CN1031198C - Producing process for micronized graphite - Google Patents
Producing process for micronized graphite Download PDFInfo
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- CN1031198C CN1031198C CN 92106580 CN92106580A CN1031198C CN 1031198 C CN1031198 C CN 1031198C CN 92106580 CN92106580 CN 92106580 CN 92106580 A CN92106580 A CN 92106580A CN 1031198 C CN1031198 C CN 1031198C
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Abstract
The present invention relates to a method for producing micronized graphite, which is composed of the working procedures of dry pulverization, the wet pulverization of a vibration ball mill, dilution, classification, concentration, purification, washing, collection, etc. Allergy acid salt or other dispersing agents are added in the working procedure of wet pulverization, water is used for preparation, and the vibration milling lasts for 20 to 140 hours. A flocculating agent is added to micronized liquid in the working procedure of concentration. Micronized graphite slurry is washed by water in the working procedure of washing. Filtering cake whose concentration is from 25 to 40 can be collected in the working procedure of collection. Qualified micronized graphite whose particle size is one micrometer can be produced. The present invention has high production efficiency and can be widely applied to the production of the micronized graphite.
Description
The present invention relates to producing process for micronized graphite, be used to make the producing process for micronized graphite of combustion engine energy-saving wear reducing additive, thin wire drawing aquadag and other solid lubricant more precisely.
Characteristics such as that crystalline flake graphite has is high temperature resistant, nontoxic, oilness is good are one of excellent materials of selecting for use of solid lubrication.In recent years, the solid lubricant development was very fast, and the miniaturization of graphite granule is had higher requirement.For example, the energy-saving friction-reducing additive used of lubricating oil requires the granularity of graphite granule less than 1 micron.Thin wire drawing aquadag also requires the granularity of graphite granule less than 1 micron.At present, domestic not production granularity still is less than the production method of 1 micron fine-grain graphite.Though external existing this technology of producing process for micronized graphite, its technical process complexity, process cycle are long, the cost costliness, and facility investment is big.The vibration of human vibromill through hundreds of hour arranged, and granularity only reaches about 80% less than 1 micron graphite granule.
Purpose of the present invention is to overcome above-mentioned shortcoming and defect, provides a kind of energy production granularity less than 1 micron, and technical process is fairly simple, process cycle is short, production efficiency has raising, production cost that the producing process for micronized graphite of reduction is arranged.
In order to achieve the above object, producing process for micronized graphite of the present invention is made of dry grinding operation and the broken operation of vibromill wet-milling.The broken operation of vibromill wet-milling is that the granularity that will obtain through the dry grinding operation is not more than 3 microns graphite to add mass ratio be 0.5～5% dispersion agent, and water is formulated into 10～30% concentration again, and vibration is 20～140 hours in vibromill.
Crystalline flake graphite has certain toughness, and comminution ratio is difficulty, and micronizing is difficulty more.For producing granularity less than 1 micron fine-grain graphite, the dry grinding operation that the present invention adopts is that first handle＜160 micron high-carbon graphite is crushed to 6 microns through high speed disintegrator, through micronizer mill graphite granule is crushed to below 3 microns again, and then broken through the vibromill wet-milling.The dispersion agent of adding 0.5～5% was formulated into the graphite water 10～30% concentration again when wet-milling was broken.Dispersion agent can be avoided the graphite granule conglomerate, and graphite grain is disperseed, and is beneficial to pulverize.Dispersion agent can be a kind of in irritated hydrochlorate, gentle acid, Mierocrystalline cellulose, sodium naphthalene sulfonate or the gum arabic, also can be other dispersion agent, and the former effect is better.Its mass ratio is that 0.5 of graphite～5% o'clock effect is best, and efficient height, cost are low.When being mixed with 10～30% concentration with water, graphite granule is convenient to pulverize.Visual dispersion agent of vibration time and concentration increased and decreased in the scope to some extent at 20～140 hours.The grain graininess of vibration was excessive when the time was too short, and effect is no longer obvious during overlong time, and wastes energy.
