CN103303924A - Silicon carbide micropowder recycling process flow - Google Patents
Silicon carbide micropowder recycling process flow Download PDFInfo
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- CN103303924A CN103303924A CN2013102566527A CN201310256652A CN103303924A CN 103303924 A CN103303924 A CN 103303924A CN 2013102566527 A CN2013102566527 A CN 2013102566527A CN 201310256652 A CN201310256652 A CN 201310256652A CN 103303924 A CN103303924 A CN 103303924A
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Abstract
The invention discloses a silicon carbide micropowder recycling process flow which comprises the following steps of: detection, namely, detecting the contents of moisture, oil and silicon carbide which are contained in a raw material to obtain a qualified raw material to be recycled; slurrying, namely, adding water to the raw material to be recycled, sufficiently stirring, and then screening and filtering to obtain filtered slurry; carrying out alkali wash, namely, sufficiently stirring the filtered slurry, and then adding sodium hydroxide for the alkali wash to obtain slurry subjected to the alkali wash; pickling, namely, sufficiently stirring the slurry subjected to the alkali wash, and then adding sulfuric acid for the pickling to obtain pickled slurry; rinsing, namely, rinsing the pickled slurry to obtain rinsed slurry; dewatering, namely, dewatering the rinsed slurry to obtain dried finished products; sorting, namely, sorting the dried finished products according to the granularity of silicon carbide to obtain sorted finished products; and carrying out mixed screening, namely, respectively screening and filtering the sorted finished products. The silicon carbide micropowder recycling process flow disclosed by the invention is easy and convenient to operate; and the produced silicon carbide micropowder finished product has the advantages of superior quality, high abrasion resistance, high modulus and better utilization value in the cutting of an on-line cutting industry.
Description
Technical field
The present invention relates to the cutting waste mortar that the silicon chip cutting produces in the sun power industry and reclaim the field again, relate in particular to a kind of technical process of from silicon chip dicing waste mortar, reclaiming silicon carbide micro-powder.
Background technology
" waste mortar recycling project " results from the manufacturing processed of solar cell.Especially in recent years the develop rapidly of silicon solar cell makes " waste mortar recycling project " also obtain very big expanding space.In silicon solar cell was produced, silicon chip manufacturing (silicon rod cutting) operation can produce a large amount of " waste mortars ", " useless cutting liquid " and part " waste silicon powder ", and we can be referred to as them and be " waste mortar ".These " waste mortars " are through processing treatment, can will wherein there be " silicon carbide micro-powder ", " the cutting liquid " and " silica flour " of high using value to extract, can produce very high economic benefit and social benefit, the service field of this project that Here it is and generation origin.
Current, the multifibres cutting machine (abbreviating " scroll saw " or " wire cutting machine " as) of free abrasive particle is all adopted in the silicon rod cutting, it is cutting silk (steel wire) quick travel on silicon rod by many diameter 0.12 millimeter of sheave traction, and by the grinding of " silicon carbide " and " cutting liquid ", carry, acting in conjunction such as cooling, it is hundreds of sheet even several thousand equidimension silicon chips of 0.12～0.20 millimeter that 6～12 inches polycrystalline silicon rods of diameter are once cut into thickness.In the cutting process of " wire cutting machine ", can use a large amount of " cutting liquid " and " silicon carbide ", and mixed in together with the silicon rod fine powder (silica flour) that cuts, formed a large amount of " waste mortar "." waste mortar " that all silicon chip cutting producers of the annual whole nation produce has the hundreds of thousands of ton, and the processing power of " waste mortar " recycling producer is limited, make quite a few " waste mortar " can not get dealing carefully with, cause the wasting of resources and environmental pollution, be much to be regretted." waste mortar recycling project " is a project that development prospect is very good." the low carbonization " of world environments and the anxiety of the energy promote the development rapidly of solar cell (photovoltaic) industry, thereby have opened up the vast market space for this project that the annual value of production in this space has hundred million yuans of hundreds ofs.Worldwide " low-carbon (LC) " reduces discharging the anxiety of motion and the energy, impels people to develop clean new forms of energy, and solar cell (photovoltaic) is undoubtedly our best choice.Catching this good market opportunity, all will be a quite significant thing to individual economy and social environment.It is with solid-liquid separation that present waste mortar reclaims common treatment again, solid waste is and reclaims the raw material that comprises silicon carbide micro-powder again, then solid waste is carried out slurrying, alkali cleaning, pickling, rinsing, oven dry etc. step and obtain silicon carbide micro-powder, complex process, cost recovery height, and often because the silicon carbide micro-powder that purity causes reclaiming inadequately is difficult to reach the technological standard of sun power crystal silicon wafer cutting edge material.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides the technical process that a kind of silicon chip dicing waste mortar reclaims silicon carbide micro-powder again, flow process is simply efficient, and the silicon carbide micro-powder purity height of acquisition can reach the technological standard of sun power crystal silicon wafer cutting edge material.
