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CN106431405A - Preparation method for graphite cylinders - Google Patents

Preparation method for graphite cylinders Download PDF

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Publication number
CN106431405A
CN106431405A CN201610793695.2A CN201610793695A CN106431405A CN 106431405 A CN106431405 A CN 106431405A CN 201610793695 A CN201610793695 A CN 201610793695A CN 106431405 A CN106431405 A CN 106431405A
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China
Prior art keywords
siccative
graphite
preparation
cylinder body
warming
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CN201610793695.2A
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CN106431405B (en
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杜明彦
匡乃刚
徐丽华
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Jixi Care-Well Carbon Products Co Ltd
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Jixi Care-Well Carbon Products Co Ltd
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/522—Graphite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
    • B28B3/02—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form
    • B28B3/022—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form combined with vibrating or jolting
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Abstract

The invention discloses a preparation method for graphite cylinders and relates to preparation methods for the graphite cylinders. The preparation method is used for solving the problems in the existing graphite cylinder preparation processes that materials are wasted, the preparation period is long, the preparation cost is high, the energy consumption of preparation is high, and the stability of prepared graphite cylinders is poor. The preparation method comprises the steps: (1) weighing raw materials: weighing the raw materials: 74% to 78% (by mass) of dry matter and the balance of asphalt; (2) carrying out blank forming: carrying out vibration forming in a mold; (3) roasting graphite cylinder blanks in a roasting furnace; and (4) carrying out graphitization on the graphite cylinder blanks. According to the preparation method, the prepared graphite cylinders are reasonable in material structure design and dependable in quality, roasting time, the raw materials, burned coal, labor hours and binding resin can be saved compared with those of the traditional production processes, and thus the preparation method has the effects of energy saving and environment-friendliness; and by adopting a vibration forming technology, the graphite cylinders are compact in structure, high in thermal stability and good in chemical stability. The preparation method is applicable to the preparation of the graphite cylinders.

Description

A kind of preparation method of graphite cylinder body
Technical field
The present invention relates to a kind of preparation method of graphite cylinder body.
Background technology
China is at national defence, scientific research, PVC chemical industry, gas chemical industry, Coal Chemical Industry, dyestuff, chemical fertilizer, pharmacy, silicon industry, spent acid In the technical processs such as reason, using substantial amounts of graphite inhibition and generation construction equipment, especially as the graphite bulk of chemical industry equipment main element, Domestic consumption reaches 9000 tons about every year, so this product market prospect is very wide.In all kinds chemical industry equipment, a lot Main element is all the graphite product combination of cylindrical shape, such as：The gas-liquid mixed room on absorption tower, lower separator, sulfuric acid dilution device Mixing chamber, Analytic Tower tower body, rectification tower body, hydrogen chloride synthesis furnace body, the burning mixing chamber of three-in-one hydrochloric acid synthetic furnace, true Empty body of heater etc. is cylindrical shape graphite product molectron.
At present, the domestic processing technique to cylindrical shape graphite product molectron is broadly divided into two kinds：One is to adopt full circle Graphite Fructus Anisi Stellati turning is cylindrical shape；Loss rate for raw materials is 17%；Diameter is bigger, will be from long curve roasting in calcining process Burn；Generally 420 hours～560 hours, the minimum multiplex coal 360Kg of product per ton, in graphitization process, power transmission amount is bigger, The graphitization process power consumption product per ton of the solid material of major diameter is 5200 degree～5600 KWhs/ton.
Another kind is to be broken after plate processing using square stock, then coheres, is processed into cylinder, this processing technology, and binding agent selects With the high binding resin of high temperature resistant, corrosion-resistant, intensity, complete from selection, processing, the hexahedro processing of plate, drying, bonding, solidification etc. Whole operation needs 4 day time；It is processed into after tabular with square stock and is processed into cylinder after splicing, processing mode takes graphite material must again Must be resin-bonded with high temperature resistant SHU, one full circle of splicing needs adhering resin 5.3～6kg, and after gluing, spontaneous curing 42 hours, also needs Regular circle processing, processing plate splicing raw material casting yield 60%, take a lot of work, take material, mass intensity is unstable.Thus both the above Selection and processing technique not only waste lot of materials, and it is high to make long in time limit, manufacturing cost, manufactures energy resource consumption big.
