CN102807207A - Method for producing high-density and high-strength graphite product with fine structure - Google Patents
Method for producing high-density and high-strength graphite product with fine structure Download PDFInfo
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- CN102807207A CN102807207A CN201210261399XA CN201210261399A CN102807207A CN 102807207 A CN102807207 A CN 102807207A CN 201210261399X A CN201210261399X A CN 201210261399XA CN 201210261399 A CN201210261399 A CN 201210261399A CN 102807207 A CN102807207 A CN 102807207A
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Abstract
The invention discloses a method for producing a high-density and high-strength graphite product with a fine structure. The method comprises the following steps of: grinding raw materials for preparing a graphite product into powder with the particle size of less than or equal to 5mu m; uniformly mixing the powder, a solvent, an adhesive, an anti-settling agent and a graphitizer; drying and forming in sequence to obtain a cylindrical or cubic formed product; and roasting the formed product, impregnating, graphitizing, and machining to obtain a finished graphite product. The raw materials are ground into the powder with the particle size of less than or equal to 5mu m, so that the problem that the graphite product produced by the prior art has anisotropy is solved; and meanwhile, components for preparing the graphite product are fully subjected to wet mixing, so that the problems of an internal crack and the like due to elastic deformation caused by temperature change are solved, various properties of the graphite product are improved, and the production cost of the graphite product is reduced.
Description
Technical field
The present invention relates to a kind of working method of graphite product, relate in particular to a kind of high-density of finestructure, the working method of high strength graphite goods.
Background technology
Graphite product is to adopt refinery coke etc. to be raw material, and coal-tar pitch etc. be caking agent, through broken, batching, mix pinch, the electro-conductive material of a kind of fire-resistant oxidation resistant of series of process manufacturings such as moulding, sintering, dipping, greying, mechanical workout.Be widely used in different field such as metallurgy, chemical industry, space flight, electronics, machinery, building materials, nuclear energy, as do bearing, the wear ring of wear-resisting usefulness; Electrospark machining is used electrode with electrode, electrochemical machining; Mold is used in continuous casting; Semiconductor production is with well heater, crucible, furnace lining; Sintering mold and aerospace flight vehicle jet vane and mover protective sleeve etc.
The raw materials such as refinery coke that present domestic production graphite product such as Graphite Electrodes etc. adopt, its grain diameter is greater than 76 μ m, and employing mixes mode and the lower melting point pitch caking agent and the mixing of other added ingredientss of pinching.Because the particle diameter of primary particle is big, viscosity is big, causes the isotropy of graphite product relatively poor, finally causes the difference of graphite product performance.In addition because mixed pinching belongs to dried mix a kind of; And caking agent has certain viscosity; Mix the mode of pinching and very easily cause the inhomogeneous of material component distribution, and, cause graphite product to produce implosion easily in process of production owing to mix the contraction ratio of uneven various components under temperature variations, the difference of contraction speed; Finally cause scrapping of graphite product, improved the production cost of graphite product greatly.
Summary of the invention
Based on above-mentioned technical problem, the present invention provides a kind of high-density of finestructure, the working method of high strength graphite goods.
Its technical solution is:
The working method of a kind of high-density of finestructure, high strength graphite goods; It may further comprise the steps: the starting material that will produce graphite product are crushed to granularity≤5um; Then itself and solvent and caking agent are mixed, make the graphite product finished product through drying, moulding, roasting, dipping, greying and mechanical workout successively again.
Further, earlier solvent and caking agent are mixed, in the liquid that mixes, add the starting material after pulverizing again and continue mixing.
Further, the starting material after the pulverizing carried out pattern to it before mixing with solvent and caking agent handles, and with the raw-material isotropy of further assurance, increases raw-material tap density and particle size distribution simultaneously.
Above-mentioned optimal seeking of raw and processed materials refinery coke or carbon black, volatile content in the starting material＜15%, sulphur content＜0.4%.
