CN106365168A - Method for purifying carbon materials in silicon carbide - Google Patents

Method for purifying carbon materials in silicon carbide Download PDF

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Publication number
CN106365168A
CN106365168A CN201610771808.9A CN201610771808A CN106365168A CN 106365168 A CN106365168 A CN 106365168A CN 201610771808 A CN201610771808 A CN 201610771808A CN 106365168 A CN106365168 A CN 106365168A
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CN
China
Prior art keywords
carbon
slip
flotation column
silicon carbide
carbon material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610771808.9A
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Chinese (zh)
Inventor
方珂
刘创
楚红斌
吕春长
夏军
杨正宏
吕本会
梁西正
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PINGDINGSHAN YICHENG NEW MATERIAL CO Ltd
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PINGDINGSHAN YICHENG NEW MATERIAL CO Ltd
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Priority to CN201610771808.9A priority Critical patent/CN106365168A/en
Publication of CN106365168A publication Critical patent/CN106365168A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/14Flotation machines
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/004Organic compounds
    • B03D1/016Macromolecular compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/02Collectors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/04Frothers
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

A method for purifying carbon materials in silicon carbide comprises the following steps: (1) weighing silicon carbide slurry, placing in a flotation column, adding a liquid detergent, polyethylene glycol and compound higher alcohols, mixing evenly, passing air from a nozzle at the bottom of the flotation column, allowing the mixture to mix fully with the air in the flotation column for use; (2) producing the high carbon material slurry through pressure controlling; (3) separating and purifying the high carbon material slurry to obtain the product. According to the method for purifying the carbon materials in silicon carbide, the carbon materials are purified by a physical way. Based on the principle that carbon materials have particle sizes different from the particle sizes of silicon carbide, through a combination of negative pressure and double-layer filter cloth, the carbon materials and silicon carbide are further separated, and the purity of the carbon materials is thus improved.

