CN104828809A - Processing method for extrusion molded medium size structure graphite material - Google Patents
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Abstract
The invention discloses a processing method for an extrusion molded medium size structure graphite material. The method comprises the steps of: S1. profiling process: preparation of calcined petroleum parched material, kneading, extrusion molding, and cooling; S2. roasting process; S3. dipping process; S4. graphitization process; and S5. machining. By means of reasonable temperature control mode and special roasting process, the method provided by the invention controls the release rate of polycondensation volatile gas, avoids crack, holes and other defects, and ensures stability of the production process. The method also employs a coating means to avoid direct contact of the blank and the filler, prevents thermal deformation of the product, and finally obtains the blank with high volume density and uniform structure. And the graphite product with excellent performance can be obtained.
Description
Technical field
The present invention relates to the working method of thick fine texture graphite material in a kind of extrusion moulding, belong to chemical material field.
Background technology
Middle thickness structure graphite is the graphite of maximum particle size between 0.5 ~ 2.0mm mainly, there is excellent heat-shock resistance, oxidation-resistance, chemical resistance and high-temperature stability, and suitable electroconductibility and uniform structure, the hot environment of various harshness can be adapted to." in extruding thick fine texture graphite material " has excellent heat-shock resistance, oxidation-resistance, chemical resistance and high-temperature stability, and outside suitable electroconductibility and uniform structure, with low cost, with short production cycle, the industries such as photovoltaic, casting, chemical industry, electronics, non-ferrous metal, pyroprocessing, pottery and refractory materials can be widely used in.
External graphite product application starting early, maintains the leading position, defines complete product system in the development and production of middle thickness structure graphite goods, and quality, the performance of product are all better, in competition in the international market, have much advantage.Produce primarily of developed countries such as the U.S., Germany, France, Japan at present, domestic market is to the demand heavy dependence import of this series products.In the mode of production, thickness structure graphite goods during overseas enterprise mainly adopts vibratory compaction mode to produce, and compared with the graphite product of large gauge, then only have the only a few enterprises such as SGL (Xi Geli) can produce in extrusion moulding mode.
At present, the middle thickness structure graphite goods that domestic enterprise produces are vibratory compaction, the granularity of goods substantially be 1mm and more than, the product of 0.8mm granularity because of process for processing difficulty greatly, yield rate is low, and cause its output very low, market has openings is large.In high-end field, what current domestic use was more is import and domestic high purity graphite products, there is the shortcomings such as price is high, the production cycle long, the occupation of capital is large, relation between supply and demand change is frequent.Application number be 200910179699.1 patent discloses coarse-grained graphite material and production technique thereof in a kind of large gauge, at more than 0.8mm, and there is the shortcoming that product resistivity is large, folding strength is low, ultimate compression strength is little in granularity in its product.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the working method of thick fine texture graphite material in a kind of extrusion moulding is provided, the folding strength of thick fine texture graphite material and ultimate compression strength in raising, reduce thermal expansivity, reduce the production difficulty of 0.8mm granularity product, improve yield rate, productivity gain.
The object of the invention is to be achieved through the following technical solutions:
A working method for thick fine texture graphite material in extrusion moulding, it comprises following steps technique:
S1. die mould technique, comprises following sub-step:
S101. the preparation of after-smithing petroleum coke siccative: get following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative, wherein by weight percentage, granularity is the calcined coke grain content of 0.5 ~ 0mm is 58 ~ 62%, and granularity is the calcined coke powder content of 0.075 ~ 0mm is 38 ~ 42%;
S102. kneading: use kneading machine by its kneading at ambient pressure the above-mentioned siccative of 95 ~ 105:25 ~ 29 weight ratio and binding agent, the kneading time is 40 ~ 80min, kneading temperature is 133 ~ 137 DEG C, and add oleic acid as additive when being dry mixed and carrying out 18 ~ 22min, oleic acid can reduce the viscosity of pitch, improve the rheological property of pitch, reduce the resistance to flow of pitch, increase its wetting property to feed particles, simultaneously, due to the reduction of asphalt viscosity, the bonding of storeroom is controlled, and avoids the generation of thickener clustering phenomena;
S103. extrusion moulding, cooling: after kneading terminates by the goods of kneading by extruder for shaping, then cool to normal temperature;
S2. sinter process: the above-mentioned goods being cooled to normal temperature are loaded stoving oven, isolated air, select corresponding Baking profile roasting, Baking profile is as following table:
360 hours roasting heating curves
387 hours Baking profile
Wherein: (1) as roasting Φ 400mm and following specification goods, top temperature 1200 DEG C, remaining time makes isothermal holding;
(2) the whole stove pickled product in roasting 18 Room adopts 360 curves, top temperature 1100 DEG C;
S3. impregnation technology: first by baked article preheating, reinstall high-pressure impregnation tank and vacuumize rear pressurization, the impregnation technology of different size graphite material is as following table:
Warm up time of all size goods, preheating temperature and clamping time
S4. graphitization technique: the goods through dip treating are loaded in graphitizing furnace; under argon shield; with the temperature rise rate of 200 DEG C/h; from room temperature to 1300 DEG C; then be warmed up to 1800 DEG C with the heat-up rate of 25 DEG C/h from 1300 DEG C, temperature reaches 1800 DEG C and is freely warming up to 2800 ~ 3000 DEG C later.Power transmission system is as following table:
All size goods power transmission system
S5. machining: graphited goods get product through machining.
