CN1244495A - Preparation of superfine graphite powder - Google Patents
Preparation of superfine graphite powder Download PDFInfo
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- CN1244495A CN1244495A CN 98112934 CN98112934A CN1244495A CN 1244495 A CN1244495 A CN 1244495A CN 98112934 CN98112934 CN 98112934 CN 98112934 A CN98112934 A CN 98112934A CN 1244495 A CN1244495 A CN 1244495A
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Abstract
The present invention is a superfine graphite powder preparation process with low power consumption and high efficiency. Through jet efflux collision and auxiliary physical pulverization process, the present invention can produce pure graphite powder with average grain size lower than 2 microns. The technological process of the present invention includes the following steps in sequence: compounding graphite suspension according to graphite 0.5-40 wt% and suspending medium 60-99.5 wt% with selected dispersant accounting for 0.2-5 wt% of the suspending medium; and repeated pulverization to obtain superfine powder. The said process is used in producing superfine graphite powder for various industrial applications.
Description
The present invention relates to a kind of method of using jets collision and auxiliary physical influence to pulverize, is a kind of preparation method of superfine graphite powder specifically.
The superfine graphite powder body material is that the eighties just begins a kind of new and high technology material of growing up mid-term, and it has purposes very widely.The common method of preparation superfine graphite was mechanical ball milling method and comminution by gas stream during modernization industry was produced.The shortcoming of mechanical ball milling method is that energy consumption is big, efficient is low, 100kg graphite is behind 4 hours ball millings, only can obtain the superfine graphite powder of 2～5kg granularity through wet concentration less than 2 μ m, and be easy to sneak into impurity in the superfine graphite powder, therefore the graphite powder of pulverizing with the mechanical ball milling method can only be applied in some occasions not high to purity, granularity requirements usually; The shortcoming of comminution by gas stream is to be difficult to the graphite powder is crushed to submicron order, and general crushing level only rests on 3～7 μ m.Except that above two kinds of methods, also once the someone attempts making the superfine graphite powder with the jets collision method, this method is at first graphite granule to be mixed with suspension, and then use the jets collision method to repeat to pulverize, again superfine graphite suspension is carried out aftertreatment at last and make the graphite powder, but find in the practice that its crushing effect is unsatisfactory, graphite granule is crushed to 2 μ m when following at needs, even repeat to pulverize repeatedly, its mean particle size of pulverizing back graphite powder is still greater than 2 μ m.
The objective of the invention is to overcome the shortcoming of above-mentioned prior art and a kind of less energy-consumption, high efficiency preparation of superfine graphite powder are provided, adopt this method that the superfine graphite yield of mean particle size in the Graphite Powder 99 body＜2 μ m is improved greatly, and make purity height, the impurity of graphite powder few.
For finishing above-mentioned purpose, technical solution provided by the present invention is: a kind of preparation method of superfine graphite powder, and its special character is that it in turn includes the following steps:
The first, the preparation graphite suspension
To be mixed with graphite suspension after graphite granule, suspension medium, the dispersant, wherein the weight percent of graphite and suspension medium is: graphite 0.5～40, suspension medium 60～99.5, the add-on of dispersion agent is 0.2～5% of a suspension medium, and dispersion agent adopts non-ionic type, anionic, fluorine surface type tensio-active agent or is used.
The second, the graphite granule superfine grinding
Make the graphite suspension for preparing under high pressure pass through the cross micropore generation jets collision of single-crystal diamond, pulverize, and repeat this process to the granularity of graphite granule and reach requirement, operating pressure during jets collision is chosen as: when graphite granule particle diameter during greater than 10 μ m, operating pressure 500～1000MPa, when the graphite particle diameter when 5 μ m are between 10 μ m, operating pressure 800～150MPa, when the graphite particle diameter when 2 μ m are between 5 μ m, operating pressure 1000～1800MPa, when graphite particle diameter during less than 2 μ m, operating pressure 1500～2000MPa.
In the above-mentioned technical solution, the weight percent of graphite and suspension medium is in graphite suspension: graphite 8-18, suspension medium 82～92 o'clock have and pulverize preferably and production effect.When content of graphite 0.5% was following, production efficiency was low, and content was greater than 40% o'clock, and suspension is difficult to preparation and process for processing.