Description

The method of purification of carbon material in a kind of carborundum
Technical field
The present invention relates to a kind of method of purification of carbon material, specially carborundum produce in carbon impurity material method of purification.
Background technology
Carbon material is to be mixed in one of silicon carbide products impurity during silicon carbide micro-powder produces, and is clean with washing under normal circumstances The foaming agent such as essence are removed, and as byproduct for treatment.Under current process conditions, in carbon material, carbon content (wt, divide by quality Number) it is only capable of reaching 60%-80%, wherein contain a certain amount of silicon carbide micro-powder, the price of carborundum will be far longer than carbon Price, therefore enterprise all are trying every possible means to separate the mixed carborundum being clipped in carbon material as far as possible, thus reaching recovery carborundum Micropowder simultaneously improves the dual purpose of carbon content.
Content of the invention
It is an object of the invention to solving above-mentioned problem, provide a kind of method of purification of carbon material in carborundum.
The technical solution adopted in the present invention is: the method for purification of carbon material in a kind of carborundum, comprises the following steps:
Step one, weigh mass concentration be 20%-40% silicon carbide slurry, the silicon carbide slurry weighing is put in flotation column, And it is added thereto to liquid detergent, Polyethylene Glycol and compound advanced alcohol, after being sufficiently mixed, it is passed through sky from the nozzle of the bottom of flotation column Gas, makes mixed slurry standby after being sufficiently mixed with air in flotation column;
Step 2, control pressure make the mixed slurry liquid level in step one form certain difference in height, mixed slurry with excessive groove The bubble being mixed to form with air forms carbon alveolar layer with enrichment under liquid detergent, Polyethylene Glycol and compound advanced alcohol collective effect, Flotation column is centrally formed a kind of thrust, makes to overflow flotation column formation high-carbon slip outside carbon alveolar layer, standby;
Step 3, the high-carbon being formed in step 2 slip is introduced cylindrical de- material cylinder by pipeline, start cylindrical de- material cylinder The negative pressure device of bottom, high-carbon slip is 3-8um filter cloth by two-layer aperture to carry out separating, and the low slip of carbon amounts passes through filter cloth Come together in cylindrical de- material cylinder, high-carbon slip is blocked on filter cloth, make formation carbon content outside filter cloth be maintained at more than 98% High purity carbon material, standby;
Step 4, the carbon material isolating upper strata filter cloth take out, and form product after dehydration.
Nozzle described in step one is Laval nozzle.
Difference in height in described step 2 is 2-4cm.
Negative pressure device pressure limit described in step 3 is 0.075-0.105mpa.
In described step one, the compound advanced alcohol of employing is r- alkyl compound advanced alcohol, liquid detergent in slip per ton, poly- Ethylene glycol, the addition of compound advanced alcohol are respectively 20 ml, 50-80ml and 20-40ml.
Beneficial effects of the present invention:
1st, in the present invention, liquid detergent mainly plays barbotage, the work of r- alkyl as surfactant during except carbon With for foaming agent and collecting agent, these three reagent are used in mixed way can be separated impurity such as carbon material from slip effectively, This is the precondition that subsequent step is purified to carbon material.
2nd, on decarbonizing technology, the critical process point of the present invention is that air-flow is introduced by the Laval nozzle from flotation column bottom Flotation column, compared to general nozzle, because the special converging diverging structure of Laval nozzle, the gas of extraction in its cavity Carborundum in slip, due to having strong impulsive force, can be sufficiently separated out by stream with carbon material, thus improving removal carbon material Ability.The another one critical process point of the present invention is using physics mode, carbon material to be purified.Using carbon material and carbonization Silicon grain degree principle of different sizes, the mode being combined with negative pressure and double-layer filter cloth, carbon material is further separated with carborundum, from And improve the purity of carbon material.In actual process operation, different according to the content situation of carbon impurity, adjust the ratio of decarbonizer And the size of negative pressure pressure can ultimately form the high purity carbon material that purity is more than 98%, also reach raising simultaneously and reclaimed carbon The purpose of SiClx powder content.
Brief description
Fig. 1 is the structural representation of carbon material equipment for purifying of the present invention;
In figure labelling: 1, pipeline, 2, cylindrical de- material cylinder, 3, negative pressure device, 4, filter cloth.
Specific embodiment
The method of purification of carbon material in a kind of carborundum, comprises the following steps:
Step one, weigh mass concentration be 20%-40% silicon carbide slurry, the silicon carbide slurry weighing is put in flotation column, And it is added thereto to liquid detergent, Polyethylene Glycol and compound advanced alcohol, after being sufficiently mixed, it is passed through sky from the nozzle of the bottom of flotation column Gas, makes mixed slurry standby after being sufficiently mixed with air in flotation column;
Step 2, control pressure make the mixed slurry liquid level in step one form certain difference in height, mixed slurry with excessive groove The bubble being mixed to form with air forms carbon alveolar layer with enrichment under liquid detergent, Polyethylene Glycol and compound advanced alcohol collective effect, Flotation column is centrally formed a kind of thrust, makes to overflow flotation column formation high-carbon slip outside carbon alveolar layer, standby;
