CN101475172A - Recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder - Google Patents
Recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder Download PDFInfo
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- CN101475172A CN101475172A CNA2008100502055A CN200810050205A CN101475172A CN 101475172 A CN101475172 A CN 101475172A CN A2008100502055 A CNA2008100502055 A CN A2008100502055A CN 200810050205 A CN200810050205 A CN 200810050205A CN 101475172 A CN101475172 A CN 101475172A
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Abstract
The invention relates to a process for reclaiming, purifying and classifying high-purity ultrafine carborundum, which is capable of producing No. 4000, No. 6000 and No. 8000 high-purity ultrafine micropowder by classification. Under the condition of semiworks production or batch production line, the process utilizes a flocculant addition method to reduce capacity of equipment and improves the reclaiming rate of 95 percent above; the process adopts a multiple diverse acid-base chemical purification method so that the content of the carborundum exceeds over 94 percent; and the process adopts a suspension method for classification and overcomes static electricity, so that particle clusters concentrate and granularity is evenly distributed and the quality of a product fully exceeds national standard and international standard and improves production efficiency.
Description
One, technical field
The present invention relates to recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder.
Two, background technology
High purity superfine silicon carbide micro powder is mainly used in the raw material of silicon carbide ceramics, silicon carbide ceramics village material is widely used in fields such as aerospace, petrochemical complex, mechano-electronic owing to have wear-resisting, corrosion-resistant, good characteristics such as hot strength is high, high thermal conductance, broad stopband.Especially high purity superfine silicon carbide micro powder has become indispensable main raw in fields such as grinding materials and grinding tool, high grade refractory, engineering ceramics, resistance heater, metallurgical deoxidation especially.
Aspect the recovery of silicon carbide, have micro mist is obtained 0.3 μ m α-SiC[and wraps China, Li Suping through repeatedly washing, filter dehydration oven dry back recovery. grinding materials and grinding tool and grinding 1995; 87:36-39]; Aspect purification, the useful vitriol oil carries out acid treatment, carries out smart purification processes with the oxygen fluoric acid then.Employing preoxidation is arranged, high temperature decarburization oxygen crystallization treatment process can prepare the higher β of purity-SiC super-fine powder [Xie Kai etc. carbonate journal 1996; 3:262-268]; Have micro mist is at first passed through the sodium hydroxid alkali cleaning, add hydrogen-oxygen acid and ρ=1.19g/cm3 concentration 38% concentrated hydrochloric acid of 1:1 then, add concentrated hydrochloric acid again, stirred 10～12 hours, static 10～12 hours, add deionized water, stir, press filtration adds deionized water again, stir, the pressure filter press filtration repeats 3-4 time, the highly purified silicon carbide micro-powder of oven dry pulverizing acquisition after cleaning [Chinese patent: a kind of purification method of ultra fine silicon carbide powder (application number: 200610115158.9)]; Aspect classification, have and utilize grading machine, ionic method [Chinese patent: a kind of production method of fine powder of silicon carbide (application number: 200510047465.3)], divide impeller that micro mist has been realized classification [Chinese patent: the analytical equipment of pulverizing mill (application number: 200520074206.5)] respectively.
Prior art can reach technology and specification of quality when small-scale production, but nearly all is not suitable for large-scale industrial production.
And difference of this project and positively effect are: reclaim process using flocculation agent method and reclaim the silicon carbide micro-powder of 0-3 μ m, and do not influence grading effect; The purifying technique of high-purity silicon carbide adopts 10%HCl and 10%H2SO
4And the 5%NaOH novel process of processing; Utilize the suspension method novel process, the super differential of silicon carbide is carried out classification.Adopt this integrated artistic can the large-scale industrialized production high purity superfine silicon carbide micro powder.
Three, summary of the invention
General technical comprises recovery, purification, classification three aspects:
Reclaim: add the flocculation agent sodium polyacrylate and quicken sedimentation and can reclaim and do not influence classification.
Purify: the novel process that adopts 10%HCl and 10%H2SO4 and 5%NaOH to process.
Classification: hydraulic classification, utilize suspension method.Material in the classification jar, by jar hypocone water inlet, make relative fines be suspended in the classification jar above, carry out abundant classification after, aspirate out the product of same specification again.Tell #4000, #6000, three kinds of specification products of #8000 from fine to coarse one by one, grading effect is good, the production efficiency height.