The crystal formation of graphite can be selected 3R, 2H type for use in the above-mentioned technical solution, and the granularity general requirement is less than 50 μ m, for enhancing productivity, can select for use granularity less than the graphite of 20 μ m for well.
Suspension medium in the above-mentioned technical solution plays carrier function, can select ordinary tap water, distilled water, saturated aqueous common salt or silicone oil etc. for use.
Aniorfic surfactant as dispersion agent in the above-mentioned technical solution adopts higher fatty acid salt, alkyl benzene sulfonate, sulfuric acid ester salt etc.; Nonionic surface active agent adopts long chain aliphatic alcohol polyethenoxy ether class, alkylphenol polyoxyethylene class, glycerine fatty acid fat and pentaerythritol fatty ester class, sorbitan fatty acid fat and sorbitan fatty acid ester class etc.
In the graphite suspension aftertreatment of the present invention, with graphite granule isolating method from suspension medium is to adopt sedimentation or centrifugal separation to separate, also can be to adopt other partition method to separate, when the graphite granule after the separation is dry, should be dry under less than 50 ℃ condition, when surpassing 50 ℃, the graphite powder is easy to caking.
Advantage of the present invention is:
1, the present invention selects anionic, non-ionic type, the drawing together property agent of the fluorine surface type surface dispersion agent as graphite suspension for use, and add-on only is 0.2～5% of a suspension medium, through evidence, it not only has dispersion effect preferably, but also can avoid graphite suspension big in the hurried change of viscosity after elementary pulverizing, hinders the shortcoming that continues pulverizing, in addition, because of its content is small, do not influence the purity of graphite powder, can not exert an influence to the follow-up use of graphite powder product.
2, the present invention thinks by analysis: in the jets collision of suspension, the strong extruding that jet produced, shearing friction power, and hyperacoustic power of tearing by force is to produce and act on graphite granule simultaneously, the size of on-load pressure has not only determined flow rate of fluid, also determined frequency of ultrasonic, have only when both reach best fit, just can produce crushing effect preferably, so the present invention is when pressurized fluidic clashes, for varigrained graphite suspension correspondence a corresponding pressure range, overcome and think that for a long time pressure is high more, jet speed is fast more, and crushing effect is good more technology prejudice just.
3, adopt the present invention can produce the superfine graphite powder of mean particle size＜1 μ m with comparalive ease, its yield can surpass 50%, reaches as high as 94%, adopts the present invention also can produce submicron down to nano level superfine graphite powder, and Unusually narrow particle size distribution.
4, adopting the present invention to produce the superfine graphite powder descends production efficiency raising, energy consumption.
Embodiment one:
The first, the preparation graphite suspension
With the 3R type graphite of mean particle size＜10 μ m graphite 17% by weight percentage, the proportioning of distilled water 83% is made graphite suspension, adds 0.5% sodium dodecyl benzenylsulfonate as dispersion agent, and preliminary mechanical stirring is to evenly;
The second, the graphite granule superfine grinding
With the graphite suspension that prepared cross micropore generation jets collision in pressure is the scope of 1200MPa, pulverize, and repeat three times, again triplicate under the pressure of 1800MPa by single-crystal diamond;
The 3rd, the aftertreatment of graphite suspension
To carry out graphite suspension behind the jets collision, adopt centrifugal separation, from wherein isolating graphite granule, and carry out drying, promptly obtain the superfine graphite powder in condition less than 50 ℃.
Gather resulting superfine graphite powder sample, test with the U.S. ZetaPlus of Brooker Hai Wen instrument company type laser light scattering particle size analyzer, wherein: particle diameter＜0.5 μ m accounts for 59%, and particle diameter＜1 μ m accounts for 70%, particle diameter＜4 μ m account for 100%, effective size of grain 1.2 μ m.