Content of the invention
The present invention in order to solve waste of material in existing graphite cylinder body preparation process, manufacturing schedule length, manufacturing cost high, Manufacture that energy resource consumption is big and the problem of the graphite cylinder body stability difference of preparation is it is proposed that a kind of preparation method of graphite cylinder body
The preparation method of graphite cylinder body of the present invention is carried out according to the following steps：
Step one, weigh raw material
It is that 74%～78% siccative and balance of Colophonium weigh raw material by mass percentage；
Described siccative by mass percentage by 60% petroleum coke particles, 20% pitch coke granule, 5%～10% pin Shape Jiao's granule and balance of graphite broken granule composition；
Described Colophonium is medium temperature coal pitch；
When described graphite cylinder body wall thickness is less than 100mm, in the siccative described in step one, the siccative more than 2mm for the particle diameter accounts for Less than the 2% of siccative gross weight, particle diameter is that the siccative of 1～2mm accounts for the 8%～14% of siccative gross weight, and particle diameter is 0.5～1mm Siccative account for the 7%～13% of siccative gross weight, particle diameter be below 0.074mm siccative account for siccative gross weight 54%～ 60%, the siccative of balance of particle diameter 0.075～0.15mm；
When described graphite cylinder body wall thickness is more than 100mm, in the siccative described in step one, the siccative more than 1mm for the particle diameter accounts for Less than the 2% of siccative gross weight, particle diameter is that the siccative of 0.5～1mm accounts for the 10%～16% of siccative gross weight, particle diameter be 0.2～ The siccative of 0.5mm accounts for the 7%～13% of siccative gross weight, and particle diameter is that the siccative of below 0.074mm accounts for the 53% of siccative gross weight ～59%, the siccative of balance of particle diameter 0.075～0.15mm；
In described petroleum coke particles, the mass content of ash is not more than 0.42%, and the mass content of volatile matters is not more than 0.8%, the mass content of sulphur content is not more than 0.8%, and petroleum coke true density is not less than 2.04g/cm2, oil resistivity is not more than 429μΩ·m；In described pitch coke granule, the mass content of ash is not more than 0.5%, and the mass content of volatile matters is not more than 1.2%, the mass content of sulphur content is not more than 0.2%, and pitch coke powder ratio resistance is not more than 350 μ Ω mm2/m；Described graphite In broken granule, the mass content of ash is not more than 0.1%, and the mass content of volatile matters is not more than 0.2%, the mass content of sulphur content It is not more than 0.2%, graphite comminuted powder ratio resistance is not more than 350 μ Ω mm2/m；Described needle coke particles are super premium needle coke Grain, senior needle coke particles or one-level needle coke particles；The coefficient of expansion of described super premium needle coke granule is not more than 2.0 × 10- 6Mm/ DEG C, sulfur weight/mass percentage composition is 0.5%, and true density is 2.12g/cm3, vanadium weight/mass percentage composition is 10ppm, nickel content Weight/mass percentage composition is 30%；The coefficient of expansion of described senior needle coke particles is 2.0 × 10-6Mm/ DEG C～3.0 × 10-6mm/ DEG C, sulfur weight/mass percentage composition is 0.6%, and true density is 2.10g/cm3, vanadium weight/mass percentage composition is 10ppm, nickel content quality Percentage composition is 30%；The coefficient of expansion of described one-level needle coke particles is 3.0 × 10-6Mm/ DEG C～4.0 × 10-6Mm/ DEG C, sulfur Part weight/mass percentage composition is 0.8%, and true density is 2.10g/cm3, vanadium weight/mass percentage composition is 10ppm, nickel content percent mass Content is 30%；
Step 2, blank molding
Siccative and Colophonium mix homogeneously are obtained compound, pours compound in mould under mould vibrations, keep mould Tool vibrations, are 1.12～2kg/cm in pressure2Pressure under compound in mould is densified to the graphite cylinder body base of object height Material；Frequency of vibration during described mould vibrations is 2300～2700 beats/min；
Step 3, graphite cylinder body blank roasting
Graphite cylinder body is placed in roaster and carries out roasting；
When described graphite cylinder body wall thickness is more than 100mm, following step is pressed in the roasting of graphite cylinder body blank described in step 3 Suddenly carry out：
The furnace temperature of roaster is warming up to 130～350 DEG C with the programming rate of 4.4 DEG C/h and is incubated after 50h, then with 1.7 DEG C/programming rate of h is warming up to 350～400 DEG C and is incubated 30h, then be warming up to 400～500 DEG C with the programming rate of 1.1 DEG C/h And be incubated 90h, then it is warming up to 500～600 DEG C with the programming rate of 1.7 DEG C/h and is incubated 60h, then the intensification speed with 3.3 DEG C/h Degree is warming up to 600～700 DEG C and is incubated 30h, then is warming up to 700～800 DEG C with the programming rate of 5.0 DEG C/h and is incubated 20h, then It is warming up to 800～1000 DEG C with the programming rate of 6.7 DEG C/h and is incubated 30h, then be warming up to 1000 with the programming rate of 10 DEG C/h ～1300 DEG C and be incubated 30h, finally it is incubated 20h at 1275～1325 DEG C；
