CN103523783A - Device and process for synchronously removing free carbon in silicon carbide micro powder - Google Patents
Device and process for synchronously removing free carbon in silicon carbide micro powder Download PDFInfo
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Abstract
The invention relates to preparation and a carbon removing device and process of silicon carbide micro powder, and in particular relates to a device and process for synchronously removing free carbon in silicon carbide micro powder. The device comprises a container with a stirring device and a water jacket, wherein a feeding hole and a discharging hole are formed in the container. The device is characterized in that the discharging hole in the container is communicated with a feeding hole of a silicon carbide sand mill through a discharge pipeline; a discharge pump is arranged on the discharge pipeline; the feeding hole in the container is communicated with a discharging hole of the silicon carbide sand mill through a feed pipeline; a feed pump is arranged on the feed pipeline. The process comprises the steps of refining, circulating, carbon removing, acid washing for purification, water washing and spray drying. The technical scheme provided by the invention has the characteristics of simple process, short production cycle, good treatment effect, high carbon removing effect, low cost and the like.
Description
Affiliated technical field
The present invention relates to a kind of preparation and carbon removing device and technique of silicon carbide micro-powder, particularly a kind of synchronous device and technique except free carbon in silicon carbide micropowder.
Background technology
Silicon carbide has very high hardness, chemical stability and certain toughness, is widely used in sealing member, ballistic resistant sheet, high temperature nozzle, mill Jie, solar cell etc.Along with scientific and technical progress, the demand of carborundum powder is in continuous increasing, and purity requirement and globule size are also more and more higher.Purity is high, fine size, grain type are good, supply falls short of demand especially for the silicon carbide sub-micro ground rice of grain group essence.
Uncombined carbon in silicon carbide not only can produce spot to silicon carbide sintered article, flower prints, and the uncombined carbon in silicon carbide is active not enough, in the sintering of silicon carbide articles, do not have the effect of carbon source, affect on the contrary the specification of quality such as density of silicon carbide articles, so silicon carbide micro-powder needs to remove uncombined carbon in the process of preparation.
Removing at present the main method that uncombined carbon in silicon carbide micro-powder adopts is, utilizes deionized water and silicon carbide micro-powder to mix, stir, and silicon carbide micro-powder is carried out to classification, removes the uncombined carbon in silicon carbide micro-powder simultaneously.As Patent Office of the People's Republic of China's on December 30th, 2009 disclosed " a kind of method of removing free carbon from silicon carbide micro powder " by name, number of patent application: 200910065419.4, the method is to utilize addition polymerization liquid collecting in fractionated container, the a small amount of uncombined carbon that floats over gathering liquid surface is removed, then precipitation, discharge, carry out de-carbon by the color of discharge port in discharge process.The method is to operator's requirement is very high, technique is loaded down with trivial details, labour intensity is large, long processing period.
Summary of the invention
The object of the invention is to overcome the defect of prior art, provide a kind of by the refinement of silicon carbide micro-powder with remove uncombined carbon and organically combine, de-carbon is effective, technique simple synchronous device and technique except free carbon in silicon carbide micropowder.
For realizing object of the present invention, technical scheme of the present invention is: a kind of synchronous device except free carbon in silicon carbide micropowder, comprise with whipping appts with the container of water jacket, opening for feed and discharge gate are installed on container, it is characterized in that the discharge gate in said vesse is connected with the opening for feed of silicon carbide sand grinding machine by marker pipe, discharge pump is installed on marker pipe, opening for feed in said vesse is connected with the discharge gate of silicon carbide sand grinding machine by feeding pipe, and fresh feed pump is installed on feeding pipe.
The whipping appts being arranged on said vesse is comprised of the vertical axes being connected with motor and two stirring rakes that are arranged on vertical axes upper and lower end, the upper and lower end of the water jacket in container is provided with water coolant inlet tube and outlet tube, bottom at container is provided with discharge gate, has uncombined carbon relief outlet on the sidewall on container top.
The above-mentioned stirring rake that is arranged on vertical axes upper end is straight-plate-type stirring rake, and its height location is corresponding with uncombined carbon relief outlet; The stirring rake that is arranged on vertical axes lower end is pusher stirring rake.