Above-mentioned solvent preferably water, alcohol, terepthaloyl moietie or toluene; The preferred pitch of above-mentioned caking agent, tar or resin, further preferred high temperature modified pitch.
Further, solvent and raw-material weight ratio are 99: 1～1: 99, and caking agent accounts for 0.1%～100% of raw-material weight.
Further, when starting material after the pulverizing and solvent and caking agent are mixed into slurry, in slurry, add anti-sedimentation agent and/or graphitizer.
Above-mentioned anti-sedimentation agent preferably carboxymethyl cellulose sodium or gather oxyethylene; The above-mentioned preferred titanium of graphitizer, iron, vanadium and oxide compound, silicon oxide or the aluminum oxide stated.
Further, preferred anti-sedimentation agent and graphitizer add in the slurry in the lump, and the anti-sedimentation agent that is added accounts for 0.1%～10% of raw-material weight, and the graphitizer that is added accounts for 0.1%～10% of raw-material weight.
Further, roasting and impregnation steps can repeat according to end-use or other requirements, and general preferred roasting and impregnation steps repeat 0～20 time.
Useful technique effect of the present invention is:
The present invention is through being crushed to granularity≤5um with starting material; Solve the graphite product that adopts prior art to produce and had anisotropic problem; Simultaneously through the mixing method of wet mixing, each component that will be used to prepare graphite product is mixed fully, has avoided the problems such as implosion that cause owing to elastic deformation that temperature variation causes; Improve each item performance of graphite product, reduced the production cost of graphite product.
Description of drawings
Fig. 1 is the SEM figure of the graphite product that makes in the embodiment of the invention 1;
Fig. 2 is the SEM figure of the graphite product that makes in the embodiment of the invention 2.
Embodiment
Below in conjunction with specific embodiment the present invention is further described.
Embodiment 1
Take by weighing the 100kg refinery coke, volatile content in the refinery coke＜15%, sulphur content＜0.4% utilizes pulverizing mill that it is carried out abrasive dust, controls final granularity≤5um.Take by weighing 200kg alcohol and 10kg hard pitch, hard pitch is added in the alcohol, stir, add the good refinery coke of mill then, stir, process mixed slurry while grinding.Mixed slurry is carried out spraying drying; Guarantee that size range is controlled at 0.1～80um; Pattern is spherical, and the gum cover of the Φ 600*1500 that packs into then utilizes isostatic pressing machine to carry out isostatic pressing; Process moulded products, it is the cubes of 0.1～800mm that moulded products can be the right cylinder or the length of side that diameter is 0.1～800mm.With the moulded products roasting kiln roasting of packing into, maturing temperature is 800 degrees centigrade, and roasting time is 300 hours, adopts softening temperature to flood less than 70 soft pitch after roasting is accomplished again.And then carry out roasting and dipping, and carry out altogether three times so repeatedly, guarantee volume density＞1.5 of graphite product.Graphite product after again roasting and dipping being accomplished carries out greying at 2900 ℃, and graphitization time is 10 days.Roasting and graphitizing process all carry out under oxygen free condition.After greying is accomplished,, carry out corresponding mechanical workout again and promptly make the graphite product finished product, like Graphite Electrodes, sintering mold etc. with the furnace temperature cooling.The SEM figure of graphite product finished product is as shown in Figure 1, and its performance index are as shown in table 1 below.
