CN103523783B - 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
Art
The present invention relates to a kind of preparation of silicon carbide micro-powder and carbon removing device and technique, particularly a kind of synchronization is except carborundum
The device of free carbon and technique in micro mist.
Background technology
Carborundum has very high hardness, chemical stability and certain toughness, is widely used in seal, shellproof
Piece, high temperature nozzle, mill Jie, solar cell etc..With scientific and technical progress, the demand of carborundum powder is constantly adding
Greatly, purity requirement and granule size also more and more higher.Purity height, fine size, grain type is good, particle swarm is smart carborundum sub-micro ground rice are more
It is that supply falls short of demand.
Free carbon in carborundum not only can produce spot, Hua Yin to carborundum sintered article, and the trip in carborundum
Not enough from carbon activity, the sintering of silicon carbide articles does not have the effect of carbon source, on the contrary density of impact silicon carbide articles etc.
Quality requirement, so silicon carbide micro-powder needs to remove free carbon during preparation.
The main method of the free carbon employing in removing silicon carbide micro-powder is, using deionized water and silicon carbide micro-powder at present
Mixing, stirring, are classified to silicon carbide micro-powder, remove the free carbon in silicon carbide micro-powder simultaneously.As Patent Office of the People's Republic of China 2009
Disclosed on December 30, in entitled " a kind of method of removing free carbon from silicon carbide micro powder ", number of patent application：
200910065419.4, the method is using addition polymerization liquid collecting in fractionated container, will float over a small amount of the dissociating assembling liquid surface
Carbon removes, and then precipitation, discharge, are carried out except carbon by the color of discharging opening in discharging process.The method is wanted to operating personnel
Ask very high, technique is loaded down with trivial details, high labor intensive, long processing period.
Content of the invention
The purpose of the present invention is the defect overcoming prior art, provides a kind of refinement by silicon carbide micro-powder and removes free
Carbon organically combines, except carbon effect is good, process is simple synchronization remove device and the technique of free carbon in silicon carbide micropowder.
For realizing the purpose of the present invention, the technical scheme is that：A kind of synchronization removes free carbon in silicon carbide micropowder
Device, including with agitating device and the container with water leg, charging aperture and discharge gate are provided with container it is characterised in that on
The discharge gate stated in container is connected with the charging aperture of silicon carbide sand grinding machine by marker pipe, the row of being provided with marker pipe
Material pump, the charging aperture in said vesse is connected with the discharge gate of silicon carbide sand grinding machine by feeding pipe, on feeding pipe
Feed pump is installed.
The agitating device being arranged on said vesse is by the vertical axes being connected with motor and to be arranged on vertical axes upper and lower end
Two paddles composition, the upper and lower end of the water leg in container is provided with cooling water inlet tube and outlet tube, in the bottom of container peace
Equipped with discharge gate, free carbon outlet is had on the side wall of upper vessel portion.
The above-mentioned paddle being arranged on vertical axes upper end is straight-plate-type paddle, its height and position and free carbon outlet phase
Corresponding；The paddle being arranged on vertical axes lower end is pusher paddle.
A kind of synchronization removes the technique of free carbon in silicon carbide micropowder, and this technique comprises the following steps：
1）Refinement, circulation：Silicon carbide micro-powder after silicon carbide sand grinding machine is ground passes through feeding pipe and is arranged on charging
Feed pump on pipeline, squeezes into except in the container in the device of free carbon in silicon carbide micropowder by silicon carbide sand mill discharge mouth,
Add pure water in container, make the slurry that the formation solid content of the silicon carbide micro-powder in container is 25 60%, after stirring,
Add flotation oil in container, start the discharge pump on marker pipe, by the silicon carbide micro-powder in container by the row in container simultaneously
Material mouth squeezes into the charging aperture of silicon carbide sand grinding machine, is circulated；
2）Except carbon：Silicon carbide micro-powder by being arranged on the paddle of vertical axes upper end, by container slurry upper strata free
Carbon is by the free carbon outlet row's container opened on the side wall of upper vessel portion；
3）Pickling purifies：After silicon carbide micro-powder reaches requirement granularity, to the carborundum in silicon carbide sand grinding machine and container
Micro mist slurry carries out pickling purification；
4）Washing：To the slurry after the pickling purification of above-mentioned steps, the running water after being filtered using quartz sand and activated carbon
After carrying out being washed to PH=4-5, deionized water is washed to PH=6-7；
5）It is spray-dried：The slurry of above-mentioned PH=6-7 is spray-dried by spray drying tower, dried material
It is finished product submicron silicon carbide micro mist.