In the kneading process of described die mould technique, binding agent is mid-temperature pitch or middle temperature modified pitch, softening temperature 95 ~ 110 DEG C.
In the kneading process of described die mould technique, the dosage of oleic acid additive is that kneading material per ton adds 1000 ~ 1200mL oleic acid.
The material chambers temp extruding press in operation of described die mould technique is 100 ~ 115 DEG C, nozzle type temperature is 105 ~ 150 DEG C, squeeze time 1 ~ 1.5min, specification is the goods pre-extrusion power of Φ≤350mm is 11 ~ 15Mpa, specification is the goods pre-extrusion power of Φ >=400mm is 7 ~ 11Mpa, vacuumize vacuum tightness more than-0.85Mpa, wherein different size graphite material extrusion speed is as follows:
Tank is no less than 2h cooling time, and total cooling time is no less than 4h.
Treat in described sinter process that roasting product is green compact, adopt the rear shove charge of woven asbesto parcel being soaked with fireproof slurry.Adopt the mode of the high temperature resistant woven asbesto parcel being soaked with fireproof slurry to process green compact, be namely soaked with the high temperature resistant woven asbesto of fireproof slurry at green surface parcel.Its action principle is, the mix asphalt in blank is substantially carbonizing from the process of room temperature to 500 DEG C, and in the process, due to the existence of high-temperature-resistant cloth, stopping composition directly cannot contact goods, can not cause detrimentally affect to the discharge of gas in goods.And reaching 800 DEG C in temperature, after high-temperature-resistant cloth forfeiture effect, goods harden and have stable profile, and no longer include the process that gas concentrates generation and discharge in a large number.
The invention has the beneficial effects as follows:
(1) refinery coke of 0.5mm or pitch coke is less than for raw material with particle diameter, appropriate oleic acid is added at kneading process, reduce the viscosity of pitch, improve the rheological property of pitch, reduce the resistance to flow of pitch, increase its wetting property to feed particles, avoid the generation of thickener clustering phenomena, solve kneading process homogeneity question.
(2) by rational temperature control method and special sinter process, control the release rate of polycondensation volatile gases, avoid the generation of the defect such as crackle, hole, ensure that the stable of production technique.
(3) adopt coated means to avoid blank to contact with the direct of stopping composition, prevent goods temperature distortion.
(4) volume density is high, the blank of even structure to adopt the mode of extrusion moulding to obtain, and by exclusive thermal treatment process, obtains the graphite product of excellent performance.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in further detail, but protection scope of the present invention is not limited to the following stated.
The working method of thick fine texture graphite material in [embodiment 1] a kind of extrusion moulding, it comprises following steps technique:
S1. die mould technique, comprises following sub-step:
S101. the preparation of after-smithing petroleum coke siccative: get following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative, wherein by weight percentage, granularity is the calcined coke grain content of 0.5mm is 58% (mass percentage), and granularity is the calcined coke powder content of 0.075mm is 42%;
S102. kneading: use kneading machine by its kneading at ambient pressure the above-mentioned siccative of 95:25 weight ratio and binding agent, the kneading time is 40min, and kneading temperature is 133 DEG C, and adds oleic acid as additive when being dry mixed and carrying out 18min;
S103. extrusion moulding, cooling: after kneading terminates by the goods of kneading by extruder for shaping, then cool to normal temperature;
S2. sinter process: the above-mentioned goods being cooled to normal temperature are loaded stoving oven, isolated air, roasting, Baking profile is as shown in the table:
360 hours roasting heating curves
S3. impregnation technology: first by baked article preheating, reinstall high-pressure impregnation tank and vacuumize rear pressurization, the impregnation technology of different size graphite material is as following table:
Warm up time of all size goods, preheating temperature and clamping time
S4. graphitization technique: the goods through dip treating are loaded in graphitizing furnace; under argon shield; with the temperature rise rate of 200 DEG C/h; from room temperature to 1300 DEG C; then be warmed up to 1800 DEG C with the heat-up rate of 25 DEG C/h from 1300 DEG C, temperature reaches 1800 DEG C and is freely warming up to 2800 DEG C later.Power transmission system is as following table:
All size goods power transmission system
S5. machining: graphited goods get product through machining.