Embodiment two:
Selecting mean particle size for use is the Graphite Powder 99 of 30 μ m, and graphite 15% by weight percentage, and the proportioning of suspension medium saturated aqueous common salt 85% is mixed with graphite suspension, and the sodium laurylsulfonate of adding 0.5% stirs as dispersion agent.Under 700PMa pressure, pulverize three times, under 1000MPa pressure, pulverize three times again, test with the laser diffraction granularity instrument, wherein: particle diameter＜1 μ m accounts for 4.01%, particle diameter＜2 μ m account for 18.02%, particle diameter＜5 μ m account for 65.88%, and particle diameter＜10 μ m account for 94.18%, volume meta particle diameter 4.86 μ m.
Embodiment three:
Selecting mean particle size for use is the Graphite Powder 99 of 30 μ m, and graphite 10% by weight percentage, and the proportioning of suspension medium distilled water 90% is mixed with graphite suspension, and the tween-80 of adding 0.5% stirs as dispersion agent.Under 800MPa pressure, pulverize three times, under 1500MPa pressure, pulverize three times again, test with the laser diffraction granularity instrument, wherein: particle diameter＜1 μ m accounts for 15.08%, particle diameter＜2 μ m account for 35.20%, particle diameter＜5 μ m account for 78.92%, and particle diameter＜8 μ m account for 96.24%, volume meta particle diameter 3.68 μ m.
Embodiment four:
Selecting mean particle size for use is the Graphite Powder 99 of 2 μ m, and graphite 3% by weight percentage, and the proportioning of suspension medium distilled water 97% is mixed with graphite suspension, and the Sodium dodecylbenzene sulfonate of adding 2% stirs as dispersion agent.Pulverize five times under 1800MPa pressure, test with the laser light scattering particle size analyzer, wherein: particle diameter＜0.2 μ m accounts for 10.41%, particle diameter＜0.5 μ m accounts for 65.72%, particle diameter＜1 μ m accounts for 94.00%, and particle diameter＜8 μ m account for 96.24%, effective size of grain 0.6523 μ m.
Claims (5)
1, a kind of preparation of superfine graphite powder is characterized in that, in turn includes the following steps:
One, preparation graphite suspension
Graphite granule, suspension medium, dispersant are mixed with graphite suspension, wherein the weight percent of graphite and suspension medium is: graphite 0.5～40, suspension medium 60～99.5, the add-on of dispersion agent is 0.2～5% of a suspension medium, and dispersion agent adopts non-ionic type, anionic, fluorine surfactant or them to be used;
Two, graphite granule superfine grinding
Make the graphite suspension for preparing under high pressure pass through the cross micropore generation jets collision of single-crystal diamond, pulverize, and repeat this process to the granularity of graphite granule and reach requirement, operating pressure during jets collision is chosen as: when graphite granule particle diameter during greater than 10 μ m, operating pressure is 500～1000MPa; When the graphite particle diameter when 5 μ m are between 10 μ m, operating pressure is 800～1500MPa; When the graphite particle diameter when 2 μ m are between 5 μ m, operating pressure is 1000～1800MPa; When graphite particle diameter during less than 2 μ m, operating pressure is 1500～2000MPa.
2, preparation of superfine graphite powder as claimed in claim 1 is characterized in that, the weight percent of graphite and suspension medium is in the described graphite suspension: graphite 8～18, suspension medium 82～92.
3, preparation of superfine graphite powder as claimed in claim 1 or 2 is characterized in that, in described dispersion agent, aniorfic surfactant adopts higher fatty acid salt, alkyl benzene sulfonate, sulfuric acid ester salt; Nonionic surface active agent adopts long chain aliphatic alcohol polyethenoxy ether class, alkylphenol polyoxyethylene class, glycerine fatty acid fat and pentaerythritol fatty ester class, sorbitan fatty acid fat and sorbitan fatty acid ester class.
4, preparation of superfine graphite powder as claimed in claim 1 or 2, it is characterized in that, after graphite granule superfine grinding step, also comprise the graphite suspension post-processing step, this step comprise with graphite granule from suspension, separate with will separate after graphite granule carry out drying.
