CN102502638A - Method for removing free carbons from fine-grained silicon carbides - Google Patents
Method for removing free carbons from fine-grained silicon carbides Download PDFInfo
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- CN102502638A CN102502638A CN2011102945581A CN201110294558A CN102502638A CN 102502638 A CN102502638 A CN 102502638A CN 2011102945581 A CN2011102945581 A CN 2011102945581A CN 201110294558 A CN201110294558 A CN 201110294558A CN 102502638 A CN102502638 A CN 102502638A
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Abstract
The invention discloses a method for removing free carbons (F.C) from fine-grained silicon carbides. According to the method, light diesel oil and industrial 4# oil are used as floatation agents, and the free carbons in the fine-grained silicon carbides are removed by a floatation method, so that the content of the F.C in the fine-grained silicon carbides can be greatly reduced to be below 0.12%; and the process is simple and convenient to realize, and new impurities cannot be introduced into the silicon carbide materials in the industrial production process. By means of the method, the control over the content index of the free carbons in the fine-grained silicon carbide products can be fully guaranteed.
Description
Technical field
The present invention relates to a kind of purifying method of removing impurity in the particulate silit, particularly relate to a kind of method that removes particulate silit Free Carbon.
Background technology
Silit (SiC) is a kind of important synthetic ceramic, has characteristics such as high firmness, high-wearing feature, erosion resistance and good high-temperature intensity.In non-oxidized substance hi-tech refractory raw materials such as contemporary C, N, B, silit is extensive, the most most economical a kind of for using.At present the industrial silit of China is divided into two kinds of black silicon carbide and green silicon carbides, is hexagonal, and proportion is 3.20～3.25, and microhardness is 2840～3320kg/mm
2
China is the big producing country and the big export country of silit, and the silit ultimate production reached about 53.5 ten thousand tons in 2009, accounts for 56.3% of whole world sum, ranks first in the world; 2010, domestic only green silicon carbide output was above 1,000,000 tons.In recent years, under the drive of low-carbon economy spring tide, the fast development of photovoltaic industry, as the material that photovoltaic industry is used, the silit particularly selling market of green silicon carbide is fiery unusually.
Silit is to be that raw material forms through the resistance furnace pyrotic smelting with silica sand, refinery coke (or coal tar), wood chip.Producing and the grinding and processing process, often having the uncombined carbon (F.C) of high level in the particulate silit.F.C content is generally 2.0～4.0% in the coarse fodder silit, even higher.
According to the national standard of common silicon carbide abrasive, as silicon carbide micro-powder product requirement F.C%≤0.70 of abrasive material use.At present, domestic photovoltaic industry is general many below 0.12 or 0.15 with the F.C% working control index of silicon carbide micro-powder abrasive material new product.The resource recovery type silicon carbide micro-powder product F .C% controlling index that applicant Jiangsu Jiayu Electronic Material CO., Ltd. is supplied is below 0.60.
Summary of the invention
The objective of the invention is in order to solve the problem that removes of particulate silit Free Carbon content overproof, and proposed a kind of method that removes particulate silit Free Carbon.
The objective of the invention is to realize like this: a kind of method that removes particulate silit Free Carbon, this method may further comprise the steps:
(1) flotation: in flotation machine, add particulate carbonization silica sand slurry successively, flotation reagent; Flotation reagent comprises trapping agent and pore forming material; With the solar oil is trapping agent, is pore forming material with No. 4 oil of industry; After stirring mediation, air flotation; After 1.0～3.0 hours, remove foam layer;
(2) collect flotation machine bottom land mortar, through dehydration, dry and obtain particulate silit highly finished product.
Solar oil comprises catalytic cracking solar oil and straight distillation light diesel oil in the method steps described in the invention (1); F.C% in the particulate silit (coarse fodder)>=2.5% o'clock, preferred catalytic cracking solar oil; F.C%≤2.5% o'clock, preferred straight distillation light diesel oil.
