CN107522203A - A kind of method for preparing silicon carbide micro-powder - Google Patents

A kind of method for preparing silicon carbide micro-powder Download PDF

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Publication number
CN107522203A
CN107522203A CN201610491309.4A CN201610491309A CN107522203A CN 107522203 A CN107522203 A CN 107522203A CN 201610491309 A CN201610491309 A CN 201610491309A CN 107522203 A CN107522203 A CN 107522203A
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China
Prior art keywords
powder
silicon carbide
carbide micro
washing
preparing silicon
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CN201610491309.4A
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Chinese (zh)
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徐�明
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TIANJIN MINGXIANG TECHNOLOGY DEVELOPMENT Co Ltd
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TIANJIN MINGXIANG TECHNOLOGY DEVELOPMENT Co Ltd
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Priority to CN201610491309.4A priority Critical patent/CN107522203A/en
Publication of CN107522203A publication Critical patent/CN107522203A/en
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Abstract

The present invention relates to a kind of method for preparing silicon carbide micro-powder, raw material is sent into processing system, obtains silicon carbide micro-powder except Free quartz, dealkalize washing, overflow size separation, centrifugal dehydration, expansion drying and sintering by flotation free carbon, magnetic separation, pickling iron removaling, washing, normal temperature alkali leaching elemental silicon, heating alkali successively.The method that ceramic grade of the present invention prepares silicon carbide micro-powder, preparation method is simple, easy to operate, improves the content of SIC in silicon carbide micro-powder, improves dry type air-flow crushing bag and gathers dust value-added content of product, improves the sintering quality of ceramic grade carborundum, safety and environmental protection.