A synchronous technique except free carbon in silicon carbide micropowder, this technique comprises the following steps:
1) refinement, circulation: the silicon carbide micro-powder after silicon carbide sand grinding machine is ground is by feeding pipe and be arranged on the fresh feed pump on feeding pipe, by silicon carbide sand mill discharge mouth, squeezed into except in the container in the device of free carbon in silicon carbide micropowder, in container, add pure water, make the silicon carbide micro-powder in container form the slurry that solid content is 25-60%, after stirring, in container, add flotation oil, start the discharge pump on marker pipe simultaneously, discharge gate by the silicon carbide micro-powder in container in container is squeezed into the opening for feed of silicon carbide sand grinding machine, circulates;
2) de-carbon: silicon carbide micro-powder is by being arranged on the stirring rake of vertical axes upper end, in the uncombined carbon relief outlet row container of opening on the sidewall by the uncombined carbon on slurry upper strata in container by container top;
3) pickling is purified: when silicon carbide micro-powder reaches after requirement granularity, the silicon carbide powder slurry material in silicon carbide sand grinding machine and container is carried out to pickling purification;
4) washing: the slurry after the pickling of above-mentioned steps is purified, utilize the tap water after quartz sand and activated carbon filtration to be washed to after PH=4-5, with deionized water, be washed to PH=6-7;
5) spraying is dry: the slurry of above-mentioned PH=6-7 is sprayed by spray-drying tower dry, dried material is finished product submicron silicon carbide micro mist.
The add-on of above-mentioned flotation oil is that the former powder of silicon carbide per ton adds 0.2L-2.0L.
Above-mentioned flotation oil is the composite of a kind of in Terpineol 350, kerosene, diesel oil, dithiocarbonic acid sodium, oleic acid, phenolic acid mixed fatty alcohol, silicone glass hydrophober, isomery hexanol or at least 2 kinds.
Above-mentioned sand mill is horizontal polydisc shredder, and grinding medium is 2-5mm silicon-carbide particle or silicon carbide ball.
The inlet temperature 120-450 ℃ of above-mentioned spray-drying tower, temperature out 80-200 ℃.
The standard of above-mentioned deionized water is resistivity Wei≤1M Ω CM.
Technical scheme of the present invention has following characteristics:
1, technique is simple, with short production cycle: the present invention organically combines silicon carbide sand grinding machine and carbon removing device, in silicon carbide thinning process, just the uncombined carbon in silicon carbide can be removed automatically by carbon removing device, can effectively shorten the production cycle 30-50%;
2, treatment effect is good: the content of the type silicon carbide Free Carbon after the present invention processes is less than 0.1%;
3, except carbon efficiencies is high: the present invention only need to add appropriate flotation oil in the process of the refinement of silicon carbide micro-powder, and the uncombined carbon of floating can be scraped to uncombined carbon clearing device by the overflow notch on uncombined carbon clearing device, except carbon efficiencies high;
4, with low cost: the flotation oil that the present invention adopts, 1 ton of α type silicon carbide micro-powder of every production, cost only increases 5-20 yuan, with low cost.
Accompanying drawing explanation
Accompanying drawing 1 is present device scheme of installation;
Accompanying drawing 2 is that the present invention synchronously removes the structural representation of the device of free carbon in silicon carbide micropowder.
Embodiment
Embodiment 1:
As shown in Figure 1, 2, the synchronous device except free carbon in silicon carbide micropowder is by forming with whipping appts and the container with water jacket 13, opening for feed and discharge gate are installed on container 4, wherein the discharge gate in container 12 is connected with the opening for feed of silicon carbide sand grinding machine 1 by marker pipe 2, and discharge pump 3 is installed on marker pipe; Opening for feed in container is connected with the discharge gate of silicon carbide sand grinding machine by feeding pipe 5, and fresh feed pump 6 is installed on feeding pipe.
The whipping appts being arranged on container is comprised of the vertical axes 14 being connected with motor 8 and two stirring rakes that are arranged on vertical axes upper and lower end, and the stirring rake of vertical axes upper end is straight-plate-type stirring rake 8, and its height location is corresponding with uncombined carbon relief outlet 9; The stirring rake that is arranged on vertical axes lower end is pusher stirring rake 11; The upper and lower end of the water jacket in container is provided with cooling water inlet pipe 10 and cooling water outlet pipe 15, in the bottom of container, discharge gate 12 is installed, and has uncombined carbon relief outlet on the sidewall on container top.
By water jacket, can lower the temperature to the silicon carbide micro-powder in container, be conducive to improve thinning effect and the work-ing life of silicon carbide sand grinding machine.