After the broken operation of vibromill wet-milling, producing process for micronized graphite of the present invention also comprise successively with the graphite liquid water after the vibration towards rare to 0.5～5% concentration towards rare operation, to assign to classification operation in the micropartical liquid to granularity less than 1 micron graphite with centrifugal classifier towards the graphite after rare, the flocculation agent that adds mass ratio 8～12% in micropartical liquid makes graphite be condensed into the enrichment process that the sedimentation of poly-group is removed upper clear supernate simultaneously, add mass ratio 100% technical hydrochloric acid in the fine-grain graphite slurries after concentrating and heat and make dispersion agent, impurity such as iron and flocculation agent dissolved purification process, fine-grain graphite slurries water after purifying is flushed to the washing procedure of PH4～5 and will captures the capture operation of the filter cake that is 20～40% concentration through the fine-grain graphite slurries after the water flushing with the high speed centrifugation catcher.
Towards rare operation is to prepare for the classification operation.
The classification operation can be with the fine-grain graphite centrifugation in micropartical liquid.The graphite granule of volume particle size is then sent to pulverizing again or is used to make other graphite products.
The flocculation agent that adds in the enrichment process can be a kind of in Tai-Ace S 150 or the alum, also can be other kind.The former flocculating result is better.Flocculation agent settles down the graphite conglomerate, and after upper clear supernate was removed, micropartical liquid further was concentrated.
The hydrochloric acid that adds in the purification process is with the dissolving of impurity such as iron, dispersion agent, flocculation agent, and after the flushing of washing procedure water, just available supercentrifuge catcher captures again.Purification process can make the ash content that concentrates micropartical liquid drop to 2～2.5% by 15～20%.
The filter cake that captures 25～40% concentration that capture after the operation is the product fine-grain graphite of present method.Get final product through dilution during use.
The task of producing process for micronized graphite of the present invention comes to this and finishes.
The invention provides the method for a kind of energy production granularity less than 1 micron fine-grain graphite, product granularity meets the requirements, and technical process is fairly simple, process cycle is short, production efficiency is higher, production cost is lower.In the fine-grain graphite of past with hour generation of vibromill vibration hundreds of, granularity only accounting for about 80% below 1 micron, present method can be produced the qualified product of 1 micron of granularity, and production efficiency has improved 0.5～3 times.The solid lubricant frictional coefficient that past makes with air-flow dry grinding method is 0.2～0.25, and the solid lubricant frictional coefficient that present method is produced can reach 0.08～0.1, has improved lubricity greatly, and energy-saving effect is obvious.The present invention can be widely used in the production of fine-grain graphite.
Below in conjunction with embodiment the present invention is done further explanation.
Embodiment 1, a kind of producing process for micronized graphite.It is broken by dry grinding, vibromill wet-milling, towards rare, classification, concentrate, operations such as purification, washing and capture constitute.In the broken operation of wet-milling, the adding mass ratio is 5% the irritated hydrochlorate of dispersion agent, and water is mixed with 30% concentration, vibration 140 hours.In rare operation, water towards rare to 4% concentration.The flocculation agent Tai-Ace S 150 that in micropartical liquid, adds 12% mass ratio in the enrichment process.In the washing procedure, fine-grain graphite slurries water is flushed to pH4.The capture operation can capture the filter cake of concentration 40%.But the qualified fine-grain graphite that present embodiment production granularity is 1 micron, production efficiency improve 0.5 times, can reach 0.1 with the solid lubricant frictional coefficient of its making.Present embodiment can be widely used in the production of fine-grain graphite.