Description

A kind of method for preparing silicon carbide micro-powder
Technical field
The invention belongs to silicon carbide micro-powder production technical field, and in particular to a kind of method for preparing silicon carbide micro-powder.
Background technology
Carborundum is also known as the stable chemical performance of moissanite, thermal conductivity factor height, thermal coefficient of expansion is small, anti-wear performance is good, because This its be widely used in various fields, such as silicon carbide powder is coated in turbine impeller or cylinder block with special process Wall, its wearability can be improved and increased the service life 1-2 times:To manufactured high grade refractory, resistance to thermal shock, small volume, again Amount is light and intensity is high, good energy-conserving effect:Low grade carborundum (containing SiC about 85%) is fabulous deoxidier, can accelerate to refine with it Steel speed, and be easy to control chemical composition, improve the quality of steel:In addition, carborundum can be also used for making excellent electric heating member Part Elema.Just because of carborundum has above-mentioned excellent performance, therefore, the preparation of carborundum is more and more widely ground Study carefully.Because the fineness and purity of the sintering character of silicon carbide ceramics and the quality of ceramic product and raw material are closely related, typically For, the purity and fineness of raw material are higher, and the sintering character of product is better, when density and the carborundum solid density of ceramics 3.2g/cm3The application performance of product is preferable when close.
The content of the invention
A kind of method for preparing silicon carbide micro-powder is provided it is an object of the invention to solve above-mentioned technical problem.
To achieve the above object, the present invention adopts the following technical scheme that:
A kind of method for preparing silicon carbide micro-powder, raw material be sent into processing system in, successively by flotation free carbon, magnetic separation, Pickling iron removaling, washing, normal temperature alkali leaching elemental silicon, heating alkali are except Free quartz, dealkalize washing, overflow size separation, centrifugal dehydration, sudden strain of a muscle It is evaporated dry and sintering and obtains silicon carbide micro-powder.
Flotation free carbon is that kerosene and oil flotation medicament foam remove free carbon according to 1: 1 volume ratio flotation.
Magnetic separation uses magnetic separator.
The pickling iron removaling is by the way that after intensity magnetic separator iron removaling, concentration be prepared by mixing into as 8% by sulfuric acid acid and water Acid solution;Mixing speed 30-40r/min;15-20 DEG C of extraction temperature, leach liquid-solid ratio 3: 1, extraction time 3-4.5h.
In normal temperature alkali leaching elemental silicon, elemental silicon reacts with sodium hydroxide under normal temperature state, wherein, mixing speed is 50-60r/min;Leaching condition is 30-35 DEG C of temperature, leaches liquid-solid ratio 3: 1, extraction time 2-3h, and the molar concentration of alkali is 25%.
Heat alkali to remove in Free quartz, heating-up temperature is 80-85 DEG C, and alkali molar concentration is 15%, warm-up time 2h;It is de- In neutralizing treatment, in dealkalize washing, band filter depickling washing speed control pH value after 15Hz, depickling is 7.5, dealkalize slurry For pure water, electrical conductivity < 8us/cm.
In overflow size separation, 25%, flow control is strictly controlled during overflow size separation in 50L/h for effluent concentration control Pelleting in below 8um, overflow ladle top overflow collection is put into precipitation cask deposit, toward adding in settling box in precipitation process Glacial acetic acid, it is 6.5 to adjust pH value in bucket.
It is in centrifugal dehydration, the good material stirring of precipitation concentration is uniform, it is sent into centrifuge and is dehydrated, centrifuge is being beaten The VFC VFC material of VFC after 25Hz, dehydration in 40Hz, blanking in 40Hz, dehydration is aqueous during material Amount≤10%;
In expansion drying, the material after dehydration is dried, and in drying, EAT control is at 280 DEG C, indoor temperature At 180 DEG C, leaving air temp is controlled below 100 DEG C for control.
The method that ceramic grade of the present invention prepares silicon carbide micro-powder, preparation method is simple, easy to operate, improves silicon carbide micro-powder Middle SIC content, improve dry type air-flow crushing bag and gather dust value-added content of product, improve the sintering quality of ceramic grade carborundum, peace Loopful is protected.
Embodiment
Below, the substantive distinguishing features and advantage of the present invention are further described with reference to example, but not office of the invention It is limited to listed embodiment.
A kind of method for preparing silicon carbide micro-powder, raw material be sent into processing system in, successively by flotation free carbon, magnetic separation, Pickling iron removaling, washing, normal temperature alkali leaching elemental silicon, heating alkali are except Free quartz, dealkalize washing, overflow size separation, centrifugal dehydration, sudden strain of a muscle It is evaporated dry and sintering and obtains silicon carbide micro-powder.
Flotation free carbon is that kerosene and oil flotation medicament foam remove free carbon according to 1: 1 volume ratio flotation.
Magnetic separation uses magnetic separator.
The pickling iron removaling is by the way that after intensity magnetic separator iron removaling, concentration be prepared by mixing into as 8% by sulfuric acid acid and water Acid solution;Mixing speed 30-40r/min;15-20 DEG C of extraction temperature, leach liquid-solid ratio 3: 1, extraction time 3-4.5h.
In normal temperature alkali leaching elemental silicon, elemental silicon reacts with sodium hydroxide under normal temperature state, wherein, mixing speed is 50-60r/min;Leaching condition is 30-35 DEG C of temperature, leaches liquid-solid ratio 3: 1, extraction time 2-3h, and the molar concentration of alkali is 25%.
Heat alkali to remove in Free quartz, heating-up temperature is 80-85 DEG C, and alkali molar concentration is 15%, warm-up time 2h;It is de- In neutralizing treatment, in dealkalize washing, band filter depickling washing speed control pH value after 15Hz, depickling is 7.5, dealkalize slurry For pure water, electrical conductivity < 8us/cm.
In overflow size separation, 25%, flow control is strictly controlled during overflow size separation in 50L/h for effluent concentration control Pelleting in below 8um, overflow ladle top overflow collection is put into precipitation cask deposit, toward adding in settling box in precipitation process Glacial acetic acid, it is 6.5 to adjust pH value in bucket.
It is in centrifugal dehydration, the good material stirring of precipitation concentration is uniform, it is sent into centrifuge and is dehydrated, centrifuge is being beaten The VFC VFC material of VFC after 25Hz, dehydration in 40Hz, blanking in 40Hz, dehydration is aqueous during material Amount≤10%;
In expansion drying, the material after dehydration is dried, and in drying, EAT control is at 280 DEG C, indoor temperature At 180 DEG C, leaving air temp is controlled below 100 DEG C for control.
The method that ceramic grade of the present invention prepares silicon carbide micro-powder, preparation method is simple, easy to operate, improves silicon carbide micro-powder Middle SIC content, improve dry type air-flow crushing bag and gather dust value-added content of product, improve the sintering quality of ceramic grade carborundum, peace Loopful is protected.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (8)