The production process of silicon carbide refinement and de-carbon is as follows:
1) refinement, circulation: 1 ton of former powder of α type silicon carbide is added to pure water, and to be mixed with solid content be 60% slurry, the slurry preparing is pumped in the container 4 in the device of de-carbon SiClx micro mist Free Carbon, stir 4 hours, after making slurry evenly, in container, add 200ml flotation oil.
Wherein: flotation oil is kerosene, the content of the former powder Free Carbon of α type silicon carbide is 1.04%, and median size is at D50=1.8 micron;
Start silicon carbide sand grinding machine and be arranged on the discharge pump 3 on marker pipe 2, the former powder slurry of silicon carbide in container is squeezed in silicon carbide sand grinding machine by silicon carbide sand mill feeding mouth, the former powder of silicon carbide is carried out to refinement, the former powder of silicon carbide after refinement is by silicon carbide sand mill discharge mouth, feeding pipe 5 and fresh feed pump 6, squeeze in container, so circulation;
2) de-carbon: silicon carbide micro-powder is by being arranged on the stirring rake of vertical axes upper end, in the uncombined carbon relief outlet row container of opening on the sidewall by the uncombined carbon on slurry upper strata in container by container top; By pusher stirring rake, slurry in container is stirred, make it form circulation up and down, be conducive on the one hand the floating of uncombined carbon, be conducive on the other hand the cooling of slurry.
3) pickling is purified: when silicon carbide micro-powder reaches after requirement granularity, the silicon carbide powder slurry material in silicon carbide sand grinding machine and container is taken out, carry out pickling purification;
4) washing: the slurry after the pickling of above-mentioned steps is purified, utilize the tap water after quartz sand and activated carbon filtration to be washed to after PH=5, with deionized water, be washed to PH=7;
5) spraying is dry: the slurry of above-mentioned PH=7 is sprayed by spray-drying tower dry, dried material is finished product submicron silicon carbide micro mist.
120 ℃ of the inlet temperatures of above-mentioned spray-drying tower, 80 ℃ of temperature outs, the standard of deionized water is that resistivity is 1.2M Ω CM left and right.
Sand mill is horizontal polydisc shredder, and grinding medium is 2-5mm silicon-carbide particle
The content of the finished product Free Carbon is at the median size D of 0.09%, α type silicon carbide after measured
50=0.55 micron.
Embodiment 2:
On the basis of embodiment 1, change some processing parameter, specific embodiment is as follows:
1) refinement, circulation: 1 ton of former powder of α type silicon carbide is added to pure water, and to be mixed with solid content be 25% slurry, the slurry preparing is pumped in the container 4 in the device of de-carbon SiClx micro mist Free Carbon, stir 2 hours, after making slurry evenly, in container, add 1800ml flotation oil.
Wherein: flotation oil is Terpineol 350, the content of the former powder Free Carbon of α type silicon carbide is 0.86%, and median size is at 2.9 microns;
2) de-carbon: silicon carbide micro-powder is by being arranged on the stirring rake of vertical axes upper end, in the uncombined carbon relief outlet row container of opening on the sidewall by the uncombined carbon on slurry upper strata in container by container top; By pusher stirring rake, slurry in container is stirred, make it form circulation up and down, be conducive on the one hand the floating of uncombined carbon, be conducive on the other hand the cooling of slurry.
3) pickling is purified: when silicon carbide micro-powder reaches after requirement granularity, the silicon carbide powder slurry material in silicon carbide sand grinding machine and container is taken out, carry out pickling purification;
4) washing: the slurry after the pickling of above-mentioned steps is purified, utilize the tap water after quartz sand and activated carbon filtration to be washed to after PH=4, with deionized water, be washed to PH=6;
5) spraying is dry: the slurry of above-mentioned PH=6 is sprayed by spray-drying tower dry, dried material is finished product submicron silicon carbide micro mist.
450 ℃ of the inlet temperatures of above-mentioned spray-drying tower, 200 ℃ of temperature outs, the standard of deionized water is that resistivity is 1.5M Ω CM left and right.Sand mill is horizontal polydisc shredder, and grinding medium is 2-5mm silicon-carbide particle;
The content of the finished product Free Carbon is at the median size D of 0.01%, α type silicon carbide after measured
50=0.67 micron.
Embodiment 3:
On the basis of embodiment 1, change some processing parameter, specific embodiment is as follows:
1) refinement, circulation: 1 ton of former powder of α type silicon carbide is added to pure water, and to be mixed with solid content be 48% slurry, the slurry preparing is pumped in the container 4 in the device of de-carbon SiClx micro mist Free Carbon, stir 3 hours, after making slurry evenly, in container, add 800ml flotation oil.