Step 3, the high-carbon being formed in step 2 slip is introduced cylindrical de- material cylinder by pipeline, start cylindrical de- material cylinder The negative pressure device of bottom, high-carbon slip is 3-8um filter cloth by two-layer aperture to carry out separating, and the low slip of carbon amounts passes through filter cloth Come together in cylindrical de- material cylinder, high-carbon slip is blocked on filter cloth, make formation carbon content outside filter cloth be maintained at more than 98% High purity carbon material, standby;
Step 4, the carbon material isolating upper strata filter cloth take out, and form product after dehydration.
Further, the nozzle described in step one is Laval nozzle.Using compound advanced alcohol be r- alkyl be combined height Level alcohol, in slip per ton, liquid detergent, Polyethylene Glycol, the addition of compound advanced alcohol are respectively 20 ml, 50-80 ml and 20- 40ml.
Further, the difference in height in described step 2 is 2-4cm.
Further, the negative pressure device pressure limit described in step 3 is 0.075-0.105mpa.
Explain the present invention below in conjunction with specific embodiment further.
Embodiment 1
The method of purification of carbon material in a kind of carborundum, comprises the following steps:
Step one, weigh the silicon carbide slurry that mass concentration is 20%, the silicon carbide slurry weighing is put in flotation column, and to Wherein add liquid detergent, Polyethylene Glycol and r- alkyl, wherein, liquid detergent in slip per ton, Polyethylene Glycol, compound advanced alcohol Addition is respectively 20 ml, 50 ml and 20ml, after being sufficiently mixed, is passed through air from the Laval nozzle of the bottom of flotation column, Make mixed slurry standby after being sufficiently mixed with air in flotation column;
Step 2, control pressure make difference in height, slip and the air of the mixed slurry liquid level in step one and excessive groove formation 2cm The bubble being mixed to form forms carbon alveolar layer with enrichment under liquid detergent, Polyethylene Glycol and compound advanced alcohol collective effect, in flotation column It is centrally formed a kind of thrust, make outside carbon alveolar layer, to overflow flotation column formation high-carbon slip, standby;
Step 3, the high-carbon being formed in step 2 slip is introduced cylindrical de- material cylinder by pipeline, start cylindrical de- material cylinder The negative pressure device of bottom, pressure limit is 0.075mpa, and high-carbon slip is 3-8um filter cloth by two-layer aperture to carry out separating, Make high-carbon slip be distributed in the low slip of the phosphorus content outside subnormal ambient, being separated to come together in confined space, make outside Form carbon content and be maintained at more than 98% high purity carbon material, standby;
Step 4, the carbon material isolating upper strata filter cloth take out, and form product after dehydration.
Embodiment 2
The method of purification of carbon material in a kind of carborundum, comprises the following steps:
Step one, weigh the silicon carbide slurry that mass concentration is 30%, the silicon carbide slurry weighing is put in flotation column, and to Wherein add liquid detergent, Polyethylene Glycol and r- alkyl, wherein, liquid detergent in slip per ton, Polyethylene Glycol, compound advanced alcohol Addition is respectively 20 ml, 60 ml and 40ml, after being sufficiently mixed, is passed through air from the Laval nozzle of the bottom of flotation column, Make mixed slurry standby after being sufficiently mixed with air in flotation column;
Step 2, control pressure make difference in height, slip and the air of the mixed slurry liquid level in step one and excessive groove formation 3cm The bubble being mixed to form forms carbon alveolar layer with enrichment under liquid detergent, Polyethylene Glycol and compound advanced alcohol collective effect, in flotation column It is centrally formed a kind of thrust, make outside carbon alveolar layer, to overflow flotation column formation high-carbon slip, standby;
Step 3, the high-carbon being formed in step 2 slip is introduced cylindrical de- material cylinder by pipeline, start cylindrical de- material cylinder The negative pressure device of bottom, pressure limit is 0.095mpa, and high-carbon slip is 3-8um filter cloth by two-layer aperture to carry out separating, Make high-carbon slip be distributed in the low slip of the phosphorus content outside subnormal ambient, being separated to come together in confined space, make outside Form carbon content and be maintained at more than 98% high purity carbon material, standby;
Step 4, the carbon material isolating upper strata filter cloth take out, and form product after dehydration.
Embodiment 3
The method of purification of carbon material in a kind of carborundum, comprises the following steps:
Step one, weigh the silicon carbide slurry that mass concentration is 40%, the silicon carbide slurry weighing is put in flotation column, and to Wherein add liquid detergent, Polyethylene Glycol and r- alkyl, wherein, liquid detergent in slip per ton, Polyethylene Glycol, compound advanced alcohol Addition is respectively 20 ml, 80 ml and 40ml, after being sufficiently mixed, is passed through air from the Laval nozzle of the bottom of flotation column, Make mixed slurry standby after being sufficiently mixed with air in flotation column;
Step 2, control pressure make difference in height, slip and the air of the mixed slurry liquid level in step one and excessive groove formation 4cm The bubble being mixed to form forms carbon alveolar layer with enrichment under liquid detergent, Polyethylene Glycol and compound advanced alcohol collective effect, in flotation column It is centrally formed a kind of thrust, make outside carbon alveolar layer, to overflow flotation column formation high-carbon slip, standby;
Step 3, the high-carbon being formed in step 2 slip is introduced cylindrical de- material cylinder by pipeline, start cylindrical de- material cylinder The negative pressure device of bottom, pressure limit is 0.105mpa, and high-carbon slip is 3-8um filter cloth by two-layer aperture to carry out separating, Make high-carbon slip be distributed in the low slip of the phosphorus content outside subnormal ambient, being separated to come together in confined space, make outside Form carbon content and be maintained at more than 98% high purity carbon material, standby;
Step 4, the carbon material isolating upper strata filter cloth take out, and form product after dehydration.

