CN101804982B - Purification method of silicon carbide superfine micropowder - Google Patents
Purification method of silicon carbide superfine micropowder Download PDFInfo
- Publication number
- CN101804982B CN101804982B CN2010101468345A CN201010146834A CN101804982B CN 101804982 B CN101804982 B CN 101804982B CN 2010101468345 A CN2010101468345 A CN 2010101468345A CN 201010146834 A CN201010146834 A CN 201010146834A CN 101804982 B CN101804982 B CN 101804982B
- Authority
- CN
- China
- Prior art keywords
- slip
- purification
- silicon carbide
- classification
- raw 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.)
- Active
Links
Abstract
The invention discloses a purification method of silicon carbide superfine micropowder, which comprises the following steps: mechanically crushing and shaping the selected silicon carbide raw material, washing the shaped raw material with initial water to remove carbon and magnetically separating the washed raw material to remove partial impurities on the surface; airing and drying the raw material washed with initial water, and carrying out crushing by a raymond mill and air flow classification to produce a product the grain diameter of which is between 1 and 15mu m; adding the product into a purification kettle, adding water to produce slurry, adding a flotation agent for floating to remove carbon, wherein the floating agent is kerosene and terpineol; respectively adding hydrochloric acid, sulfuric acid and hydrofluoric acid into the purification kettle; stirring the mixture and then washing with water until the pH value reaches about 7; adding solid sodium hydroxide and solid calcium hydroxide into the purification kettle then washing with water after stirring; and feeding the washed mixture to a classification kettle for classification after the pH value reaches 7. Through the purification treatment by using silicon carbide, the superfine micropowder is easy to separate. The product has the advantages of high purity, small grain diameter distribution, uniform grains, fewer impurities, high quality and wider application range.
Description
Technical field
The present invention relates to the purification process of a kind of production technology of silit, particularly a kind of silicon carbide super micro powder.
Background technology
Characteristics such as silit has stable chemical performance, and thermal conductivity is high, and thermal expansivity is low, and hardness is high, and wear resistance and self-sharpening are strong extensively are used in industries such as processing rigid alloy and opticglass.In recent years, along with the development of world semiconductor industry, silit is in the multi-thread cutting of silicon single crystal, polysilicon, piezoelectric quartz crystal and grind and be used widely, and is especially all the more so in the photovoltaic industry of high speed development.Its quality is not only relevant with its purity, and relevant with its particle fineness, and its purity is high more, thinner its application quality of particle is high more, and range of application is wide more.And traditional working method can only be produced the product about 10 μ m, and size distribution is too big, and particle is inhomogeneous; Impurity is more; Owing to do not carry out purification process, or mode is not right, handles not thorough; Impurity such as the iron cpd of the weak magnetic of the irony in the slip, nonmagnetics, carbon, free silica, silicon-dioxide can not be removed, and will cause ultra-fine micropowder not easily separated.
Summary of the invention
The technical problem that the present invention will solve is the deficiency to prior art, has proposed a kind of purification process of silicon carbide super micro powder of efficient removal impurity.
The technical problem that the present invention will solve realizes that through following technical scheme a kind of purification process of silicon carbide super micro powder is characterized in:
The sic raw material of choosing, after Mechanical Crushing, shaping, carry out just washing de-carbon, magnetic separation, remove partly impurity of surface;
Just the raw material after the washing is produced the product of particle diameter between 1-15 μ m through behind the dryness in the sun behind Raymond machine pulverizing, air classification;
The product after the above-mentioned classification, be added in the purification kettle, add water and process slip; The mass percent concentration of slip is 30%; Add flotation agent simultaneously and carry out the flotation de-carbon, flotation agent is kerosene and pine camphor oil, and the add-on of every kind of oil is that slip per ton adds the 80-120 milliliter; After de-carbon finishes; In purification kettle, add concentration more respectively and be 36% hydrochloric acid, concentration and be 98% sulfuric acid, concentration and be 35% hydrofluoric acid; Slip per ton adds hydrochloric acid 5-7 kilogram, sulfuric acid 5-7 kilogram, hydrofluoric acid 0.5-0.7 kilogram; Addition sequence is first hydrochloric acid, sulfuric acid, adds hydrofluoric acid at last, stirs 10 hours; And then with clear water towards 3-4 time, the pH in its slip is reached about 7; In purification kettle, add solid sodium hydroxide, solid hydrogen quicklime again; Slip per ton adds sodium hydroxide 6-8 kilogram, calcium hydroxide 6-8 kilogram, stirred 10 hours, and then with flushing with clean water 3-4 time; Make the pH of its slip reach 7, can deliver to the classification still and carry out classification.The technical problem that the present invention will solve can also further realize that just wash in the de-carbon process, it is the 280-350 milliliter that silit per ton adds the kerosene amount through following technical scheme.