When described graphite cylinder body wall thickness is less than 100mm, following step is pressed in the roasting of graphite cylinder body blank described in step 3 Suddenly carry out：
The furnace temperature of roaster is warming up to 130～350 DEG C with the programming rate of 4.4 DEG C/h and is incubated after 50h, then with 1.7 DEG C/programming rate of h is warming up to 350～400 DEG C and is incubated 30h, then be warming up to 400～500 DEG C with the programming rate of 1.4 DEG C/h And be incubated 70h, then it is warming up to 500～600 DEG C with the programming rate of 2.0 DEG C/h and is incubated 50h, then the intensification speed with 4.0 DEG C/h Degree is warming up to 600～700 DEG C and is incubated 25h, then is warming up to 700～800 DEG C with the programming rate of 5.0 DEG C/h and is incubated 20h, then It is warming up to 800～1000 DEG C with the programming rate of 8 DEG C/h and be incubated 25h, then it is warming up to 1000 with the programming rate of 10 DEG C/h～ 1300 DEG C and be incubated 30h, finally it is incubated 20h at 1275～1325 DEG C；
Step 4, graphite cylinder body blank graphitization
Fill full resistance material into the graphite cylinder body blank after roasting, the insulation material parcel stone being 500～800mm with thickness The upper bottom surface of ink cylinder body blank and bottom surface, wrap up the circumference table of graphite cylinder body blank with the resistance material that thickness is 100～150mm Face, then with thickness be 350～400mm insulation material wrap up resistance material circumferential surface, graphitizing furnace bottom tile 500～ The furnace burdening of 1000mm；Then start graphitization；
Described graphited heating means are：
First graphitization in-furnace temperature was at the uniform velocity warming up to 1650～1750 DEG C in 58～62 hours, then 20～24 At the uniform velocity it is warming up to 2250～2350 DEG C in hour, be finally warming up to 2500 DEG C in 5～6 hours, that is, complete；
Described resistance material is the compound of graphitized coke and green coke, and the mass ratio of the compound of graphitized coke and green coke is 7: 3, resistance material granularity is 10～25mm；Described insulation material is the mixture of metallurgical coke and quartz sand, metallurgical wherein in mixture The mass fraction of coke powder is 65%～75%, and the granularity of insulation material is 0～6mm；Described furnace burdening bottom is the accumulation after compacting Density is 1.039～0.850Kg/m3Quartz sand, top is quartz sand and the metallurgical coke compound after compacting, and top mixes In material, the mass fraction of quartz sand is 30%～40%, and in furnace burdening, the granularity of metallurgical coke is 0～10mm.
The present invention possesses following beneficial effect：
1st, pass through scientific algorithm before present invention preparation, then carry out graphite cylinder body material preparation again, institute is in the process of the present invention The graphite cylinder body reasonable in design of preparation, reliable in quality；Graphite cylinder body outer surface flawless prepared by the inventive method, no Hole, even structure, wall thickness reduction amount is ± 1mm, and the both ends of the surface depth of parallelism 0.15%, perpendicularity franchise ± 0.1% are cracked side between the teeth and fallen rib Length is not more than 30mm, cracks side between the teeth and falls rib depth and is not more than 3mm；Article length can reach 400～1000mm and is certified products；Produce Product bending strength 18MPa, comprcssive strength 24～28MPa, bulk density 1.62～1.68g/cm3, ratio resistance 6.2～7.5 μ Ω mm2/ m, ash is less than 0.5%, and linear expansion coefficient is not more than 2.4 × 10-6Mm/ DEG C (between 100 DEG C～600 DEG C), elastic modelling quantity It is not more than 12Gpa；
2nd, graphite cylinder body is prepared using the inventive method, raw material can save at least 17% than traditional processing technology, and original The method first preparing real core cylinder compare, roasting time can be saved on calcining process 100 hours, save coal-fired 360Kg/ ton, Graphitizing process in product per ton can economize on electricity more than 300 degree, mechanical processing process with splicing circle make production technology compared with, often Part graphite cylinder body can save man-hour 56 hours, saves binding resin 5.3～6Kg/m2, the therefore present invention possesses energy-saving and environmental protection Effect；
3rd, the graphite cylinder body specifications and models that the inventive method can be prepared are complete, using vibration moulding technology, make graphite cylinder body Compact structure, intensity index directivity gap is little, is preferable graphite inhibition and generation construction equipment the selection of material, and the inventive method system The standby non-directional Strength Changes of product longtime running.