Four, embodiment
One, reclaims
1, raw material sources
Use the silicon carbide bulk of Baishan energy silicon carbide limited liability company.
(1) telling the fines less than #3000 that contains in the overflow water of slurry tank of #2000-0 in the grading operation reclaims.
When (2) dividing #2000-#3000 in classification, the slip of telling earlier less than 3000-0 reclaims.
(3) slip in the overflow water in #2000-#8000 finished product pond reclaims.
More than the fines slurry at three places all flow into and reclaim settling tank and reclaim.
2, removal process and method
According to entering the slip flow that reclaims in the settling tank, with the flocculation agent sodium polyacrylate after the chemicals feeder interpolation dilution, every cubic metre is added 60-100g.Adding dose increases and decreases with sedimentation effect.
Two, purify
Purification process is through three hypo acid alkali cleanings
Add in the soda acid cask washing (φ 2000 * 2000) earlier for the first time, raw material (#4000-0) discharges water after sedimentation in 16 hours for 1.2 tons, starts stirring after discharging water and adds sulfuric acid (H simultaneously
2SO
4) 80-100kg, heat simultaneously, be warmed to 70-80 ℃, back insulation 4 hours, (be not with #8000 to be as the criterion when discharging water, begin to discharge water, discharge water and wash acid, open and precipitate 6-10 hour again after stirring through sedimentation in 6-8 hour with coarse fodder with the dewatering outlet, discharge water again, through 4-6 time, make the acid pH value of slip reach 6-7, repeated hydrogenation sodium oxide (NaOH) 10-20kg, and heat, open stirring, be warmed to 70-80 ℃, be incubated 2 hours, add and precipitate 6-10 hour after water stirs and discharge water again, through 4-6 time, make the slip alkaline ph value reach 8-9.
For the second time add hydrochloric acid (Hcl) 20-40kg and add sulfuric acid (H
2SO
4) 30-40kg, heat simultaneously (following work is with for the first time identical).
Add hydrochloric acid (Hcl) 20-30kg for the third time, and add sulfuric acid (H
2SO
4) 30-40kg, heat simultaneously (following work is with for the second time identical).
Above purification process main purpose is to remove metallic iron and ferric oxide, also can remove impurity such as partial oxidation calcium, magnesium oxide, aluminum oxide and free silica, and the carborundum content purity of product is improved.
Three, classification
1, water treatment
Divide so thin product to the water quality requirement height, water also needs to increase electrodialytic water and handles through outside normal purification, softening, electrical conductivity of water is reduced, by original electrical conductivity of water is that 350 μ S/cm drop to below the 100 μ S/cm, has reduced the attraction of positive and negative charge, is convenient to classification.
2, dispersion agent is carried out processing treatment
Common dispersion agent water glass, process water glass contains granule foreign, and directly using to increase product impurity reduction product purity.Re-use through smart the filtration.
3, suspension method hydraulic classification
Slip after soda acid washed adds dispersion agent and fully stirs (adding and disperseing dosage is 1.8-3kg).After particle is fully disperseed on inspection, pump in the groove in the classification jar from stirring, introduce water with the time stage pot bottom and upwards flow (discharge 100-200L/h), after classification jar water was full, water was by the fines of last upflow tube outflow＜#8000.The fines elution time should be 24-36 hour.
Fines is told the back increases discharge (200-300L/h), begins branch #8000's.With the dark slip of suction tube sucking-off classification jar top 300-500mm, wait the classification jar after full, to aspirate again again.After #8000 had divided, increased water flow amount (300-600t/h) began branch #6000's again to aspirate repeatedly (about 3-5 time).Method by above minute #8000 is carried out classification, divided #6000, and increased water flow amount (500-800l/h) begins branch #4000 again, divides #4000's with top same working method.Reduce discharge after having divided, flow is 100-200l/h, etc. the material of #4000 emits, and is classified as end.
Above classification process increases water yield size, and same specification grading suction number of times all will be checked size composition, whether meets product granularity and forms standard-required and decide.