The flotation reagent consumption is the dried particulate silit of 50g～130g/t in the method steps described in the invention (1), and wherein: the solar oil consumption is the dried particulate silit of 35～100g/t, and No. 4 oily consumptions of industry are the dried particulate silit of 15～35g/t.
The mode that removes foam layer in the method steps described in the invention (1) comprises that machinery is scraped and gets or overflow from the mortar face.
Principle of the present invention: big quantity research shows that particulate silit (coarse fodder) the Free Carbon overwhelming majority is the amorphousness form, and quality is soft, and natural flotation property is better.Consider the composition characteristic and the F.C content situation of silit coarse fodder, the collecting performance to trapping agent in floatation process has higher requirements, and is then relatively low to its selectivity requirement, better to the latherability requirement of pore forming material.
The present invention selects solar oil as trapping agent, and it is big that it forms fluctuation ratio kerosene, and especially aromaticity content is more much higher than straight distillation light diesel oil like aromaticity content in the catalytic cracking solar oil; Generally, the collecting performance of solar oil is higher than kerosene, but selectivity is not as kerosene.Solar oil is big because of its molecular weight, so viscosity is higher, dispersive oil droplet size is big in water, and surface spreading becomes the speed of oil film slow, but its hydrophobicity is strong, and is therefore, more favourable as the collecting agent of particulate silit Free Carbon during flotation.
No. 4 oily main raw materials of industry are the sub products in the synthesizing polyethylene alcohol process, and wide material sources wherein contain low amounts of resin impurity, and price is low, and latherability is strong than No. 2 oil.Simultaneously, such pore forming material decomposes in tail water very soon, oxidation, loses deleterious effect.
Advantage of the present invention is: the present invention utilizes method for floating to remove the uncombined carbon in the particulate silit; Can reduce significantly below the F.C content to 0.12% in the particulate silit; And technology realizes easy, in Industrial processes, can not introduce new impurity to silicon carbide materials.Adopt present method, the control of particulate silicon carbide products Free Carbon content's index can be fully guaranteed.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1:
Get the GC2000+ type particulate silit coarse fodder behind Jiangsu Jiayu Electronic Material CO., Ltd.'s air classification, through detecting its SiC purity 94.5%, particle diameter D
50Be worth 3.5 μ m, F.C content 2.12%.
The above-mentioned GC2000+ type of 400Kg particulate silit coarse fodder is joined in the stirred pot, add 300 kilograms of ionized waters, starch as particulate carbonization silica sand the back that stirs.
In the SF-0.70 type flotation machine, add above-mentioned particulate carbonization silica sand slurry, 44g flotation reagent (wherein: 32g straight distillation light diesel oil, No. 4 oil of 12g industry) successively, after stirring was in harmonious proportion, the beginning air flotation after 1.5 hours, was scraped the mode of getting through machinery and is removed foam layer; Collect flotation machine bottom land mortar, through dehydration, dry and obtain particulate silit highly finished product.Through detecting, its F.C content is 0.08%.
Embodiment 2:
Get the particulate silit coarse fodder that is purchased from market, Henan, through detecting its SiC purity 97.6%, particle diameter D
50Be worth 5.5 μ m, F.C content 1.11%.
The above-mentioned particulate dust of 1000Kg is joined in the stirred pot, add 800 kilograms of ionized waters, starch as particulate carbonization silica sand the back that stirs.
In the XJ-2.8 type flotation machine, add above-mentioned particulate carbonization silica sand slurry, 80g flotation reagent (wherein: 60g catalytic cracking solar oil, No. 4 oil of 20g industry) successively; After stirring mediation; The beginning air flotation after 1.5 hours, is scraped the mode of getting through machinery and is removed foam layer; Collect flotation machine bottom land mortar, through dehydration, dry and obtain particulate silit highly finished product.Through detecting, its F.C content is 0.05%.