Table 1
| Inspection parameter | Purity | The primary particle degree | Volume density | Ultimate compression strength | Folding strength |
| Unit | % | μm | g/cm 3 | Mpa | Mpa |
| The Graphite Electrodes finished product | 99 | 3 | 1.75 | 78 | 37 |
Embodiment 2
Take by weighing the 100kg refinery coke, utilize pulverizing mill that it is carried out abrasive dust, control final granularity≤5um.Then the refinery coke that grinds is carried out pattern and handle, guarantee the isotropy of refinery coke, increase the tap density and the particle size distribution of refinery coke simultaneously, make its tap density be controlled at 0.5～1.7g/cm
3, particle size distribution is controlled at 0.1～30um.Take by weighing 150kg alcohol and 15kg hard pitch, hard pitch is added in the alcohol, stir; Add the refinery coke after pattern is handled then; Stir while grinding, in slurry, add 10Kg Xylo-Mucine and 10Kg silicon oxide simultaneously, process mixed slurry.Mixed slurry is carried out spraying drying; Guarantee that size range is controlled at 0.1～80um; Pattern is spherical, and the gum cover of the Φ 600*1500 that packs into then utilizes isostatic pressing machine to carry out isostatic pressing; Process moulded products, it is the cubes of 0.1～800mm that moulded products can be the right cylinder or the length of side that diameter is 0.1～800mm.With the moulded products roasting kiln roasting of packing into, maturing temperature is 800 degrees centigrade, and roasting time is 300 hours, adopts softening temperature to flood less than 70 soft pitch after roasting is accomplished again.And then carry out roasting and dipping, and carry out altogether three times so repeatedly, guarantee volume density＞1.5 of graphite product.Graphite product after again roasting and dipping being accomplished carries out greying at 2900 ℃, and graphitization time is 10 days.Roasting and graphitizing process all carry out under oxygen free condition.After greying is accomplished,, carry out corresponding mechanical workout again and promptly make the graphite product finished product, like Graphite Electrodes etc. with the furnace temperature cooling.The SEM figure of graphite product finished product is as shown in Figure 2, and its performance index are as shown in table 2 below.
Table 2
| Inspection parameter | Purity | The primary particle degree | Volume density | Ultimate compression strength | Folding strength |
| Unit | % | μm | g/cm 3 | Mpa | Mpa |
| The Graphite Electrodes finished product | 99.5 | 2 | 1.8 | 76 | 40 |
Embodiment 3
Take by weighing the 100kg refinery coke, utilize pulverizing mill that it is carried out abrasive dust, control final granularity≤5um.Then the refinery coke that grinds is carried out pattern and handle, guarantee the isotropy of refinery coke, increase the tap density and the particle size distribution of refinery coke simultaneously, make its tap density be controlled at 0.5～1.7g/cm
3, particle size distribution is controlled at 0.1～30um.Take by weighing 250kg alcohol and 20kg hard pitch, hard pitch is added in the alcohol, stir; Add the refinery coke after pattern is handled then; Stir while grinding, in slurry, add 10kg simultaneously and gather oxyethylene and 5kg aluminum oxide, process mixed slurry.Mixed slurry is carried out spraying drying, guarantee that size range is controlled at 0.1～80um, pattern is spherical, utilizes moulding press to be pressed then.With the moulded products roasting kiln roasting of packing into, maturing temperature is 800 degrees centigrade, and roasting time is 300 hours, adopts softening temperature to flood less than 70 soft pitch after roasting is accomplished again.And then carry out roasting and dipping, and carry out altogether four times so repeatedly, guarantee volume density＞1.5 of graphite product.Graphite product after again roasting and dipping being accomplished carries out greying at 2900 ℃, and graphitization time is 10 days.Roasting and graphitizing process all carry out under protection of inert gas.After greying is accomplished,, carry out corresponding mechanical workout again and promptly make the graphite product finished product with the furnace temperature cooling.Graphite product end properties index is as shown in table 3 below.