Claims (3)
1. recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder comprises following processing step:
(1) reclaims
Telling the fines less than #3000 that contains in the overflow water of slurry tank of #2000-0 in the grading operation reclaims;
When dividing #2000-#3000 in classification, the slip of telling earlier less than 3000-0 reclaims;
Slip in the overflow water in #2000-#8000 finished product pond reclaims;
More than the fines slurry at three places all flow into and reclaim settling tank and reclaim.
According to entering the slip flow that reclaims in the settling tank, with the flocculation agent sodium polyacrylate after the chemicals feeder interpolation dilution, every cubic metre is added 60-100g.
(2) purify
Purification process is through three hypo acid alkali cleanings
Add in the soda acid cask washing (φ 2000 * 2000) earlier for the first time, raw material (#4000-0) discharges water after sedimentation in 16 hours for 1.2 tons, start stirring after discharging water and add sulfuric acid 80-100kg simultaneously, heat simultaneously, be warmed to 700-800 ℃, back insulation 4 hours, (be not with #8000 to be as the criterion when discharging water, begin to discharge water, discharge water and wash acid through sedimentation in 6-8 hour with coarse fodder with the dewatering outlet, open and precipitate 6-10 hour again after stirring, discharge water again, through 4-6 time, make the acid pH value of slip reach 6-7, repeated hydrogenation sodium oxide 10-20kg, and heat, open stirring, be warmed to 70-80 ℃, be incubated 2 hours, add and precipitate 6-10 hour after water stirs and discharge water again, through 4-6 time, make the slip alkaline ph value reach 8-9;
For the second time add hydrochloric acid 20-40kg and add sulfuric acid 30-40kg, heat simultaneously (following work is with for the first time identical);
Add hydrochloric acid 20-30kg for the third time, and add sulfuric acid 30-40kg, heat simultaneously (following work is with for the second time identical);
(3) classification
Slip after soda acid washed adds dispersion agent and fully stirs (adding and disperseing dosage is 1.8-3kg).After particle is fully disperseed on inspection, pump in the groove in the classification jar from stirring, introduce water with the time stage pot bottom and upwards flow (discharge 100-200L/h), after classification jar water was full, water was by the fines of last upflow tube outflow＜#8000.The fines elution time should be 24-36 hour;
Fines is told the back increases discharge (200-300L/h), begins branch #8000's.With the dark slip of suction tube sucking-off classification jar top 300-500mm, wait the classification jar after full, to aspirate again again.After #8000 had divided, increased water flow amount (300-600t/h) began branch #6000's again to aspirate repeatedly (about 3-5 time).Method by above minute #8000 is carried out classification, divided #6000, and increased water flow amount (500-800l/h) begins branch #4000 again, divides #4000's with top same working method.Reduce discharge after having divided, flow is 100-200l/h, etc. the material of #4000 emits, and is classified as end.
2. as outside the normal purification of claim 1 grading technology institute water process, softening, also increase electrodialytic water and handle, electrical conductivity of water is dropped to below the 100 μ S/cm by 350 μ S/cm.
3. be the smart filtered water glass of process as the used dispersion agent of claim 1 grading technology.