The present invention compared with prior art carries out purification process through silit, the ultra-fine micropowder separate easily.Its product purity is high, size distribution is little, uniform particles, impurity is few, quality is high, and range of application is wide more.
Embodiment
A kind of purification process of silicon carbide super micro powder, its process step is:
The sic raw material of choosing; (be shaped as down the step thunder and cover to grind and create conditions, reduce it and produce load, through Mechanical Crushing, shaping because the high speed rotating during shaping; Can be a material surface Impurity removal part) after carry out just washing de-carbon, magnetic separation, remove partly impurity of surface;
Just the raw material after the washing is produced the product of particle diameter between 1-15 μ m through behind the dryness in the sun behind Raymond machine pulverizing, air classification; Just in the washing de-carbon process, it is the 280-350 milliliter that silit per ton adds the kerosene amount.
The product after the above-mentioned classification, be added in the purification kettle, add water and process slip; The mass percent concentration of slip is 30%; Add flotation agent simultaneously and carry out the flotation de-carbon, flotation agent is kerosene and pine camphor oil, and the add-on of every kind of oil is that slip per ton adds the 80-120 milliliter; After de-carbon finishes; In purification kettle, add concentration more respectively and be 36% hydrochloric acid, concentration and be 98% sulfuric acid, concentration and be 35% hydrofluoric acid; Slip per ton adds hydrochloric acid 5-7 kilogram, sulfuric acid 5-7 kilogram, hydrofluoric acid 0.5-0.7 kilogram; Addition sequence is first hydrochloric acid, sulfuric acid, adds hydrofluoric acid at last, stirs 10 hours; And then with clear water towards 3-4 time, the pH in its slip is reached about 7; In purification kettle, add solid sodium hydroxide (solid 99.8%), solid hydrogen quicklime (solid 99.8%) (weight ratio of two kinds of alkali is 1: 1) etc. again; Slip per ton adds sodium hydroxide 6-8 kilogram, calcium hydroxide 6-8 kilogram; Stirred 10 hours; And then, make the pH of its slip reach 7 with flushing with clean water 3-4 time, can deliver to the classification still and carry out classification.
Claims (2)
1. the purification process of a silicon carbide super micro powder is characterized in that:
The sic raw material of choosing, after Mechanical Crushing, shaping, carry out just washing de-carbon, magnetic separation, remove partly impurity of surface;
Just the raw material after the washing is produced the product of particle diameter between 1-15 μ m through behind the dryness in the sun behind Raymond machine pulverizing, air classification;
The product after the above-mentioned classification, be added in the purification kettle, add water and process slip; The mass percent concentration of slip is 30%; Add flotation agent simultaneously and carry out the flotation de-carbon, flotation agent is kerosene and pine camphor oil, and the add-on of every kind of oil is that slip per ton adds the 80-120 milliliter; After de-carbon finishes; In purification kettle, add concentration more respectively and be 36% hydrochloric acid, concentration and be 98% sulfuric acid, concentration and be 35% hydrofluoric acid; Slip per ton adds hydrochloric acid 5-7 kilogram, sulfuric acid 5-7 kilogram, hydrofluoric acid 0.5-0.7 kilogram; Addition sequence is first hydrochloric acid, sulfuric acid, adds hydrofluoric acid at last, stirs 10 hours; And then with clear water towards 3-4 time, the pH in its slip is reached about 7; In purification kettle, add solid sodium hydroxide, solid hydrogen quicklime again; Slip per ton adds sodium hydroxide 6-8 kilogram, calcium hydroxide 6-8 kilogram, stirred 10 hours, and then with flushing with clean water 3-4 time; Make the pH of its slip reach 7, can deliver to the classification still and carry out classification.