Wherein: flotation oil is dithiocarbonic acid sodium, the content of the former powder Free Carbon of α type silicon carbide is 0.64%, and median size is at 3.2 microns;
2) de-carbon: silicon carbide micro-powder is by being arranged on the stirring rake of vertical axes upper end, in the uncombined carbon relief outlet row container of opening on the sidewall by the uncombined carbon on slurry upper strata in container by container top; By pusher stirring rake, slurry in container is stirred, make it form circulation up and down, be conducive on the one hand the floating of uncombined carbon, be conducive on the other hand the cooling of slurry.
3) pickling is purified: when silicon carbide micro-powder reaches after requirement granularity, the silicon carbide powder slurry material in silicon carbide sand grinding machine and container is taken out, carry out pickling purification;
4) washing: the slurry after the pickling of above-mentioned steps is purified, utilize the tap water after quartz sand and activated carbon filtration to be washed to after PH=4, with deionized water, be washed to PH=7;
5) spraying is dry: the slurry of above-mentioned PH=7 is sprayed by spray-drying tower dry, dried material is finished product submicron silicon carbide micro mist.
300 ℃ of the inlet temperatures of above-mentioned spray-drying tower, 100 ℃ of temperature outs, the standard of deionized water is that resistivity is 1.3M Ω CM left and right.Sand mill is horizontal polydisc shredder, and grinding medium is 2-5mm silicon carbide spheroidal particle;
The content of the finished product Free Carbon is at the median size D of 0.03%, α type silicon carbide after measured
50=0.69 micron.
Embodiment 4-10.
On the basis of above-mentioned arbitrary embodiment, change composition and the consumption of flotation oil, the median size of the content of the finished product Free Carbon and α type silicon carbide is as following table.
| Embodiment | Flotation oil | The content of uncombined | Median size | |
| 4 | Diesel oil 900ml | 0.01% | D 50=0.56 micron | |
| 5 | Oleic acid 1200ml | 0.03% | D 50=0.59 micron | |
| 6 | Phenolic acid mixed fatty alcohol 880ml | 0.04% | D 50=0.69 micron | |
| 7 | Silicone glass hydrophober 2000ml | 0.08% | D 50=0.62 micron | |
| 8 | Isomery hexanol 600ml | 0.05% | D 50=0.57 micron | |
| 9 | Terpineol 350, each 500ml of kerosene | 0.06% | D
50=0.61 |
|
| 10 | Diesel oil, oleic acid, each 300ml of phenolic acid mixed fatty alcohol | 0.07% | D 50=0.65 micron |
Flotation oil is in the above-described embodiments commercial technical grade product.
Claims (9)
1. a synchronous device except free carbon in silicon carbide micropowder, comprise with whipping appts with the container of water jacket, opening for feed and discharge gate are installed on container, it is characterized in that the discharge gate (12) in said vesse (4) is connected with the opening for feed of silicon carbide sand grinding machine (1) by marker pipe (2), discharge pump (3) is installed on marker pipe, opening for feed in said vesse is connected with the discharge gate of silicon carbide sand grinding machine by feeding pipe (5), and fresh feed pump (6) is installed on feeding pipe.
2. the synchronous device except free carbon in silicon carbide micropowder according to claim 1, it is characterized in that being arranged on whipping appts on said vesse (4) is comprised of the vertical axes (14) being connected with motor (8) and two stirring rakes being arranged on vertical axes upper and lower end, the upper and lower end of the water jacket in container (13) is provided with water coolant inlet tube and outlet tube, discharge gate (12) is installed in the bottom of container, on the sidewall on container top, has uncombined carbon relief outlet (9).
3. the synchronous device except free carbon in silicon carbide micropowder according to claim 2, is characterized in that the above-mentioned stirring rake that is arranged on vertical axes (14) upper end is straight-plate-type stirring rake, and its height location is corresponding with uncombined carbon relief outlet (9); The stirring rake that is arranged on vertical axes lower end is pusher stirring rake (11).