Priority Applications (1)
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|---|---|---|---|
| CNA2008100502055A CN101475172A (en) | 2008-01-03 | 2008-01-03 | Recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder |
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| CNA2008100502055A CN101475172A (en) | 2008-01-03 | 2008-01-03 | Recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804983A (en) * | 2010-04-23 | 2010-08-18 | 连云港佳宇电子材料科技有限公司 | Recovery, purification and classification method of high-purity silicon carbide micro-powder |
| CN101811088A (en) * | 2010-04-15 | 2010-08-25 | 连云港东渡碳化硅有限公司 | Method for grading inside overflow of silicon carbide super micro powder |
| CN101913605A (en) * | 2010-07-14 | 2010-12-15 | 中平能化集团易成新材料有限公司 | Method for separating silicon carbide from silicon carbide micro-powder graded byproducts |
| CN101948193A (en) * | 2010-08-31 | 2011-01-19 | 中平能化集团易成新材料有限公司 | Preparation method of water for classifying micropowder |
| CN102009977A (en) * | 2010-10-29 | 2011-04-13 | 临沭山田研磨材有限公司 | Special dispersant for hydraulic overflow classification for high-purity superfine silicon carbide micro powder for linear cutting and using method |
| CN101661297B (en) * | 2009-09-14 | 2011-05-25 | 东南大学 | Fine control method for improving classification efficiency of water overflow of silicon carbide micro powder |
| CN102311115A (en) * | 2011-08-24 | 2012-01-11 | 江阴巨能微粉科技有限公司 | Preparation method of high-purity green silicon carbide micropowder |
| CN103056019A (en) * | 2012-12-15 | 2013-04-24 | 河南富耐克超硬材料股份有限公司 | Multistage micro powder sorting method and micro powder sorting device for implementing method |
| CN105129801A (en) * | 2015-07-16 | 2015-12-09 | 河南新大新材料股份有限公司 | Recycle and reuse method of by-product from production of silicon carbide |
| CN106744964A (en) * | 2016-11-21 | 2017-05-31 | 西北矿冶研究院 | Process for recovering silicon carbide from silicon carbide waste |
| CN107159443A (en) * | 2017-06-28 | 2017-09-15 | 烟台华锐微粉有限公司 | A kind of quiet levigation method of powder |
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2008
- 2008-01-03 CN CNA2008100502055A patent/CN101475172A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101661297B (en) * | 2009-09-14 | 2011-05-25 | 东南大学 | Fine control method for improving classification efficiency of water overflow of silicon carbide micro powder |
| CN101811088A (en) * | 2010-04-15 | 2010-08-25 | 连云港东渡碳化硅有限公司 | Method for grading inside overflow of silicon carbide super micro powder |
| CN101811088B (en) * | 2010-04-15 | 2013-01-09 | 连云港市沃鑫高新材料有限公司 | Method for grading inside overflow of silicon carbide super micro powder |
| CN101804983A (en) * | 2010-04-23 | 2010-08-18 | 连云港佳宇电子材料科技有限公司 | Recovery, purification and classification method of high-purity silicon carbide micro-powder |
| CN101913605A (en) * | 2010-07-14 | 2010-12-15 | 中平能化集团易成新材料有限公司 | Method for separating silicon carbide from silicon carbide micro-powder graded byproducts |
| CN101948193B (en) * | 2010-08-31 | 2012-07-04 | 平顶山易成新材料股份有限公司 | Preparation method of water for classifying micropowder |
| CN101948193A (en) * | 2010-08-31 | 2011-01-19 | 中平能化集团易成新材料有限公司 | Preparation method of water for classifying micropowder |
| CN102009977B (en) * | 2010-10-29 | 2012-07-25 | 临沭山田研磨材有限公司 | Special dispersant for hydraulic overflow classification for high-purity superfine silicon carbide micro powder for linear cutting and using method |
| CN102009977A (en) * | 2010-10-29 | 2011-04-13 | 临沭山田研磨材有限公司 | Special dispersant for hydraulic overflow classification for high-purity superfine silicon carbide micro powder for linear cutting and using method |
| CN102311115A (en) * | 2011-08-24 | 2012-01-11 | 江阴巨能微粉科技有限公司 | Preparation method of high-purity green silicon carbide micropowder |
| CN103056019A (en) * | 2012-12-15 | 2013-04-24 | 河南富耐克超硬材料股份有限公司 | Multistage micro powder sorting method and micro powder sorting device for implementing method |
| CN103056019B (en) * | 2012-12-15 | 2015-06-17 | 富耐克超硬材料股份有限公司 | Multistage micro powder sorting method and micro powder sorting device for implementing method |
| CN105129801A (en) * | 2015-07-16 | 2015-12-09 | 河南新大新材料股份有限公司 | Recycle and reuse method of by-product from production of silicon carbide |
| CN105129801B (en) * | 2015-07-16 | 2017-05-10 | 河南易成新能源股份有限公司 | Recycle and reuse method of by-product from production of silicon carbide |
| CN106744964A (en) * | 2016-11-21 | 2017-05-31 | 西北矿冶研究院 | Process for recovering silicon carbide from silicon carbide waste |
| CN107159443A (en) * | 2017-06-28 | 2017-09-15 | 烟台华锐微粉有限公司 | A kind of quiet levigation method of powder |
| CN107159443B (en) * | 2017-06-28 | 2019-02-22 | 烟台华锐微粉有限公司 | A kind of quiet levigation method of powder |
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Open date: 20090708 |