4th, the graphite cylinder body heat transfer property of the inventive method preparation is stainless 3～4 times, and heat stability is high, and chemistry is steady Qualitative good；
5th, the graphite cylinder body that the inventive method obtains can be widely used in absorption tower, Analytic Tower, vacuum drying oven, hydrogen chloride synthesis Stove, the main element of tail gas absorber, can heating, cooling different process production process in, its main element have pressure, Decay resistance, so that be employed equipment more energy-saving and environmental protection；
6th, in preparation process of the present invention, vibro-moulding process is a kind of new graphite cylinder body blank moulding process, in high frequency Under the vibration of rate, the blanking in vibration, hot gas can be made to discharge, be always maintained at grinding tool vibrations, base during preparing blank Material inside and outside wall again by frictional force counteracting force so as to surfaces externally and internally fineness and internal density improve, make final products Mechanical strength directional difference is little, so vibro-moulding process is reasonable in design.
Specific embodiment：
Technical solution of the present invention is not limited to act specific embodiment set forth below, also includes between each specific embodiment Arbitrarily reasonable combination.
Specific embodiment one：A kind of preparation method of graphite cylinder body is carried out according to the following steps：
Step one, weigh raw material
It is that 74%～78% siccative and balance of Colophonium weigh raw material by mass percentage；
Described siccative by mass percentage by 60% petroleum coke particles, 20% pitch coke granule, 5%～10% pin Shape Jiao's granule and balance of graphite broken granule composition；
Step 2, blank molding
Siccative and Colophonium mix homogeneously are obtained compound, pours compound in mould under mould vibrations, keep mould Tool vibrations, are 1.12～2kg/cm in pressure2Pressure under compound in mould is densified to the graphite cylinder body base of object height Material；Frequency of vibration during described mould vibrations is 2300～2700 beats/min；
Step 3, graphite cylinder body blank roasting
Graphite cylinder body is placed in roaster and carries out roasting；
Step 4, graphite cylinder body blank graphitization
Fill full resistance material into the graphite cylinder body blank after roasting, the insulation material parcel stone being 500～800mm with thickness The upper bottom surface of ink cylinder body blank and bottom surface, wrap up the circumference table of graphite cylinder body blank with the resistance material that thickness is 100～150mm Face, then with thickness be 350～400mm insulation material wrap up resistance material circumferential surface, graphitizing furnace bottom tile 500～ The furnace burdening of 1000mm；Then start graphitization；
Described graphited heating means are：
First graphitization in-furnace temperature was at the uniform velocity warming up to 1650～1750 DEG C in 58～62 hours, then 20～24 At the uniform velocity it is warming up to 2250～2350 DEG C in hour, be finally warming up to 2500 DEG C in 5～6 hours, that is, complete；
Described resistance material is the compound of graphitized coke and green coke, and the mass ratio of the compound of graphitized coke and green coke is 7: 3, resistance material granularity is 10～25mm；Described insulation material is the mixture of metallurgical coke and quartz sand, metallurgical wherein in mixture The mass fraction of coke powder is 65%～75%, and the granularity of insulation material is 0～6mm；Described furnace burdening bottom is the accumulation after compacting Density is 1.039～0.850Kg/m3Quartz sand, top is quartz sand and the metallurgical coke compound after compacting, and top mixes In material, the mass fraction of quartz sand is 30%～40%, and in furnace burdening, the granularity of metallurgical coke is 0～10mm.