The addition of above-mentioned flotation oil is that the former powder of carborundum per ton adds 0.2L 2.0L.
Above-mentioned flotation oil is terpinol, kerosene, diesel oil, dithiocarbonic acids sodium, oleic acid, phenolic acid mixed fatty alcohol, organosilicon
One of glass hydrophober, isomery hexanol or at least 2 kinds compounding.
Above-mentioned sand mill is horizontal polydisc grinder, and abrasive media is 2-5mm silicon-carbide particle or carbonization silicon ball.
Inlet temperature 120-450 DEG C of above-mentioned spray drying tower, outlet temperature 80-200 DEG C.
The standard of above-mentioned deionized water is 1M Ω CM for resistivity.
Technical scheme has the characteristics that：
1st, process is simple, with short production cycle：Silicon carbide sand grinding machine is organically combined by the present invention with carbon removing device, in carborundum
So that it may automatically remove the free carbon in carborundum by carbon removing device while thinning process, can effectively shorten the production cycle
30—50%；
2nd, high treating effect：In type carborundum after present invention process, the content of free carbon is less than 0.1%；
3rd, carbon efficiencies are removed high：The present invention only needs to, during the refinement of silicon carbide micro-powder, add appropriate flotation oil,
The free carbon floating can be scraped to outside free carbon remove device by the overflow notch in free carbon remove device, except carbon efficiencies
High；
4th, with low cost：The flotation oil that the present invention adopts, often produces 1 ton of α type silicon carbide micro-powder, and cost only increases 5-20 unit
RMB, with low cost.
Brief description
Accompanying drawing 1 is present device scheme of installation；
Accompanying drawing 2 is the structural representation that the present invention synchronously removes the device of free carbon in silicon carbide micropowder.
Specific embodiment
Embodiment 1：
As shown in Figure 1, 2, the synchronous device removing free carbon in silicon carbide micropowder is by band agitating device and band water leg 13
Container composition, charging aperture and discharge gate are provided with container 4, the discharge gate 12 wherein in container pass through marker pipe 2 with
The charging aperture of silicon carbide sand grinding machine 1 is connected, and is provided with discharge pump 3 on marker pipe；Charging aperture in container passes through charging
Pipeline 5 is connected with the discharge gate of silicon carbide sand grinding machine, is provided with feed pump 6 on feeding pipe.
The agitating device being arranged on container is by the vertical axes 14 being connected with motor 7 and to be arranged on vertical axes upper and lower end
Two paddles composition, the paddle of vertical axes upper end is straight-plate-type paddle 8, its height and position and free carbon outlet 9
Corresponding；The paddle being arranged on vertical axes lower end is pusher paddle 11；The upper and lower end of the water leg in container is provided with
Cooling water inlet pipe 10 and cooling water outlet pipe 15, are provided with discharge gate 12 in the bottom of container, on the side wall of upper vessel portion
Have free carbon outlet.
Silicon carbide micro-powder in container can be lowered the temperature by water leg, be conducive to improving the refinement of silicon carbide sand grinding machine
Effect and service life.
Carborundum refines and except the production process of carbon is as follows：
1）Refinement, circulation：Former for 1 ton of α type carborundum powder is added pure water and is configured to the slurry that solid content is 60%, by prepare
Slurry pumps into except, in the container 4 in the device of free carbon in silicon carbide micropowder, stirring 4 hours, after making slurry uniform, into container
Add 200ml flotation oil.