2. the purification process of silicon carbide super micro powder according to claim 1 is characterized in that: just wash in the de-carbon process, it is the 280-350 milliliter that silit per ton adds the kerosene amount.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101468345A CN101804982B (en) | 2010-04-15 | 2010-04-15 | Purification method of silicon carbide superfine micropowder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101468345A CN101804982B (en) | 2010-04-15 | 2010-04-15 | Purification method of silicon carbide superfine micropowder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101804982A CN101804982A (en) | 2010-08-18 |
| CN101804982B true CN101804982B (en) | 2012-06-06 |
Family
ID=42606965
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101468345A Active CN101804982B (en) | 2010-04-15 | 2010-04-15 | Purification method of silicon carbide superfine micropowder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101804982B (en) |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920959B (en) * | 2009-06-15 | 2014-04-16 | 江苏乐园新材料集团有限公司 | Process for purifying silicon carbide micro powder for linear cutting |
| CN102190300A (en) * | 2011-04-13 | 2011-09-21 | 河南城建学院 | Method for comprehensive utilization of coal gangue |
| CN102320602A (en) * | 2011-08-18 | 2012-01-18 | 白山峰泰源研磨材有限公司 | Purifying method of green silicon-carbide micropowder |
| CN102424385B (en) * | 2011-09-08 | 2013-03-13 | 新疆新路标光伏材料有限公司 | Apparatus and method for removing free carbon in carbonized silicon micropowder |
| CN102502638A (en) * | 2011-10-08 | 2012-06-20 | 江苏佳宇资源利用股份有限公司 | Method for removing free carbons from fine-grained silicon carbides |
| CN102432011A (en) * | 2011-10-08 | 2012-05-02 | 江苏佳宇资源利用股份有限公司 | Method for synchronously removing iron and silicon impurities in silicon carbide micro-powder |
| CN102951641B (en) * | 2012-11-01 | 2014-05-14 | 临沭山田研磨材有限公司 | Water-saving and environmental protection-type preparation method of silicon carbide micro-powder for silicon wafer wire cutting |
| CN102923706B (en) * | 2012-11-29 | 2015-04-29 | 江苏乐园新材料集团有限公司 | Preparation method of silicon carbide micro powder capable of improving dispersity |
| CN103923605B (en) * | 2014-03-14 | 2015-12-02 | 唐山圣诺纳微科技有限公司 | A kind of making method of silicon carbide ball |
| CN103922756B (en) * | 2014-04-28 | 2015-04-15 | 湖南金马铝业有限责任公司 | Surface treatment process method for silicon carbide powder |
| CN104261409B (en) * | 2014-09-29 | 2016-08-24 | 平顶山易成新材料有限公司 | A kind of preparation method of the silicon carbide powder as organic composite material reinforcement |
| CN106276907A (en) * | 2016-08-23 | 2017-01-04 | 怀远县金浩电子科技有限公司 | A kind of processing method of lightning protection device carbide fine powder |
| CN107640742B (en) * | 2017-11-17 | 2023-01-06 | 江西硅辰科技有限公司 | Silicon-based efficient solid hydrogen production agent |
| CN110272772B (en) * | 2019-08-05 | 2021-02-19 | 中南大学 | Preparation method of ultra-pure anthracite |
| CN113277515A (en) * | 2020-09-30 | 2021-08-20 | 连云港市沃鑫高新材料有限公司 | High-purity silicon carbide micro powder for silicon wafer cutting and preparation device and method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1689718A (en) * | 2004-04-21 | 2005-11-02 | 尹克胜 | Waste sand treating method in crystal processing |
| CN101033066A (en) * | 2006-03-06 | 2007-09-12 | 张捷平 | Method of recovering silicon carbide micro-powder |
-
2010
- 2010-04-15 CN CN2010101468345A patent/CN101804982B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1689718A (en) * | 2004-04-21 | 2005-11-02 | 尹克胜 | Waste sand treating method in crystal processing |
| CN101033066A (en) * | 2006-03-06 | 2007-09-12 | 张捷平 | Method of recovering silicon carbide micro-powder |
Non-Patent Citations (1)
| Title |
|---|