5, preparation of superfine graphite powder as claimed in claim 4 is characterized in that, the drying temperature the when graphite granule after the described separation carries out drying is less than 50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98112934 CN1244495A (en) | 1998-08-10 | 1998-08-10 | Preparation of superfine graphite powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98112934 CN1244495A (en) | 1998-08-10 | 1998-08-10 | Preparation of superfine graphite powder |
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| CN1244495A true CN1244495A (en) | 2000-02-16 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086962C (en) * | 1999-01-25 | 2002-07-03 | 孔令和 | Automatically controlled multifunctional superfine pulverizer |
| CN102390829A (en) * | 2011-07-26 | 2012-03-28 | 大同新成新材料股份有限公司 | Graphite powder used in furnace end, Acheson furnace end structure and maintenance method thereof |
| CN102689895A (en) * | 2010-12-30 | 2012-09-26 | 王宏晓 | Preparation method and application of high-purity high-fineness graphite powder |
| CN103964420A (en) * | 2011-09-27 | 2014-08-06 | 王宏晓 | Preparation method of high-purity high-fineness graphite powder |
| CN105060281A (en) * | 2015-07-22 | 2015-11-18 | 深圳市贝特瑞新能源材料股份有限公司 | Nano-graphite slurry preparation method |
| CN105985838A (en) * | 2015-02-04 | 2016-10-05 | 青岛路比特化学有限公司 | Graphite lubricating oil friction-reducing additive and preparation method thereof |
| CN105985834A (en) * | 2015-02-04 | 2016-10-05 | 青岛路比特化学有限公司 | Energy-saving and anti-friction graphite lubricating oil and preparation method therefor |
| CN106554012A (en) * | 2016-10-11 | 2017-04-05 | 江苏华力索菲新材料有限公司 | The preparation method of modified superfine Graphene |
| CN107500285A (en) * | 2017-09-30 | 2017-12-22 | 湖南国盛石墨科技有限公司 | The preparation method of superfine graphite |
-
1998
- 1998-08-10 CN CN 98112934 patent/CN1244495A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086962C (en) * | 1999-01-25 | 2002-07-03 | 孔令和 | Automatically controlled multifunctional superfine pulverizer |
| CN102689895A (en) * | 2010-12-30 | 2012-09-26 | 王宏晓 | Preparation method and application of high-purity high-fineness graphite powder |
| CN102689895B (en) * | 2010-12-30 | 2014-07-09 | 王宏晓 | Preparation method and application of high-purity high-fineness graphite powder |
| CN102390829A (en) * | 2011-07-26 | 2012-03-28 | 大同新成新材料股份有限公司 | Graphite powder used in furnace end, Acheson furnace end structure and maintenance method thereof |
| CN102390829B (en) * | 2011-07-26 | 2013-03-27 | 大同新成新材料股份有限公司 | Graphite powder used in furnace end, Acheson furnace end structure and maintenance method thereof |
| CN103964420A (en) * | 2011-09-27 | 2014-08-06 | 王宏晓 | Preparation method of high-purity high-fineness graphite powder |
| CN105985834A (en) * | 2015-02-04 | 2016-10-05 | 青岛路比特化学有限公司 | Energy-saving and anti-friction graphite lubricating oil and preparation method therefor |
| CN105985838A (en) * | 2015-02-04 | 2016-10-05 | 青岛路比特化学有限公司 | Graphite lubricating oil friction-reducing additive and preparation method thereof |
| CN105060281A (en) * | 2015-07-22 | 2015-11-18 | 深圳市贝特瑞新能源材料股份有限公司 | Nano-graphite slurry preparation method |
| CN105060281B (en) * | 2015-07-22 | 2018-10-30 | 深圳市贝特瑞新能源材料股份有限公司 | A kind of preparation method of nano-graphite slurry |
| CN106554012A (en) * | 2016-10-11 | 2017-04-05 | 江苏华力索菲新材料有限公司 | The preparation method of modified superfine Graphene |
| CN106554012B (en) * | 2016-10-11 | 2018-09-28 | 江苏华力索菲新材料有限公司 | The preparation method of modified superfine graphene |
| CN107500285A (en) * | 2017-09-30 | 2017-12-22 | 湖南国盛石墨科技有限公司 | The preparation method of superfine graphite |
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