In the kneading process of described die mould technique, binding agent is mid-temperature pitch or middle temperature modified pitch, softening temperature 95 DEG C.
In the kneading process of described die mould technique, the dosage of oleic acid additive is that kneading material per ton adds 1000mL oleic acid.
The material chambers temp extruding press in operation of described die mould technique is 100 DEG C, nozzle type temperature is 105 DEG C, squeeze time 1min, specification is the goods pre-extrusion power of Φ≤350mm is 11Mpa, specification is the goods pre-extrusion power of Φ >=400mm is 7Mpa, vacuumize vacuum tightness at-0.85Mpa, wherein different size graphite material extrusion speed is as follows:
Tank 2h cooling time, total cooling time 4h.
Treat in described sinter process that roasting product is green compact, adopt the rear shove charge of woven asbesto parcel being soaked with fireproof slurry.
The working method of thick fine texture graphite material in [embodiment 2] a kind of extrusion moulding, it comprises following steps technique:
S1. die mould technique, comprises following sub-step:
S101. the preparation of after-smithing petroleum coke siccative: get following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative, wherein by weight percentage, granularity is the calcined coke grain content of 0.4mm is 60%, and granularity is the calcined coke powder content of 0.065mm is 40%;
S102. kneading: use kneading machine by its kneading at ambient pressure the above-mentioned siccative of 97:27 weight ratio and binding agent, the kneading time is 60min, and kneading temperature is 135 DEG C, and adds oleic acid as additive when being dry mixed and carrying out 20min;
S103. extrusion moulding, cooling: after kneading terminates by the goods of kneading by extruder for shaping, then cool to normal temperature;
S2. sinter process: the above-mentioned goods being cooled to normal temperature are loaded stoving oven, isolated air, roasting, Baking profile is as shown in the table:
387 hours Baking profile
S3. impregnation technology: first by baked article preheating, reinstall high-pressure impregnation tank and vacuumize rear pressurization, the impregnation technology of different size graphite material is as following table:
Warm up time of all size goods, preheating temperature and clamping time
S4. graphitization technique: the goods through dip treating are loaded in graphitizing furnace; under argon shield; with the temperature rise rate of 200 DEG C/h; from room temperature to 1300 DEG C; then be warmed up to 1800 DEG C with the heat-up rate of 25 DEG C/h from 1300 DEG C, temperature reaches 1800 DEG C and is freely warming up to 2900 DEG C later.Power transmission system is as following table:
All size goods power transmission system
S5. machining: graphited goods get product through machining.
In the kneading process of described die mould technique, binding agent is mid-temperature pitch or middle temperature modified pitch, softening temperature 100 DEG C.
In the kneading process of described die mould technique, the dosage of oleic acid additive is that kneading material per ton adds 1100mL oleic acid.
The material chambers temp extruding press in operation of described die mould technique is 110 DEG C, nozzle type temperature is 135 DEG C, squeeze time 1.25min, specification is the goods pre-extrusion power of Φ≤350mm is 13Mpa, specification is the goods pre-extrusion power of Φ >=400mm is 9Mpa, vacuumize vacuum tightness at-0.9Mpa, wherein different size graphite material extrusion speed is as follows:
Tank 3h cooling time, total cooling time 5h.
Treat in described sinter process that roasting product is green compact, adopt the rear shove charge of woven asbesto parcel being soaked with fireproof slurry.