Embodiment 3:
Get particulate dust in the sack cleaner of Jiangsu Jiayu Electronic Material CO., Ltd.'s silicon carbide micro-powder air classification technology, through detecting its SiC purity 93.0%, particle diameter D
50Be worth 2.1 μ m, F.C content 3.51%.
The above-mentioned particulate dust of 200Kg is joined in the stirred pot, add 200 kilograms of ionized waters, starch as particulate carbonization silica sand the back that stirs.
In the SF-0.37 type flotation machine, add above-mentioned particulate carbonization silica sand slurry, 23g flotation reagent (wherein: 16g catalytic cracking solar oil, No. 4 oil of 7g industry) successively; After stirring mediation; The beginning air flotation is after 1.0 hours, through removing foam layer from the mortar face mode of overflowing; Collect flotation machine bottom land mortar, through dehydration, dry and obtain the particulate dust highly finished product.Through detecting, its F.C content is 0.10%.
Claims (4)
1. method that removes particulate silit Free Carbon is characterized in that this method may further comprise the steps:
(1) flotation: in flotation machine, add particulate carbonization silica sand slurry successively, flotation reagent; Flotation reagent comprises trapping agent and pore forming material; With the solar oil is trapping agent, is pore forming material with No. 4 oil of industry; After stirring mediation, air flotation; After 1.0～3.0 hours, remove foam layer;
(2) collect flotation machine bottom land mortar, through dehydration, dry and obtain particulate silit highly finished product.
2. according to the said a kind of method that removes particulate silit Free Carbon of claim 1, it is characterized in that: solar oil comprises catalytic cracking solar oil and straight distillation light diesel oil described in the step (1); F.C% in the particulate silit (coarse fodder)>=2.5% o'clock, preferred catalytic cracking solar oil; F.C%≤2.5% o'clock, preferred straight distillation light diesel oil.
3. according to the said a kind of method that removes particulate silit Free Carbon of claim 1; It is characterized in that: flotation reagent consumption described in the step (1) is the dried particulate silit of 50g～130g/t; Wherein: the solar oil consumption is the dried particulate silit of 35～100g/t, and No. 4 oily consumptions of industry are the dried particulate silit of 15～35g/t.
4. according to the said a kind of method that removes particulate silit Free Carbon of claim 1, it is characterized in that: the mode that removes foam layer described in the step (1) comprises that machinery is scraped and gets or overflow from the mortar face.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011102945581A CN102502638A (en) | 2011-10-08 | 2011-10-08 | Method for removing free carbons from fine-grained silicon carbides |
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| CN2011102945581A CN102502638A (en) | 2011-10-08 | 2011-10-08 | Method for removing free carbons from fine-grained silicon carbides |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101491888A (en) * | 2009-03-05 | 2009-07-29 | 南昌大学 | Foam flotation method capable of separating silicon powder and carbon silicon powder |
| CN101804982A (en) * | 2010-04-15 | 2010-08-18 | 连云港东渡碳化硅有限公司 | Purification method of silicon carbide superfine micropowder |
| CN102173419A (en) * | 2011-02-28 | 2011-09-07 | 江苏科理德再生科技有限公司 | Method for recycling silicon powder from silicon slice cut waste mortar |
-
2011
- 2011-10-08 CN CN2011102945581A patent/CN102502638A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101491888A (en) * | 2009-03-05 | 2009-07-29 | 南昌大学 | Foam flotation method capable of separating silicon powder and carbon silicon powder |
| CN101804982A (en) * | 2010-04-15 | 2010-08-18 | 连云港东渡碳化硅有限公司 | Purification method of silicon carbide superfine micropowder |
| CN102173419A (en) * | 2011-02-28 | 2011-09-07 | 江苏科理德再生科技有限公司 | Method for recycling silicon powder from silicon slice cut waste mortar |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Application publication date: 20120620 |