Claims (5)

1. in a kind of carborundum carbon material method of purification it is characterised in that: comprise the following steps:
Step one, weigh mass concentration be 20%-40% silicon carbide slurry, the silicon carbide slurry weighing is put in flotation column, And it is added thereto to liquid detergent, Polyethylene Glycol and compound advanced alcohol, after being sufficiently mixed, it is passed through sky from the nozzle of the bottom of flotation column Gas, makes mixed slurry standby after being sufficiently mixed with air in flotation column;
Step 2, control pressure make the mixed slurry liquid level in step one form certain difference in height, mixed slurry with excessive groove The bubble being mixed to form with air forms carbon alveolar layer with enrichment under liquid detergent, Polyethylene Glycol and compound advanced alcohol collective effect, Flotation column is centrally formed a kind of thrust, makes to overflow flotation column formation high-carbon slip outside carbon alveolar layer, standby;
Step 3, the high-carbon being formed in step 2 slip is introduced cylindrical de- material cylinder by pipeline, start cylindrical de- material cylinder The negative pressure device of bottom, high-carbon slip is 3-8um filter cloth by two-layer aperture to carry out separating, and the low slip of carbon amounts passes through filter cloth Come together in cylindrical de- material cylinder, high-carbon slip is blocked on filter cloth, make formation carbon content outside filter cloth be maintained at more than 98% High purity carbon material, standby;
Step 4, the carbon material isolating upper strata filter cloth take out, and form product after dehydration.
2. as claimed in claim 1 in a kind of carborundum carbon material method of purification it is characterised in that: the nozzle described in step one For Laval nozzle.
3. as claimed in claim 1 in a kind of carborundum carbon material method of purification it is characterised in that: the height in described step 2 Degree difference is 2-4cm.
4. as claimed in claim 1 in a kind of carborundum carbon material method of purification it is characterised in that: the negative pressure described in step 3 Device pressure limit is 0.075-0.105mpa.
5. as claimed in claim 1 in a kind of carborundum carbon material method of purification it is characterised in that: in described step one, adopt Compound advanced alcohol is r- alkyl compound advanced alcohol, liquid detergent, Polyethylene Glycol, the addition of compound advanced alcohol in slip per ton Amount is respectively 20 ml, 50-80ml and 20-40ml.
CN201610771808.9A 2016-08-31 2016-08-31 Method for purifying carbon materials in silicon carbide Pending CN106365168A (en)

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Citations (6)

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Publication number Priority date Publication date Assignee Title
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CN102923705A (en) * 2012-11-22 2013-02-13 宁夏东方钽业股份有限公司 Method for removing free carbon in carborundum micro powder
CN103008093A (en) * 2012-12-05 2013-04-03 平顶山易成新材料股份有限公司 Method for separating free carbon from ultra-fine silicon carbide powder
CN104211064A (en) * 2014-08-29 2014-12-17 平顶山易成新材料有限公司 Impurity removing process for enhancing quality of silicon carbide fine micro powder
CN104874489A (en) * 2015-05-21 2015-09-02 许昌皓邦新能源科技有限公司 Carbon removal device for silicon carbide
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Publication number Priority date Publication date Assignee Title
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CN102923705A (en) * 2012-11-22 2013-02-13 宁夏东方钽业股份有限公司 Method for removing free carbon in carborundum micro powder
CN103008093A (en) * 2012-12-05 2013-04-03 平顶山易成新材料股份有限公司 Method for separating free carbon from ultra-fine silicon carbide powder
CN104211064A (en) * 2014-08-29 2014-12-17 平顶山易成新材料有限公司 Impurity removing process for enhancing quality of silicon carbide fine micro powder
CN104874489A (en) * 2015-05-21 2015-09-02 许昌皓邦新能源科技有限公司 Carbon removal device for silicon carbide
CN104986767A (en) * 2015-06-03 2015-10-21 河南新大新材料股份有限公司 Carbon removing apparatus and method for silicon carbide micropowder

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Application publication date: 20170201