| 赵平等.陶瓷级碳化硅微粉提纯试验研究.《非金属矿》.2009,第32卷(第4期),文章内容 1样品性质及工艺流程，2 试验方法. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101804982A (en) | 2010-08-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101804982B (en) | Purification method of silicon carbide superfine micropowder | |
| CN110510620B (en) | Purification method of high-purity quartz sand tailings | |
| CN102249236B (en) | Production process for silicon carbide micropowder | |
| CN100528488C (en) | Method for recycling silica powder and carborundum powder from cut waste mortar | |
| CN102285654B (en) | Production method of silicon wafer cutting blade material | |
| CN107555426B (en) | Low-energy-consumption large-batch preparation process of high-purity microcrystalline graphite and high-purity microcrystalline graphite prepared by same | |
| CN101623898B (en) | Chemical recovery method for mortar in wire cutting technology | |
| CN101391871A (en) | Method for preparing high purity quartz sand | |
| CN100571877C (en) | High-iron bauxite ferro-aluminum comprehensive utilization of separation method | |
| CN101475172A (en) | Recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder | |
| CN104387094B (en) | Technique recycled by a kind of steel-making refractory materials | |
| CN107661810A (en) | A kind of method that arkose quartzite prepares glass sand | |
| CN102527492A (en) | Method for preparing super iron ore concentrate by using low-grade magnetic iron ore | |
| WO2022057227A1 (en) | Illite, preparation method therefor and use thereof | |
| JP2010168255A (en) | Method for removing metal-containing material and method for refining silicon | |
| CN115178363A (en) | Preparation of ultra-pure quartz powder from argillaceous quartzite and comprehensive utilization process | |
| CN101811699B (en) | Method of recycling silicon carbide powder | |
| CN103803981A (en) | Method for preparing submicron silicon carbide powder | |
| CN101392326B (en) | Method for recovering gold from all-sliming cyanidation gold extraction slag | |
| CN101215074B (en) | Production technique for drawing crystal powder used for low-hydroxyl quartz glass soft pipe and pipe drawing method | |
| CN108394903A (en) | A kind of preparation method of nanometer silicon carbide micro mist | |
| CN106915757B (en) | A kind of Brown Alundum super fine purifying technique | |
| RU2492143C1 (en) | Method of producing high-quality quartz grit | |
| CN110885239A (en) | Preparation method of high-purity fused quartz powder | |
| CN102773149B (en) | Dressing and purification method of powder quartz |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| ASS | Succession or assignment of patent right |
Owner name: LIANYUNGANG WOXIN NEW HIGH-TECH. MATERIAL CO., LTD Free format text: FORMER OWNER: LIANYUNGANG DONGDU SILICON CARBIE CO., LTD. Effective date: 20110329 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 222300 STATIONED PLACE IN SHILIANGHE TOWN, DONGHAI COUNTY, LIANYUNGANG CITY, JIANGSU PROVINCE TO: 222300 WEST OF WEIXING RIVER, SOUTH OF JIXIANG ROAD, WEST AREA OF DONGHAI ECONOMIC DEVELOPMENT ZONE, DONGHAI COUNTY, LIANYUNGANG CITY, JIANGSU PROVINCE |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20110329 Address after: 222300, Lianyungang, Jiangsu, Donghai County East China Sea Economic Development Zone, the west side auspicious Road South, satellite Hexi Applicant after: Lianyungang Woxin High-Technology Materials Co., Ltd. Address before: 222300 Jiangsu city of Lianyungang province Donghai County Shilianghe town resident Applicant before: Lianyungang Dongdu Silicon Carbide Co., Ltd. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20100818 Assignee: Lianyungang Dongdu Silicon Carbide Co., Ltd. Assignor: Lianyungang Woxin High-Technology Materials Co., Ltd. Contract record no.: 2013320000525 Denomination of invention: Purification method of silicon carbide superfine micropowder Granted publication date: 20120606 License type: Exclusive License Record date: 20130606 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model |