Embodiment 2, a kind of producing process for micronized graphite.It is broken by dry grinding, vibromill wet-milling, towards rare, classification, concentrate, operations such as purification, washing and capture constitute.In the broken operation of wet-milling, the adding mass ratio is 3% the gentle acid of dispersion agent, and water is mixed with 10% concentration, vibration 70 hours.In rare operation, water towards rare to 3% concentration.The flocculation agent alum that in micropartical liquid, adds 10% mass ratio in the enrichment process.In the washing procedure fine-grain graphite slurries water is flushed to pH5.The capture operation can capture the filter cake of concentration 30%.But the qualified fine-grain graphite that present embodiment production granularity is 1 micron, production efficiency improves 1 times.Solid lubricant frictional coefficient with its making can reach 0.08.Also can be used for making thin wire drawing graphite, combustion engine energy-saving wear reducing additive etc.Present embodiment can be widely used in the fine-grain graphite production.
Embodiment 3, a kind of producing process for micronized graphite.It is broken by dry grinding, vibromill wet-milling, towards rare, classification, concentrate, operations such as purification, washing and capture constitute.In the broken operation of wet-milling, the adding mass ratio is 3% dispersion agent Mierocrystalline cellulose, and water is mixed with 10% concentration, vibration 140 hours.In rare operation, water towards rare to 1% concentration.The alum that in micropartical liquid, adds 8% mass ratio in the enrichment process.In the washing procedure, fine-grain graphite slurries water is flushed to pH4.The capture operation can capture the filter cake of concentration 30%.But the qualified fine-grain graphite that present embodiment production granularity is 1 micron, production efficiency improve 3 times, can reach 0.1 with the solid lubricant frictional coefficient of its making.Present embodiment can be widely used in the production of fine-grain graphite.
Embodiment 4, a kind of producing process for micronized graphite.It is broken by dry grinding, vibromill wet-milling, towards rare, classification, concentrate, operations such as purification, washing and capture constitute.In the broken operation of wet-milling, the adding mass ratio is 3% dispersion agent sodium naphthalene sulfonate, and water is mixed with 15% concentration, vibration 20 hours.In rare operation, water towards rare to 5% concentration.The Tai-Ace S 150 that in micropartical liquid, adds 10% mass ratio in the enrichment process.In the washing procedure fine-grain graphite slurries water is flushed to pH5.The capture operation can capture the filter cake of concentration 35%.But the qualified fine-grain graphite that present embodiment production granularity is 1 micron, production efficiency improves 1 times.Solid lubricant frictional coefficient with its making can reach 0.09.Also can be used for making thin wire drawing graphite, combustion engine energy-saving wear reducing additive etc.Present embodiment can be widely used in the fine-grain graphite production.
Embodiment 5, a kind of producing process for micronized graphite.It is broken by dry grinding, vibromill wet-milling, towards rare, classification, concentrate, operations such as purification, washing and capture constitute.In the broken operation of wet-milling, the adding mass ratio is 0.5% dispersion agent gum arabic, and water is mixed with 17% concentration, vibration 80 hours.In rare operation, water towards rare to 0.5% concentration.The alum that in micropartical liquid, adds 12% mass ratio in the enrichment process.In the washing procedure fine-grain graphite slurries water is flushed to pH5.The capture operation can capture the filter cake of concentration 25%.But the qualified fine-grain graphite that present embodiment production granularity is 1 micron, production efficiency improves 1 times.Solid lubricant frictional coefficient with its making can reach 0.08.Also can be used for making thin wire drawing graphite, combustion engine energy-saving antifriction additive etc.Present embodiment can be widely used in the fine-grain graphite production.