For achieving the above object, the present invention adopts following technical scheme:
A kind of silicon carbide micro-powder reclaims technical process again, comprises following steps:
(1) detect: moisture, oil content, silicon-dioxide and carborundum content in the solid feed that detection silicon chip dicing waste mortar solid-liquid separation obtains obtain raw material to be recycled;
(2) slurrying: raw material to be recycled is added water fully stir the back screening and filtering, obtain to filter disposed slurry;
(3) alkali cleaning: after will filtering disposed slurry and fully stirring, drop into the low alkali of sodium hydroxide and carry out alkali cleaning, obtain the alkali cleaning disposed slurry;
(4) pickling: after the alkali cleaning disposed slurry fully stirred, drop into sulfuric acid and carry out pickling, obtain the pickling disposed slurry;
(5) rinsing: the pickling disposed slurry is carried out rinsing, obtain the rinsing disposed slurry;
(6) dehydration: the rinsing disposed slurry is dewatered, obtain oven dry back finished product;
(7) branch: classify finished product behind the acquisition branch to drying the back finished product according to carborundum granularity;
(8) mix sieve: finished product behind the branch is carried out screening and filtering respectively.
Further, the ratio of step (2) raw material to be recycled and water is 2:1, and after fully stirring, adopts the supersonic filter screening and filtering.
Further, sodium hydrate content 〉=99% in the low alkali of step (3) sodium hydroxide, the ratio that drops into the low alkali of sodium hydroxide during alkali cleaning is 1.5%～2% of filtration disposed slurry, and the alkali cleaning number of times is 8～10 times; Qualified when alkali cleaning disposed slurry pH value≤9.0, carborundum content 〉=98%.
Further, it is 2%～2.5% of alkali cleaning disposed slurry that step (4) drops into the sulfuric acid ratio, and after abundant stirring and precipitation reaction, with the spent acid emptying, obtains the pickling disposed slurry.
Further, adopt tap water to carry out rinsing to the pickling disposed slurry in the step (5), when rinsing disposed slurry pH value is 6.5～7.5, use the rinsing of pure water secondary instead; When rinsing disposed slurry pH value is 6～7, qualified when specific conductivity＜20, carborundum content 〉=99%.
Further, step (6) adopts centrifuge dewatering, when dehydration back water content≤8%, adopts flash distillation machine or microwave drying second dehydration, water content behind the second dehydration≤0.1%.
Further, step (7) adopts ultrasonic vibration sieve screening and filtering, make branch after finished product scattered, do not unite, epigranular does not have impurity.
Beneficial effect: (1) this technical process is simple, easy and simple to handle, and owing to adopt the low alkali of general sodium hydroxide and sulfuric acid, cost is low; (2) this technical process is provided with the branch flow process, can reclaim the different model finished product according to carborundum granularity, makes the silicon carbide micro-powder final product quality of production superior, and it is higher to reclaim benefit; (3) this process using ultrasonic vibration sieve screening and filtering, finished product is scattered, does not unite, and epigranular does not have impurity.
Description of drawings
Fig. 1 is this process flow diagram.
Embodiment
Below in conjunction with accompanying drawing the present invention is done further explanation.
As shown in Figure 1, a kind of silicon carbide micro-powder provided by the invention reclaims technical process again, comprises the steps:
(1) detect: moisture, oil content, silicon-dioxide and carborundum content in the solid feed that detection silicon chip dicing waste mortar solid-liquid separation obtains obtain qualified raw material to be recycled;
(2) slurrying: raw material to be recycled is added water fully stir the back screening and filtering, obtain to filter disposed slurry;
(3) alkali cleaning: after will filtering disposed slurry and fully stirring, drop into the low alkali of sodium hydroxide and carry out alkali cleaning, obtain the alkali cleaning disposed slurry;
(4) pickling: after the alkali cleaning disposed slurry fully stirred, drop into sulfuric acid and carry out pickling, obtain the pickling disposed slurry;
(5) rinsing: the pickling disposed slurry is carried out rinsing, obtain the rinsing disposed slurry;
(6) dehydration: the rinsing disposed slurry is dewatered, obtain oven dry back finished product;
(7) branch: classify finished product behind the acquisition branch to drying the back finished product according to carborundum granularity;
(8) mix sieve: finished product behind the branch is carried out screening and filtering respectively.