Wherein：Flotation oil is kerosene, and in the former powder of α type carborundum, 1.04%, average grain diameter is in D50=for the content of free carbon
1.8 micron；
Start silicon carbide sand grinding machine and the discharge pump 3 being arranged on marker pipe 2, by former for the carborundum in container slurry material
Squeeze in silicon carbide sand grinding machine by silicon carbide sand mill feeding mouth, to carborundum, former powder refines, the carborundum after refinement
Former powder passes through silicon carbide sand mill discharge mouth, feeding pipe 5 and feed pump 6, squeezes in container, so circulates；
2）Except carbon：Silicon carbide micro-powder by being arranged on the paddle of vertical axes upper end, by container slurry upper strata free
Carbon is by the free carbon outlet row's container opened on the side wall of upper vessel portion；By pusher paddle, slurry in container is carried out
Stirring circulates up and down so as to be formed, and is on the one hand conducive to the floating of free carbon, is on the other hand conducive to the cooling of slurry.
3）Pickling purifies：After silicon carbide micro-powder reaches requirement granularity, by the carborundum in silicon carbide sand grinding machine and container
Micro mist slurry takes out, and carries out pickling purification；
4）Washing：To the slurry after the pickling purification of above-mentioned steps, the running water after being filtered using quartz sand and activated carbon
After carrying out being washed to pH=5, deionized water is washed to pH=7；
5）It is spray-dried：The slurry of above-mentioned pH=7 is spray-dried by spray drying tower, dried material is
For finished product submicron silicon carbide micro mist.
120 DEG C of the inlet temperature of above-mentioned spray drying tower, 80 DEG C of outlet temperature, the standard of deionized water for resistivity is
1.2M Ω cm about.
Sand mill is horizontal polydisc grinder, and abrasive media is 2-5mm silicon-carbide particle.
After measured in final products free carbon content 0.09%, α type carborundum average grain diameter D50=0.55 micron.
Embodiment 2：
On the basis of embodiment 1, change some technological parameters, specific embodiment is as follows：
1）Refinement, circulation：Former for 1 ton of α type carborundum powder is added pure water and is configured to the slurry that solid content is 25%, by prepare
Slurry pumps into except, in the container 4 in the device of free carbon in silicon carbide micropowder, stirring 2 hours, after making slurry uniform, into container
Add 1800ml flotation oil.
Wherein：Flotation oil is terpinol, and in the former powder of α type carborundum, 0.86%, average grain diameter is 2.9 for the content of free carbon
Micron；
2）Except carbon：Silicon carbide micro-powder by being arranged on the paddle of vertical axes upper end, by container slurry upper strata free
Carbon is by the free carbon outlet row's container opened on the side wall of upper vessel portion；By pusher paddle, slurry in container is carried out
Stirring circulates up and down so as to be formed, and is on the one hand conducive to the floating of free carbon, is on the other hand conducive to the cooling of slurry.
3）Pickling purifies：After silicon carbide micro-powder reaches requirement granularity, by the carborundum in silicon carbide sand grinding machine and container
Micro mist slurry takes out, and carries out pickling purification；
4）Washing：To the slurry after the pickling purification of above-mentioned steps, the running water after being filtered using quartz sand and activated carbon
After carrying out being washed to pH=4, deionized water is washed to pH=6；
5）It is spray-dried：The slurry of above-mentioned pH=6 is spray-dried by spray drying tower, dried material is
For finished product submicron silicon carbide micro mist.
450 DEG C of the inlet temperature of above-mentioned spray drying tower, 200 DEG C of outlet temperature, the standard of deionized water for resistivity is
1.5M Ω cm about.Sand mill is horizontal polydisc grinder, and abrasive media is 2-5mm silicon-carbide particle；
After measured in final products free carbon content 0.01%, α type carborundum average grain diameter D50=0.67 micron.