4. synchronously except a technique for free carbon in silicon carbide micropowder, this technique comprises the following steps:
1) refinement, circulation: the silicon carbide micro-powder after silicon carbide sand grinding machine is ground is by feeding pipe (5) and be arranged on the fresh feed pump (6) on feeding pipe, by silicon carbide sand mill discharge mouth, squeezed into except in the container in the device of free carbon in silicon carbide micropowder (4), in container, add pure water, make the silicon carbide micro-powder in container form the slurry that solid content is 25-60%, after stirring, in container, add flotation oil, start the discharge pump (3) on marker pipe (2) simultaneously, discharge gate by the silicon carbide micro-powder in container in container (12) is squeezed into the opening for feed of silicon carbide sand grinding machine, circulate,
2) de-carbon: silicon carbide micro-powder is by being arranged on the stirring rake of vertical axes (14) upper end, in uncombined carbon relief outlet (9) the row container of opening on the sidewall by the uncombined carbon on slurry upper strata in container by container top;
3) pickling is purified: when silicon carbide micro-powder reaches after requirement granularity, the silicon carbide powder slurry material in silicon carbide sand grinding machine and container is carried out to pickling purification;
4) washing: the slurry after the pickling of above-mentioned steps is purified, utilize the tap water after quartz sand and activated carbon filtration to be washed to after PH=4-5, with deionized water, be washed to PH=6-7;
5) spraying is dry: the slurry of above-mentioned PH=6-7 is sprayed by spray-drying tower dry, dried material is finished product submicron silicon carbide micro mist.
5. according to claim 4 synchronously except the technique of free carbon in silicon carbide micropowder, the add-on that it is characterized in that above-mentioned flotation oil is that the former powder of silicon carbide per ton adds 0.2L-2.0L.
6. the synchronous technique except free carbon in silicon carbide micropowder according to claim 5, is characterized in that above-mentioned flotation oil is the composite of a kind of in Terpineol 350, kerosene, diesel oil, dithiocarbonic acid sodium, oleic acid, phenolic acid mixed fatty alcohol, silicone glass hydrophober, isomery hexanol or at least 2 kinds.
7. the synchronous technique except free carbon in silicon carbide micropowder according to claim 6, is characterized in that above-mentioned sand mill is horizontal polydisc shredder, and grinding medium is 2-5mm silicon-carbide particle or silicon carbide ball.
8. according to claim 7 synchronously except the technique of free carbon in silicon carbide micropowder, it is characterized in that the inlet temperature 120-450 ℃ of above-mentioned spray-drying tower, temperature out 80-200 ℃.
9. according to claim 8 synchronously except the technique of free carbon in silicon carbide micropowder, the standard that it is characterized in that above-mentioned deionized water is that resistivity is≤1M Ω CM.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105062152A (en) * | 2015-09-08 | 2015-11-18 | 南通市金菱电器有限公司 | Grinding-modification integrated production device and technique, and application thereof |
| CN105127009A (en) * | 2015-08-26 | 2015-12-09 | 连云港龙塔研磨材料有限公司 | Flotation device and method for removing free carbon in silicon carbide powder |
| CN105948055A (en) * | 2016-05-30 | 2016-09-21 | 山田研磨材料有限公司 | Purification method of high-purity silicon carbide micro powder for semiconductor |
| 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 |
| CN107226471A (en) * | 2017-07-25 | 2017-10-03 | 安徽正丰再生资源有限公司 | A kind of silicon carbide micro-powder purifying plant |
| CN108752003A (en) * | 2018-08-17 | 2018-11-06 | 宁夏和兴碳基材料有限公司 | The preparation method of silicon carbide fine ceramics silicon carbide micro-powder |
| CN111086989A (en) * | 2019-08-15 | 2020-05-01 | 上海衡益特陶新材料有限公司 | Manufacturing system of high-purity boron carbide powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105127009A (en) * | 2015-08-26 | 2015-12-09 | 连云港龙塔研磨材料有限公司 | Flotation device and method for removing free carbon in silicon carbide powder |
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| CN107226471A (en) * | 2017-07-25 | 2017-10-03 | 安徽正丰再生资源有限公司 | A kind of silicon carbide micro-powder purifying plant |
| CN108752003A (en) * | 2018-08-17 | 2018-11-06 | 宁夏和兴碳基材料有限公司 | The preparation method of silicon carbide fine ceramics silicon carbide micro-powder |
| CN108752003B (en) * | 2018-08-17 | 2021-06-22 | 宁夏和兴碳基材料有限公司 | Preparation method of silicon carbide micro powder for silicon carbide fine ceramic |
| CN111086989A (en) * | 2019-08-15 | 2020-05-01 | 上海衡益特陶新材料有限公司 | Manufacturing system of high-purity boron carbide powder |
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