The working method of thick fine texture graphite material in [embodiment 3] a kind of extrusion moulding, it comprises following steps technique:
S1. die mould technique, comprises following sub-step:
S101. the preparation of after-smithing petroleum coke siccative: get following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative, wherein by weight percentage, granularity is the calcined coke grain content of 0.3mm is 62%, and granularity is the calcined coke powder content of 0.045mm is 38%;
S102. kneading: use kneading machine by its kneading at ambient pressure the above-mentioned siccative of 105:29 weight ratio and binding agent, the kneading time is 80min, and kneading temperature is 137 DEG C, and adds oleic acid as additive when being dry mixed and carrying out 22min;
S103. extrusion moulding, cooling: after kneading terminates by the goods of kneading by extruder for shaping, then cool to normal temperature;
S2. sinter process: the above-mentioned goods being cooled to normal temperature are loaded stoving oven, isolated air, roasting, Baking profile is as shown in the table:
360 hours roasting heating curves
S3. impregnation technology: first by baked article preheating, reinstall high-pressure impregnation tank and vacuumize rear pressurization, the impregnation technology of different size graphite material is as following table:
Warm up time of all size goods, preheating temperature and clamping time
S4. graphitization technique: the goods through dip treating are loaded in graphitizing furnace; under argon shield; with the temperature rise rate of 200 DEG C/h; from room temperature to 1300 DEG C; then be warmed up to 1800 DEG C with the heat-up rate of 25 DEG C/h from 1300 DEG C, temperature reaches 1800 DEG C and is freely warming up to 3000 DEG C later.Power transmission system is as following table:
All size goods power transmission system
S5. machining: graphited goods get product through machining.
In the kneading process of described die mould technique, binding agent is mid-temperature pitch or middle temperature modified pitch, softening temperature 110 DEG C.
In the kneading process of described die mould technique, the dosage of oleic acid additive is that kneading material per ton adds 1200mL oleic acid.
The material chambers temp extruding press in operation of described die mould technique is 115 DEG C, nozzle type temperature is 150 DEG C, squeeze time 1.5min, specification is the goods pre-extrusion power of Φ≤350mm is 15Mpa, specification is the goods pre-extrusion power of Φ >=400mm is 11Mpa, vacuumize vacuum tightness at-1.0Mpa, wherein different size graphite material extrusion speed is as follows:
Tank 4h cooling time, total cooling time 6h.
Treat in described sinter process that roasting product is green compact, adopt the rear shove charge of woven asbesto parcel being soaked with fireproof slurry.
Claims (8)
1. the working method of thick fine texture graphite material in extrusion moulding, it is characterized in that, it comprises following steps:
S1. die mould technique, comprises following sub-step:
S101. the preparation of after-smithing petroleum coke siccative: get following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative, wherein by weight percentage, granularity is the calcined coke grain content of 0.5 ~ 0mm is 58 ~ 62%, and granularity is the calcined coke powder content of 0.075 ~ 0mm is 38 ~ 42%;
S102. kneading: use kneading machine by its kneading at ambient pressure the above-mentioned siccative of 95 ~ 105:25 ~ 29 weight ratio and binding agent, the kneading time is 40 ~ 80min, and kneading temperature is 133 ~ 137 DEG C, and adds oleic acid as additive when being dry mixed and carrying out 18 ~ 22min;
S103. extrusion moulding, cooling: after kneading terminates by the goods of kneading by electrode extruder extrusion moulding, be then cooled to normal temperature;
S2. sinter process: the above-mentioned goods being cooled to normal temperature are loaded stoving oven, under the condition of isolated air, selects corresponding Baking profile to carry out roasting;
S3. impregnation technology: first by baked article preheating, reinstalls high-pressure impregnation tank and vacuumizes rear impregnating by pressure;
S4. graphitization technique: the goods through dip treating are loaded in graphitizing furnace, under argon shield, carries out greying;
S5. machining: graphited goods get product through machining.
2. the working method of thick fine texture graphite material in a kind of extrusion moulding according to claim 1, it is characterized in that, in the kneading process of described die mould technique, binding agent is mid-temperature pitch or middle temperature modified pitch, softening temperature 95 ~ 110 DEG C.
3. the working method of thick fine texture graphite material in a kind of extrusion moulding according to claim 1, is characterized in that, in the kneading process of described die mould technique, the dosage of oleic acid additive is that kneading material per ton adds 1000 ~ 1200mL oleic acid.
4. the working method of thick fine texture graphite material in a kind of extrusion moulding according to claim 1, it is characterized in that, in the extrusion moulding operation of described die mould technique, the material chambers temp of press is 100 ~ 115 DEG C, nozzle type temperature is 105 ~ 150 DEG C, squeeze time 1 ~ 1.5min, specification is the goods pre-extrusion power of Φ≤350mm is 11 ~ 15Mpa, specification is the goods pre-extrusion power of Φ >=400mm is 7 ~ 11Mpa, vacuumize vacuum tightness more than-0.85Mpa, products of different specifications extrusion speed is different, tank is no less than 2h cooling time, and total cooling time is no less than 4h.