Embodiment 3：
On the basis of embodiment 1, change some technological parameters, specific embodiment is as follows：
1）Refinement, circulation：Former for 1 ton of α type carborundum powder is added pure water and is configured to the slurry that solid content is 48%, by prepare
Slurry pumps into except, in the container 4 in the device of free carbon in silicon carbide micropowder, stirring 3 hours, after making slurry uniform, into container
Add 800ml flotation oil.
Wherein：Flotation oil is dithiocarbonic acids sodium, in the former powder of α type carborundum the content of free carbon 0.64%, average grain diameter
At 3.2 microns；
2）Except carbon：Silicon carbide micro-powder by being arranged on the paddle of vertical axes upper end, by container slurry upper strata free
Carbon is by the free carbon outlet row's container opened on the side wall of upper vessel portion；By pusher paddle, slurry in container is carried out
Stirring circulates up and down so as to be formed, and is on the one hand conducive to the floating of free carbon, is on the other hand conducive to the cooling of slurry.
3）Pickling purifies：After silicon carbide micro-powder reaches requirement granularity, by the carborundum in silicon carbide sand grinding machine and container
Micro mist slurry takes out, and carries out pickling purification；
4）Washing：To the slurry after the pickling purification of above-mentioned steps, the running water after being filtered using quartz sand and activated carbon
After carrying out being washed to pH=4, deionized water is washed to pH=7；
5）It is spray-dried：The slurry of above-mentioned pH=7 is spray-dried by spray drying tower, dried material is
For finished product submicron silicon carbide micro mist.
300 DEG C of the inlet temperature of above-mentioned spray drying tower, 100 DEG C of outlet temperature, the standard of deionized water for resistivity is
1.3M Ω cm about.Sand mill is horizontal polydisc grinder, and abrasive media is 2-5mm carborundum spheric granules；
After measured in final products free carbon content 0.03%, α type carborundum average grain diameter D50=0.69 micron.
Embodiment 4-10：
On the basis of any of the above-described embodiment, change composition and the consumption of flotation oil, in final products, free carbon contains
Amount and the average grain diameter such as following table of α type carborundum.
| Embodiment | Flotation oil | The content of free carbon | Average grain diameter |
| 4 | Diesel oil 900ml | 0.01% | D50=0.56 micron |
| 5 | Oleic acid 1200ml | 0.03% | D50=0.59 micron |
| 6 | Phenolic acid mixed fatty alcohol 880ml | 0.04% | D50=0.69 micron |
| 7 | Silicone glass hydrophober 2000ml | 0.08% | D50=0.62 micron |
| 8 | Isomery hexanol 600ml | 0.05% | D50=0.57 micron |
| 9 | The each 500ml of terpinol, kerosene | 0.06% | D50=0.61 micron |
| 10 | Diesel oil, oleic acid, each 300ml of phenolic acid mixed fatty alcohol | 0.07% | D50=0.65 micron |
Flotation oil in the above-described embodiments is commercial technical grade product.
Claims (9)
1. a kind of synchronization removes the device of free carbon in silicon carbide micropowder, including with agitating device and the container with water leg, is holding
Charging aperture and discharge gate are provided with device it is characterised in that said vesse（4）In discharge gate（12）By marker pipe（2）With
Silicon carbide sand grinding machine（1）Charging aperture be connected, discharge pump is provided with marker pipe（3）, charging aperture in said vesse
By feeding pipe（5）It is connected with the discharge gate of silicon carbide sand grinding machine, feed pump is provided with feeding pipe（6）, holding
Free carbon outlet is had on the side wall on device top（9）.
2. synchronization according to claim 1 removes the device of free carbon in silicon carbide micropowder it is characterised in that being arranged on above-mentioned
Container（4）On agitating device be by with motor（7）Connected vertical axes（14）Stir be arranged on vertical axes upper and lower end two
Mix oar composition, the water leg in container（13）Upper and lower end cooling water inlet tube and outlet tube is installed, be provided with the bottom of container
Discharge gate（12）.