Claims (8)
1, a kind of producing process for micronized graphite that is constituted by dry grinding operation and the broken operation of vibromill wet-milling, it is characterized in that the broken operation of said vibromill wet-milling is that the granularity that will obtain through the dry grinding operation is not more than 3 microns graphite to add mass ratio be 0.5～5% dispersion agent, water is formulated into 10～30% concentration again, vibration is 20～140 hours in vibromill, after the broken operation of vibromill wet-milling, also comprise successively the graphite water after the vibration towards rare to the rare operation of dashing of 0.5～5% concentration, to assign to powder level operation in the micropartical liquid to granularity less than 1 micron graphite with centrifugal classifier towards the graphite after rare, adding mass ratio in micropartical liquid is that 8～12% flocculation agent make graphite be condensed into the enrichment process that the sedimentation of poly-group is removed upper clear supernate simultaneously, the technical hydrochloric acid and the heating that add mass ratio 100% in the fine-grain graphite slurries after concentrating make dispersion agent, impurity such as iron and flocculation agent dissolved purification process, fine-grain graphite slurries water after purifying is flushed to the washing procedure of PH4～5 and will captures the capture operation of the filter cake that is 25～40% concentration through the graphite slurries after the water flushing with the high speed centrifugation catcher.
2,, it is characterized in that said dispersion agent is irritated hydrochlorate according to the described producing process for micronized graphite of claim 1.
3,, it is characterized in that said dispersion agent is gentle acid according to the described producing process for micronized graphite of claim 1.
4,, it is characterized in that said dispersion agent is a Mierocrystalline cellulose according to the described producing process for micronized graphite of claim 1.
5,, it is characterized in that said dispersion agent is a sodium naphthalene sulfonate according to the described producing process for micronized graphite of claim 1.
6,, it is characterized in that said dispersion agent is a gum arabic according to the described producing process for micronized graphite of claim 1.
7,, it is characterized in that said flocculation agent is a Tai-Ace S 150 according to the described producing process for micronized graphite of claim 1.
8,, it is characterized in that said flocculation agent is an alum according to the described producing process for micronized graphite of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106580 CN1031198C (en) | 1992-06-24 | 1992-06-24 | Producing process for micronized graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106580 CN1031198C (en) | 1992-06-24 | 1992-06-24 | Producing process for micronized graphite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1080648A CN1080648A (en) | 1994-01-12 |
| CN1031198C true CN1031198C (en) | 1996-03-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 92106580 Expired - Fee Related CN1031198C (en) | 1992-06-24 | 1992-06-24 | Producing process for micronized graphite |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326266C (en) * | 2003-12-26 | 2007-07-11 | 比亚迪股份有限公司 | A negative electrode graphite material for lithium-ion secondary battery and preparation method thereof |
| CN1293149C (en) * | 2004-05-17 | 2007-01-03 | 洛阳市冠奇工贸有限责任公司 | Process for preparing crystal nodulizing graphite |
| US10100266B2 (en) | 2006-01-12 | 2018-10-16 | The Board Of Trustees Of The University Of Arkansas | Dielectric nanolubricant compositions |
| CN101379168A (en) | 2006-01-12 | 2009-03-04 | 阿肯色大学评议会 | Nanoparticle compositions and methods for making and using the same |
| CN102443484B (en) * | 2010-10-10 | 2015-11-25 | 王鸿灏 | Multipurpose processing liquid of water-based nanometer flake graphite |
| US8476206B1 (en) | 2012-07-02 | 2013-07-02 | Ajay P. Malshe | Nanoparticle macro-compositions |
| CN104261398B (en) * | 2014-09-29 | 2017-02-15 | 广东东莞市天润电子材料有限公司 | Raw material for preparing graphene and preparation method thereof |
| CN105316084A (en) * | 2015-11-24 | 2016-02-10 | 苏州盖德精细材料有限公司 | Gear lubricating oil nanometer additives and preparation method thereof |
| CN106517167B (en) * | 2016-10-25 | 2018-05-04 | 成都新柯力化工科技有限公司 | A kind of method and graphene microchip that graphene microchip is prepared by setting rotary screw in vibromill |
| CN107440096A (en) * | 2017-08-08 | 2017-12-08 | 湖北瑞晟生物有限责任公司 | A kind of preparation method of rose powder |
| CN109065884A (en) * | 2018-08-17 | 2018-12-21 | 东莞市凯金新能源科技股份有限公司 | The preparation method and material of acid wash purification resistance material artificial graphite pore-creating negative electrode material |
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