Present embodiment possesses following beneficial effect：
1st, pass through scientific algorithm before present embodiment preparation, then carry out graphite cylinder body material preparation again, so this enforcement The graphite cylinder body reasonable in design of methods preparation, reliable in quality；Outside graphite cylinder body prepared by present embodiment method Surface flawless, no hole, even structure, wall thickness reduction amount is ± 1mm, the both ends of the surface depth of parallelism 0.15%, perpendicularity franchise ± 0.1%, crack side between the teeth and fall rib length and be not more than 30mm, crack side between the teeth and fall rib depth and be not more than 3mm；Article length can reach 400～1000mm And it is certified products；Product bending strength 18MPa, comprcssive strength 24～28MPa, bulk density 1.62～1.68g/cm3, than electricity Resistance 6.2～7.5 μ Ω mm2/ m, ash is less than 0.5%, and linear expansion coefficient is not more than 2.4 × 10-6Mm/ DEG C (at 100 DEG C～600 DEG C Between), elastic modelling quantity is not more than 12Gpa；
2nd, graphite cylinder body is prepared using present embodiment method, raw material can save at least 17% than traditional processing technology, with Original method first preparing real core cylinder compares, and can save roasting time 100 hours on calcining process, saves coal-fired 360Kg/ Ton, graphitizing process in product per ton can economize on electricity more than 300 degree, mechanical processing process with splicing circle making production technology phase Can save 56 hours man-hours, save binding resin 5.3～6Kg/m by every graphite cylinder body for ratio2, therefore present embodiment possesses section Energy, the effect of environmental protection；
3rd, the graphite cylinder body specifications and models that present embodiment method can be prepared are complete, using vibration moulding technology, make graphite Tube structure is fine and close, and intensity index directivity gap is little, is preferable graphite inhibition and generation construction equipment the selection of material, and this embodiment party The non-directional Strength Changes of product longtime running of formula method preparation.
4th, the graphite cylinder body heat transfer property of present embodiment method preparation is stainless 3～4 times, and heat stability is high, changes Learn good stability；
5th, the graphite cylinder body that present embodiment method obtains can be widely used in absorption tower, Analytic Tower, vacuum drying oven, hydrogen chloride Synthetic furnace, the main element of tail gas absorber, can be in heating, the different process production process of cooling, and its main element has Pressure, decay resistance, so that be employed equipment more energy-saving and environmental protection；
6th, in present embodiment preparation process, vibro-moulding process is a kind of new graphite cylinder body blank moulding process, Under high-frequency vibration, the blanking in vibration, hot gas can be made to discharge, be always maintained at grinding tool shake during preparing blank Dynamic, the inside and outside wall of blank again by frictional force counteracting force so as to surfaces externally and internally fineness and internal density improve, make finally to produce The mechanical strength directional difference of product is little, so vibro-moulding process is reasonable in design.
Specific embodiment two：Present embodiment from unlike specific embodiment one：During described in step one, Colophonium is Warm coal tar pitch.Other identical with specific embodiment one.
Specific embodiment three：Present embodiment from unlike specific embodiment one or two：When described graphite tube When body wall thickness is less than 100mm, in the siccative described in step one, the siccative more than 2mm for the particle diameter accounts for less than the 2% of siccative gross weight, grain Footpath is that the siccative of 1～2mm accounts for the 8%～14% of siccative gross weight, and particle diameter is that the siccative of 0.5～1mm accounts for the 7% of siccative gross weight ～13%, particle diameter is that the siccative of below 0.074mm accounts for the 54%～60% of siccative gross weight, balance of particle diameter 0.075～ The siccative of 0.15mm.Other identical with specific embodiment one or two.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：When described stone When black cylinder wall thickness are more than 100mm, in the siccative described in step one particle diameter be more than 1mm siccative account for the 2% of siccative gross weight with Under, particle diameter is that the siccative of 0.5～1mm accounts for the 10%～16% of siccative gross weight, and particle diameter is that the siccative of 0.2～0.5mm accounts for siccative The 7%～13% of gross weight, particle diameter is that the siccative of below 0.074mm accounts for the 53%～59% of siccative gross weight, balance of particle diameter The siccative of 0.075～0.15mm.Other identical one of with specific embodiment one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：When described stone When black cylinder wall thickness are more than 100mm, the roasting of graphite cylinder body blank described in step 3 is carried out according to the following steps：