3. synchronization according to claim 2 removes the device of free carbon in silicon carbide micropowder it is characterised in that above-mentioned be arranged on
Vertical axes（14）The paddle of upper end is straight-plate-type paddle, its height and position and free carbon outlet（9）Corresponding；It is arranged on
The paddle of vertical axes lower end is pusher paddle（11）.
4. a kind of synchronization removes the technique of free carbon in silicon carbide micropowder, and this technique comprises the following steps：
1）Refinement, circulation：Silicon carbide micro-powder after silicon carbide sand grinding machine is ground passes through feeding pipe（5）Be arranged on feed pipe
Feed pump on road（6）, squeezed into except the container in the device of free carbon in silicon carbide micropowder by silicon carbide sand mill discharge mouth（4）
Interior, add pure water in container, make the slurry that the formation solid content of the silicon carbide micro-powder in container is 25 60%, after stirring,
Add flotation oil in container, start marker pipe simultaneously（2）On discharge pump（3）, by the silicon carbide micro-powder in container by holding
Discharge gate in device（12）Squeeze into the charging aperture of silicon carbide sand grinding machine, be circulated；
2）Except carbon：Silicon carbide micro-powder is by being arranged on vertical axes（14）The paddle of upper end, by container slurry upper strata free
Carbon is by the free carbon outlet opened on the side wall of upper vessel portion（9）In amount discharge container；
3）Pickling purifies：After silicon carbide micro-powder reaches requirement granularity, to the silicon carbide micro-powder in silicon carbide sand grinding machine and container
Slurry carries out pickling purification；
4）Washing：To the slurry after the pickling purification of above-mentioned steps, the running water after being filtered using quartz sand and activated carbon is carried out
After being washed to pH=4-5, deionized water is washed to pH=6-7；
5）It is spray-dried：The slurry of above-mentioned pH=6-7 is spray-dried by spray drying tower, dried material is
Finished product submicron silicon carbide micro mist.
5. synchronization according to claim 4 removes the technique of free carbon in silicon carbide micropowder it is characterised in that above-mentioned flotation oil
Addition be the former powder of carborundum per ton add 0.2L 2.0L.
6. synchronization according to claim 5 removes the technique of free carbon in silicon carbide micropowder it is characterised in that above-mentioned flotation oil
For terpinol, kerosene, diesel oil, dithiocarbonic acids sodium, oleic acid, phenolic acid mixed fatty alcohol, silicone glass hydrophober, isomery hexanol
One of or at least 2 kinds compounding.
7. synchronization according to claim 6 removes the technique of free carbon in silicon carbide micropowder it is characterised in that above-mentioned sand mill
For horizontal polydisc grinder, abrasive media is 2-5mm silicon-carbide particle.
8. synchronization according to claim 7 removes the technique of free carbon in silicon carbide micropowder it is characterised in that above-mentioned spraying is done
Inlet temperature 120-450 DEG C of dry tower, outlet temperature 80-200 DEG C.
9. synchronization according to claim 8 removes the technique of free carbon in silicon carbide micropowder it is characterised in that above-mentioned deionization
The standard of water is 1M Ω cm for resistivity.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105127009B (en) * | 2015-08-26 | 2018-04-06 | 连云港龙塔研磨材料有限公司 | The flotation unit and method of free carbon in a kind of removal carborundum powder |
| 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 |
| CN105948055B (en) * | 2016-05-30 | 2017-12-22 | 山田研磨材料有限公司 | The method of purification of semiconductor high-purity silicon carbide micro-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 |
| 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 |
| 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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| US4293099A (en) * | 1979-07-02 | 1981-10-06 | Silag, Inc. | Recovery of silicon carbide whiskers from coked, converted rice hulls by froth flotation |
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