Below in conjunction with specific examples in the factory whole process flow is described in detail:
(1) detect: the solid feed that the silicon chip dicing waste mortar solid-liquid separation is obtained detects, and the content of its contained humidity, oil content, silicon-dioxide, silicon carbide and impurity what detect.
Sampling is according to coming 20% of goods tonnage, sampling per ton during detection.At first carry out moisture measurement, sample of sample mixing per ton of sampling, take by weighing 50 grams, be accurate to 0.1 gram.Then sample is put into thermostatic drying chamber.With 120 ° of C of temperature furnishing, oven dry is 120 minutes in loft drier, measures moisture; Carry out oil content then and detect, roasted at multifunctional electric furnace except the sample of moisture last time, make the oil content combustion of the inside clean, take by weighing the content of oil content at balance; Order number by microscopic examination silicon carbide at last.
(2) slurrying: throw into and add water in the slurrying pond and stir detecting good raw material, long 2.3 meters of slurrying pond, wide 1.4 meters high 1.3 meters, every pond feeds intake about 2 tons, and the ratio 1:2 of water and raw material stirred 1 hour.The slurry that stirs is sent into the ultrasonic vibration sieve by pipeline filter, ultrasonic vibration sieve screen cloth 180# squeezes into the alkali cleaning of alkali cleaning pond then
(3) alkali cleaning: squeeze into the alkali cleaning of alkali cleaning pond filtering good slurry with pump, long 6.3 meters of alkali cleaning pond, wide 1.3 meters, high 1.2 meters, 24 altogether, every pond slip is controlled between 4.2 ± 0.3 tons.Must fully stir during alkali cleaning, churning time adds low alkali (sodium hydrate content 〉=a 99%) bag about 2 hours then, reacts 2-3 hour, and ﹙ adjusts reaction times length ﹚ according to seasonal variation, continues to drop into low alkali then, thoroughly is purpose to react.The ratio that adds low alkali is 1.5%-2%, and the reaction times is 12 hours, and the alkali cleaning number of times is generally controlled in 8-10 time again.With slurry PH≤9.0, carborundum content 〉=98% alkali cleaning pond is qualified after the alkali cleaning.
(4) pickling: the good slip of alkali cleaning squeezed into pump carry out pickling in the acid wash drum, 1.9 meters of the diameters of acid wash drum, high 1.1 meters, about about 1.2 tons of every barrel material adds the preceding fully stirring of acid, and the ratio that adds sulfuric acid is 2%-2.5%, add the acid back and fully stir precipitation reaction in 30 minutes, reaction times is 12 hours, and question response finishes the back top spent acid water emptying, sends into rinsing bath.
(5) rinsing: the slurry after the pickling is added the tap water rinsing earlier, and 4-6 back of rinsing pH value reaches about 7, uses the pure water rinsing again 1-2 time, reach 6-7 with rinsing disposed slurry pH value, specific conductivity reaches below 20, and carborundum content reaches more than 99%, and opacity clearly then is qualified.
(6) dehydration: centrifuge dewatering is adopted in dehydration, the good slurry of rinsing is squeezed into whizzer with pump dewater.Each bench centrifuge, about 300 kilograms of dnockouts, dewatering time are about 20 minutes, and dehydration back water content≤8% is used flash distillation machine or microwave drying then, oven dry back water content≤0.1%.
(7) branch: the raw material good oven dry is divided into qualified finished product by the branch machine, and finished product has three numbers: 1200#, 1500#, 2000#.
The finished product standard
| The order number | D3 | D50 | D94 | F.C | Fe203 | SiC | PH | Electricity is led |
| 1200# | ≤15 | 10±0.3 | ≥6.6 | ≤0.15 | ≤0.15 | ≥99% | 5-7 | ≤50 |
| 1500# | ≤13 | 8.3±0.3 | ≥5.6 | ≤0.15 | ≤0.15 | ≥99% | 5-7 | ≤50 |
| 2000# | ≤11 | 6.9±0.3 | ≥4.6 | ≤0.15 | ≤0.15 | ≥98.5 | 5-7 | ≤50 |
(8) mix sieve: dividing good finished product to sieve after ultrasonic vibration, the purpose of sieving makes finished product scattered, does not unite, and epigranular does not have impurity.
The easy operation of technology that the present invention proposes, the silicon carbide micro-powder scatter coefficient height that washes out is not united, and cost is low, and the silicon carbide micro-powder final product quality of production is superior, and wear resistance is strong, modulus height, better utility value in the online cutting industry cutting.