5. the working method of thick fine texture graphite material in a kind of extrusion moulding according to claim 1, it is characterized in that, Baking profile 360 hours roasting heating curves of described sinter process are as follows:
(1) temperature range 130 ~ 350 DEG C, time length 44h, heat-up rate 5.0 DEG C/h,
(2) temperature range 350 ~ 400 DEG C, time length 25h, heat-up rate 2.0 DEG C/h,
(3) temperature range 400 ~ 500 DEG C, time length 88h, heat-up rate 1.14 DEG C/h,
(4) temperature range 500 ~ 600 DEG C, time length 78h, heat-up rate 1.28 DEG C/h,
(5) temperature range 600 ~ 700 DEG C, time length 35h, heat-up rate 2.9 DEG C/h,
(6) temperature range 700 ~ 800 DEG C, time length 18h, heat-up rate 5.5 DEG C/h,
(7) temperature range 800 ~ 1000 DEG C, time length 25h, heat-up rate 8.0 DEG C/h,
(8) temperature range 1000 ~ 1250 DEG C, time length 25h, heat-up rate 10 DEG C/h,
(9) 1250 DEG C of insulations, time length 22h,
(10) temperature range 1250 ~ 800 DEG C, time length 15h, heat-up rate-30 DEG C/h.
6. the working method of thick fine texture graphite material in a kind of extrusion moulding according to claim 1, it is characterized in that, the Baking profile of described sinter process also comprises 387 hours roasting heating curves:
(1) temperature range 130 ~ 350 DEG C, time length 44h, heat-up rate 5.0 DEG C/h,
(2) temperature range 350 ~ 450 DEG C, time length 50h, heat-up rate 2.0 DEG C/h,
(3) temperature range 450 ~ 550 DEG C, time length 100h, heat-up rate 1.0 DEG C/h,
(4) temperature range 550 ~ 650 DEG C, time length 80h, heat-up rate 1.25 DEG C/h,
(5) temperature range 650 ~ 700 DEG C, time length 23h, heat-up rate 2.17 DEG C/h,
(6) temperature range 700 ~ 800 DEG C, time length 20h, heat-up rate 5.0 DEG C/h,
(7) temperature range 800 ~ 1000 DEG C, time length 25h, heat-up rate 8.0 DEG C/h,
(8) temperature range 1000 ~ 1250 DEG C, time length 25h, heat-up rate 10 DEG C/h,
(9) 1250 DEG C of insulations, time length 20h,
(10) temperature range 1250 ~ 800 DEG C, time length 15h, heat-up rate-30 DEG C/h.
7. the working method of thick fine texture graphite material in a kind of extrusion moulding according to claim 1, is characterized in that, treat that roasting product is green compact in described sinter process, adopts shove charge after the woven asbesto parcel being soaked with fireproof slurry.
8. the working method of thick fine texture graphite material in a kind of extrusion moulding according to claim 1, it is characterized in that, described graphitization technique temperature increasing schedule is: with the temperature rise rate of 200 DEG C/h, from room temperature to 1300 DEG C, then be warmed up to 1800 DEG C with the heat-up rate of 25 DEG C/h from 1300 DEG C, temperature reaches 1800 DEG C and is freely warming up to 2800 ~ 3000 DEG C later.
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Cited By (5)
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| CN106699183A (en) * | 2016-12-28 | 2017-05-24 | 浙江佳力风能技术有限公司 | Composite graphite cold iron material, manufacturing method of composite graphite cold iron and composite graphite cold iron |
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| CN108751182A (en) * | 2018-06-04 | 2018-11-06 | 中钢集团新型材料（浙江）有限公司 | One kind roasting roasting technique for isostatic pressing formed graphite one |
| CN112225561A (en) * | 2020-10-29 | 2021-01-15 | 许子隆 | Artificial graphite electrode machining pretreatment method |
| CN116409993A (en) * | 2023-03-08 | 2023-07-11 | 江西宁昱鸿新材料有限公司 | Preparation method of high-strength medium-coarse graphite |
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| CN116409993A (en) * | 2023-03-08 | 2023-07-11 | 江西宁昱鸿新材料有限公司 | Preparation method of high-strength medium-coarse graphite |
| CN116409993B (en) * | 2023-03-08 | 2024-02-09 | 江西宁昱鸿新材料有限公司 | Preparation method of high-strength medium-coarse graphite |
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Application publication date: 20150812 |