flow washs
10 ~ 14M is injected in eddy flow mortar preparing tank3Cyclone water, open stirring, by step 3) filter cake preparation suspension be transported in described eddy flow mortar preparing tank, obtain mortar suspension, gained mortar suspension solid content is between 15% ~ 25%, then mortar suspension is carried out six stage countercurrent washings, obtain overflow suspension and underflow suspension, concentration filter pressing is carried out respectively with pressure filter, underflow suspension is after filter pressing, filtrate, as eddy flow the recycled process water, enters eddy flow filter pressing water collecting tank, and filter cake enters slurry commanding tank and is configured to underflow slurry;
Alkali cleaning
By step 4) in the underflow slurry that obtains deliver to caustic treater alkali liquor and carry out alkali cleaning, wash 4 ~ 6h, the slurry after washing is delivered to alkali cleaning band filter and is rinsed, and controlling washing disposed slurry pH value is 7 ~ 8, obtains filter cake and filtrate;
Pickling
By step 5) gained filter cake is configured to slurry, delivers to pickling tank acid solution and carries out pickling, washs 4 ~ 6h, and the slurry after washing is delivered to pickling band filter and is rinsed, and controlling washing disposed slurry pH value is 6 ~ 7, obtains filter cake and filtrate;
Dry, sieve, pack
By step 6) gained filter cake feeding plate centrifuge dehydrate, it is then fed into three steaming drying machines and carries out expansion drying, material after expansion drying is delivered to cyclopneumatic separator and carries out sub-material, deliver to batch mixer again, after stirring 25 ~ 35min, vibrosieve is sieved, and obtains finished product carborundum, packing packaging.
2. the method reclaiming carborundum from crystal silicon waste mortar for wire cutting according to claim 1, it is characterised in that moisture��8% in described waste mortar, silica flour content��7wt%, pH value is 6 ~ 7.
3. the method reclaiming carborundum from crystal silicon waste mortar for wire cutting according to claim 1, it is characterised in that described step 3) in carry out five filter pressings by 3 pressure filter being sequentially connected with.
4. the method reclaiming carborundum from crystal silicon waste mortar for wire cutting according to claim 1 or 3, it is characterised in that described step 3) filter pressing process after, moisture content��60% in filtrate, moisture content��30% in filter cake.
5. the method reclaiming carborundum from crystal silicon waste mortar for wire cutting according to claim 1, it is characterized in that, described step 4) in by one ~ Pyatyi underflow tank and the first ~ the 6th eddy flow tank realize six stage countercurrents washing, from underflow tank, obtain described underflow suspension, from eddy flow tank, obtain described overflow suspension.
6. the method reclaiming carborundum according to claim 1 or 5 from crystal silicon waste mortar for wire cutting, it is characterised in that described step 4) in grain diameter >=standard value D94 in bed material suspension.
7. the method reclaiming carborundum according to claim 1 or 5 from crystal silicon waste mortar for wire cutting, it is characterized in that, described step 4) in overfall suspension after filter pressing, filtrate is as eddy flow the recycled process water, entering eddy flow filter pressing water collecting tank, filter cake is then as pottery fine powder packaging warehouse-in.
8. the method reclaiming carborundum from crystal silicon waste mortar for wire cutting according to claim 1, it is characterised in that described step 7) in, moisture content��0.2% after plate centrifuge dehydrate.
9. the method reclaiming carborundum from crystal silicon waste mortar for wire cutting according to claim 1, it is characterized in that, described step 7) in screening operation include: start conveying worm enter first ultrasonic activation sieve once sieve, again through second ultrasonic activation sieve carry out regrading.
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Cited By (3)
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| CN105856073A (en) * | 2016-06-20 | 2016-08-17 | 福建晶安光电有限公司 | Recovery method of sapphire polishing waste liquid |
| CN106335902A (en) * | 2016-08-24 | 2017-01-18 | 山田研磨材料有限公司 | Method for recovering carbonized silica powder |
| CN107116708A (en) * | 2017-06-14 | 2017-09-01 | 太仓协鑫光伏科技有限公司 | A kind of method for analyzing the front and rear silicon-carbide particle change of mortar cutting |
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Cited By (6)
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| CN106335902B (en) * | 2016-08-24 | 2019-02-19 | 山田研磨材料有限公司 | A kind of recovery method of silicon carbide micro-powder |
| CN107116708A (en) * | 2017-06-14 | 2017-09-01 | 太仓协鑫光伏科技有限公司 | A kind of method for analyzing the front and rear silicon-carbide particle change of mortar cutting |
| CN107116708B (en) * | 2017-06-14 | 2019-05-28 | 苏州功业肆点零智能科技有限公司 | A method of analysis mortar cutting front and back silicon-carbide particle variation |
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