The above only is preferred implementation of the present invention; be noted that for those skilled in the art; under the prerequisite that does not break away from the principle of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. a silicon carbide micro-powder reclaims technical process again, it is characterized in that comprising following steps:
(1) detect: moisture, oil content, silicon-dioxide and carborundum content in the solid feed that detection silicon chip dicing waste mortar solid-liquid separation obtains obtain raw material to be recycled;
(2) slurrying: raw material to be recycled is added water fully stir the back screening and filtering, obtain to filter disposed slurry;
(3) alkali cleaning: after will filtering disposed slurry and fully stirring, drop into the low alkali of sodium hydroxide and carry out alkali cleaning, obtain the alkali cleaning disposed slurry;
(4) pickling: after the alkali cleaning disposed slurry fully stirred, drop into sulfuric acid and carry out pickling, obtain the pickling disposed slurry;
(5) rinsing: the pickling disposed slurry is carried out rinsing, obtain the rinsing disposed slurry;
(6) dehydration: the rinsing disposed slurry is dewatered, obtain oven dry back finished product;
(7) branch: classify finished product behind the acquisition branch to drying the back finished product according to carborundum granularity;
(8) mix sieve: finished product behind the branch is carried out screening and filtering respectively.
2. a kind of silicon carbide micro-powder according to claim 1 reclaims technical process again, it is characterized in that: the ratio of step (2) raw material to be recycled and water is 2:1, and adopts the supersonic filter screening and filtering.
3. a kind of silicon carbide micro-powder according to claim 1 reclaims technical process again, it is characterized in that: sodium hydrate content 〉=99% in the low alkali of step (3) sodium hydroxide, the ratio that drops into the low alkali of sodium hydroxide during alkali cleaning is 1.5%～2% of filtration disposed slurry, and the alkali cleaning number of times is 8～10 times; Qualified when alkali cleaning disposed slurry pH value≤9.0, carborundum content 〉=98%.
4. a kind of silicon carbide micro-powder according to claim 1 reclaims technical process again, it is characterized in that: it is 2%～2.5% of alkali cleaning disposed slurry that step (4) drops into the sulfuric acid ratio, and after abundant stirring and precipitation reaction, with the spent acid emptying, thereby obtain the pickling disposed slurry.
5. a kind of silicon carbide micro-powder according to claim 1 reclaims technical process again, it is characterized in that: adopt tap water to carry out rinsing to the pickling disposed slurry in the step (5), when rinsing disposed slurry pH value is 6.5～7.5, use the rinsing of pure water secondary instead; When rinsing disposed slurry pH value is 6～7, qualified when specific conductivity＜20, carborundum content 〉=99%.
6. a kind of silicon carbide micro-powder according to claim 1 reclaims technical process again, it is characterized in that: step (6) adopts centrifuge dewatering, when dehydration back water content≤8%, adopt flash distillation machine or microwave drying second dehydration, water content behind the second dehydration≤0.1%.
7. a kind of silicon carbide micro-powder according to claim 1 reclaims technical process again, it is characterized in that: step (7) adopts ultrasonic vibration sieve screening and filtering.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179715A (en) * | 2016-06-24 | 2016-12-07 | 河南易成新能源股份有限公司 | Crystal silicon wafer cutting edge material fine powder minimizing technology |
| CN106335902A (en) * | 2016-08-24 | 2017-01-18 | 山田研磨材料有限公司 | Method for recovering carbonized silica powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982536A (en) * | 2010-11-02 | 2011-03-02 | 林小妹 | Method for recovering silicon carbide and polyethylene glycol cutting fluid from waste silicon wafer cutting fluid |
| CN103030144A (en) * | 2011-09-28 | 2013-04-10 | 汇隆科技有限公司 | Method for recovering silicon carbide in waste liquid |
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- 2013-06-25 CN CN2013102566527A patent/CN103303924A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982536A (en) * | 2010-11-02 | 2011-03-02 | 林小妹 | Method for recovering silicon carbide and polyethylene glycol cutting fluid from waste silicon wafer cutting fluid |
| CN103030144A (en) * | 2011-09-28 | 2013-04-10 | 汇隆科技有限公司 | Method for recovering silicon carbide in waste liquid |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179715A (en) * | 2016-06-24 | 2016-12-07 | 河南易成新能源股份有限公司 | Crystal silicon wafer cutting edge material fine powder minimizing technology |
| CN106179715B (en) * | 2016-06-24 | 2018-07-20 | 河南易成新能源股份有限公司 | Crystal silicon wafer cutting edge material fine powder minimizing technology |
| CN106335902A (en) * | 2016-08-24 | 2017-01-18 | 山田研磨材料有限公司 | Method for recovering carbonized silica powder |
| 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 |
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Application publication date: 20130918 |