Table 3
| Inspection parameter | Purity | The primary particle degree | Volume density | Ultimate compression strength | Folding strength |
| Unit | % | μm | g/cm 3 | Mpa | Mpa |
| The Graphite Electrodes finished product | 99.6 | 3 | 1.85 | 78 | 38 |
Embodiment 4
Take by weighing the 100kg carbon black, volatile content in the carbon black＜15%, sulphur content＜0.4% utilizes pulverizing mill that it is carried out abrasive dust, controls final granularity≤5um.Then the refinery coke that grinds is carried out pattern and handle, guarantee the isotropy of refinery coke, increase the tap density and the particle size distribution of refinery coke simultaneously, make its tap density be controlled at 0.5～1.7g/cm
3, particle size distribution is controlled at 0.1～30um.Take by weighing 200kg alcohol and 20kg hard pitch, hard pitch is added in the alcohol, stir, add the refinery coke after pattern is handled then, stir, in slurry, add the 10kg Xylo-Mucine simultaneously, process mixed slurry while grinding.Mixed slurry is carried out spraying drying, guarantee that size range is controlled at 0.1～80um, pattern is spherical, utilizes isostatic pressing machine to be pressed then.With the moulded products roasting kiln roasting of packing into, maturing temperature is 800 degrees centigrade, and roasting time is 300 hours, adopts softening temperature to flood less than 70 soft pitch after roasting is accomplished again.And then carry out roasting and dipping, and carry out altogether three times so repeatedly, guarantee volume density＞1.5 of graphite product.Graphite product after again roasting and dipping being accomplished carries out greying at 2900 ℃, and graphitization time is 10 days.Roasting and graphitizing process all carry out under protection of inert gas.After greying is accomplished,, carry out corresponding mechanical workout again and promptly make the graphite product finished product with the furnace temperature cooling.Graphite product end properties index is as shown in table 4 below.
Table 4
| Inspection parameter | Purity | The primary particle degree | Volume density | Ultimate compression strength | Folding strength |
| Unit | % | μm | g/cm 3 | Mpa | Mpa |
| The Graphite Electrodes finished product | 99.7 | 3 | 1.85 | 80 | 40 |
Claims (10)
1. the working method of the high-density of a finestructure, high strength graphite goods is characterised in that it may further comprise the steps:
The starting material of producing graphite product are crushed to granularity≤5um, then itself and solvent and caking agent are mixed, make the graphite product finished product through drying, moulding, roasting, dipping, greying and mechanical workout successively again.
2. the working method of the high-density of a kind of finestructure according to claim 1, high strength graphite goods is characterized in that: earlier solvent and caking agent are mixed, in the liquid that mixes, add the starting material after pulverizing again and continue mixing.
3. the working method of the high-density of a kind of finestructure according to claim 1, high strength graphite goods is characterized in that: the starting material after the pulverizing carried out pattern to it before mixing with solvent and caking agent handles.
4. the working method of the high-density of a kind of finestructure according to claim 1, high strength graphite goods, it is characterized in that: said starting material are refinery coke or carbon black, volatile content in the starting material＜15%, sulphur content＜0.4%.
5. the working method of the high-density of a kind of finestructure according to claim 1, high strength graphite goods, it is characterized in that: said solvent is water, alcohol, terepthaloyl moietie or toluene; Said caking agent is pitch, tar or resin.
6. the working method of the high-density of a kind of finestructure according to claim 1, high strength graphite goods, it is characterized in that: solvent and raw-material weight ratio are 99: 1～1: 99, and caking agent accounts for 0.1%～100% of raw-material weight.
7. the working method of the high-density of a kind of finestructure according to claim 1, high strength graphite goods is characterized in that: when starting material after the pulverizing and solvent and caking agent are mixed into slurry, in slurry, add anti-sedimentation agent and/or graphitizer.
8. the working method of the high-density of a kind of finestructure according to claim 7, high strength graphite goods, it is characterized in that: said anti-sedimentation agent is Xylo-Mucine or gathers oxyethylene; Said graphitizer is titanium, iron, vanadium and oxide compound thereof, silicon oxide or aluminum oxide.
9. the working method of the high-density of a kind of finestructure according to claim 7, high strength graphite goods; It is characterized in that: the anti-sedimentation agent that is added accounts for 0.1%～10% of raw-material weight, and the graphitizer that is added accounts for 0.1%～10% of raw-material weight.