  1. A kind of 1. method for preparing silicon carbide micro-powder, it is characterised in that raw material is sent into processing system, is dissociated successively by flotation Carbon, magnetic separation, pickling iron removaling, washing, normal temperature alkali leaching elemental silicon, heating alkali except Free quartz, dealkalize washing, overflow size separation, from Heart dehydration, expansion drying and sintering obtain silicon carbide micro-powder.
  2. 2. the method according to claim 1 for preparing silicon carbide micro-powder, it is characterised in that flotation free carbon is kerosene and oil Floating agent foam removes free carbon according to 1: 1 volume ratio flotation.
  3. 3. the method according to claim 1 for preparing silicon carbide micro-powder, it is characterised in that magnetic separation uses magnetic separator.
  4. 4. the method according to claim 1 for preparing silicon carbide micro-powder, it is characterised in that the pickling iron removaling is by strong After magnetic separator iron removaling, sulfuric acid acid and water be prepared by mixing into concentration as 8% acid solution;Mixing speed 30-40r/min; 15-20 DEG C of extraction temperature, leach liquid-solid ratio 3: 1, extraction time 3-4.5h.
  5. 5. the method according to claim 1 for preparing silicon carbide micro-powder, it is characterised in that in normal temperature alkali leaching elemental silicon, Elemental silicon reacts with sodium hydroxide under normal temperature state, wherein, mixing speed 50-60r/min;Leaching condition is temperature 30- 35 DEG C, liquid-solid ratio 3: 1 is leached, extraction time 2-3h, the molar concentration of alkali is 25%.
  6. 6. the method according to claim 1 for preparing silicon carbide micro-powder, it is characterised in that heating alkali is removed in Free quartz, Heating-up temperature is 80-85 DEG C, and alkali molar concentration is 15%, warm-up time 2h;In dealkalize washing, in dealkalize washing, band filter Depickling washing speed control pH value after 15Hz, depickling is 7.5, and dealkalize slurry is pure water, electrical conductivity < 8us/cm.
  7. 7. the method according to claim 1 for preparing silicon carbide micro-powder, it is characterised in that in overflow size separation, effluent concentration Control is 25%, and flow control is in 50L/h, and strictly control particle overflows on below 8um, overflow ladle top during overflow size separation Stream collection is put into precipitation cask deposit, and toward glacial acetic acid is added in settling box in precipitation process, it is 6.5 to adjust pH value in bucket.
  8. 8. the method according to claim 1 for preparing silicon carbide micro-powder, it is characterised in that in centrifugal dehydration, will precipitate dense The material stirring to have contracted is uniform, is sent into centrifuge and is dehydrated, and centrifuge VFC in dnockout in 40Hz, is dehydrated time-varying Frequency control material moisture≤10% of VFC after 25Hz, dehydration in 40Hz, blanking;
    In expansion drying, the material after dehydration is dried, and in drying, at 280 DEG C, indoor temperature controls for EAT control At 180 DEG C, leaving air temp is controlled below 100 DEG C.
CN201610491309.4A 2016-06-22 2016-06-22 A kind of method for preparing silicon carbide micro-powder Pending CN107522203A (en)

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Application Number Priority Date Filing Date Title
CN201610491309.4A CN107522203A (en) 2016-06-22 2016-06-22 A kind of method for preparing silicon carbide micro-powder

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Application Number Priority Date Filing Date Title
CN201610491309.4A CN107522203A (en) 2016-06-22 2016-06-22 A kind of method for preparing silicon carbide micro-powder

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113680462A (en) * 2021-10-27 2021-11-23 苏州锦艺新材料科技有限公司 Production process of spherical silicon micropowder

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113680462A (en) * 2021-10-27 2021-11-23 苏州锦艺新材料科技有限公司 Production process of spherical silicon micropowder
CN113680462B (en) * 2021-10-27 2021-12-31 苏州锦艺新材料科技有限公司 Production process of spherical silicon micropowder

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