10. the working method of the high-density of a kind of finestructure according to claim 1, high strength graphite goods, it is characterized in that: roasting and impregnation steps repeat 0～20 time.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103553664A (en) * | 2013-10-23 | 2014-02-05 | 上海科盛陶瓷有限公司 | Manufacturing method of composite ceramic graphite crucible special for tin melting |
| CN105271207A (en) * | 2015-11-24 | 2016-01-27 | 巴中意科碳素有限公司 | Preparation process of isostatic pressing isotropic graphite |
| CN105289646A (en) * | 2015-11-15 | 2016-02-03 | 江苏丹诚环境工程有限公司 | Method for producing electrical accelerant catalyst of special type carbon material |
| CN107032792A (en) * | 2017-05-16 | 2017-08-11 | 江西宁新新材料股份有限公司 | A kind of high-strength high-density graphite material and preparation method thereof |
| CN108529612A (en) * | 2017-12-19 | 2018-09-14 | 大同新成新材料股份有限公司 | A kind of isostatic pressing formed graphite product and its production method |
| CN110668820A (en) * | 2019-11-18 | 2020-01-10 | 青岛瀚博电子科技有限公司 | Preparation method of high-performance carbon graphite product with superfine structure |
| CN110683845A (en) * | 2019-11-18 | 2020-01-14 | 青岛瀚博电子科技有限公司 | Preparation method of carbon graphite product with superfine structure |
| CN116003131A (en) * | 2022-08-31 | 2023-04-25 | 青岛瀚博电子科技有限公司 | Preparation method of high-strength carbon graphite product |
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Cited By (12)
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| CN103553664A (en) * | 2013-10-23 | 2014-02-05 | 上海科盛陶瓷有限公司 | Manufacturing method of composite ceramic graphite crucible special for tin melting |
| CN105289646A (en) * | 2015-11-15 | 2016-02-03 | 江苏丹诚环境工程有限公司 | Method for producing electrical accelerant catalyst of special type carbon material |
| CN105289646B (en) * | 2015-11-15 | 2018-01-05 | 江苏丹诚环境工程有限公司 | A kind of production method of the electric catalyst catalyst of extraordinary carbon materials |
| CN105271207A (en) * | 2015-11-24 | 2016-01-27 | 巴中意科碳素有限公司 | Preparation process of isostatic pressing isotropic graphite |
| CN107032792A (en) * | 2017-05-16 | 2017-08-11 | 江西宁新新材料股份有限公司 | A kind of high-strength high-density graphite material and preparation method thereof |
| CN107032792B (en) * | 2017-05-16 | 2020-12-11 | 江西宁新新材料股份有限公司 | High-strength high-density graphite material and preparation method thereof |
| CN108529612A (en) * | 2017-12-19 | 2018-09-14 | 大同新成新材料股份有限公司 | A kind of isostatic pressing formed graphite product and its production method |
| CN108529612B (en) * | 2017-12-19 | 2019-10-25 | 大同新成新材料股份有限公司 | A kind of isostatic pressing formed graphite product and its production method |
| CN110668820A (en) * | 2019-11-18 | 2020-01-10 | 青岛瀚博电子科技有限公司 | Preparation method of high-performance carbon graphite product with superfine structure |
| CN110683845A (en) * | 2019-11-18 | 2020-01-14 | 青岛瀚博电子科技有限公司 | Preparation method of carbon graphite product with superfine structure |
| CN116003131A (en) * | 2022-08-31 | 2023-04-25 | 青岛瀚博电子科技有限公司 | Preparation method of high-strength carbon graphite product |
| CN116003131B (en) * | 2022-08-31 | 2024-01-26 | 青岛瀚博电子科技有限公司 | Preparation method of high-strength carbon graphite product |
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Application publication date: 20121205 |