The furnace temperature of roaster is warming up to 130～350 DEG C with the programming rate of 4.4 DEG C/h and is incubated after 50h, then with 1.7 DEG C/programming rate of h is warming up to 350～400 DEG C and is incubated 30h, then be warming up to 400～500 DEG C with the programming rate of 1.1 DEG C/h And be incubated 90h, then it is warming up to 500～600 DEG C with the programming rate of 1.7 DEG C/h and is incubated 60h, then the intensification speed with 3.3 DEG C/h Degree is warming up to 600～700 DEG C and is incubated 30h, then is warming up to 700～800 DEG C with the programming rate of 5.0 DEG C/h and is incubated 20h, then It is warming up to 800～1000 DEG C with the programming rate of 6.7 DEG C/h and is incubated 30h, then be warming up to 1000 with the programming rate of 10 DEG C/h ～1300 DEG C and be incubated 30h, finally it is incubated 20h at 1275～1325 DEG C.Other identical one of with specific embodiment one to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：When described stone When black cylinder wall thickness are less than 100mm, the roasting of graphite cylinder body blank described in step 3 is carried out according to the following steps：
The furnace temperature of roaster is warming up to 130～350 DEG C with the programming rate of 4.4 DEG C/h and is incubated after 50h, then with 1.7 DEG C/programming rate of h is warming up to 350～400 DEG C and is incubated 30h, then be warming up to 400～500 DEG C with the programming rate of 1.4 DEG C/h And be incubated 70h, then it is warming up to 500～600 DEG C with the programming rate of 2.0 DEG C/h and is incubated 50h, then the intensification speed with 4.0 DEG C/h Degree is warming up to 600～700 DEG C and is incubated 25h, then is warming up to 700～800 DEG C with the programming rate of 5.0 DEG C/h and is incubated 20h, then It is warming up to 800～1000 DEG C with the programming rate of 8 DEG C/h and be incubated 25h, then it is warming up to 1000 with the programming rate of 10 DEG C/h～ 1300 DEG C and be incubated 30h, finally it is incubated 20h at 1275～1325 DEG C.Other identical one of with specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Described in step In petroleum coke particles, the mass content of ash is not more than 0.42%, and the mass content of volatile matters is not more than 0.8%, the matter of sulphur content Amount content is not more than 0.8%, and petroleum coke true density is not less than 2.04g/cm2, oil resistivity no more than 429 μ Ω m.Other Identical with one of specific embodiment one to six.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Described in step In pitch coke granule, the mass content of ash is not more than 0.5%, and the mass content of volatile matters is not more than 1.2%, the quality of sulphur content Content is not more than 0.2%, and pitch coke powder ratio resistance is not more than 350 μ Ω mm2/m.Other and specific embodiment one to seven One of identical.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：Described in step In the broken granule of graphite, the mass content of ash is not more than 0.1%, and the mass content of volatile matters is not more than 0.2%, the quality of sulphur content Content is not more than 0.2%, and graphite comminuted powder ratio resistance is not more than 350 μ Ω mm2/m.Other and specific embodiment one to eight One of identical.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：Described in step Needle coke particles are super premium needle coke granule, senior needle coke particles or one-level needle coke particles；Described super premium needle coke granule The coefficient of expansion be not more than 2.0 × 10-6Mm/ DEG C, sulfur weight/mass percentage composition is 0.5%, and true density is 2.12g/cm3, vanadium matter Amount percentage composition is 10ppm, and nickel content weight/mass percentage composition is 30%；The coefficient of expansion of described senior needle coke particles is 2.0 ×10-6Mm/ DEG C～3.0 × 10-6Mm/ DEG C, sulfur weight/mass percentage composition is 0.6%, and true density is 2.10g/cm3, vanadium quality hundred Content is divided to be 10ppm, nickel content weight/mass percentage composition is 30%；The coefficient of expansion of described one-level needle coke particles is 3.0 × 10- 6Mm/ DEG C～4.0 × 10-6Mm/ DEG C, sulfur weight/mass percentage composition is 0.8%, and true density is 2.10g/cm3, vanadium percent mass contains Measure as 10ppm, nickel content weight/mass percentage composition is 30%.Other identical one of with specific embodiment one to nine.
Verify beneficial effects of the present invention with following examples：
Embodiment 1：
The preparation method of present embodiment graphite cylinder body is carried out according to the following steps：
Step one, weigh raw material
It is that 74%～78% siccative and balance of Colophonium weigh raw material by mass percentage；
Described siccative by mass percentage by 60% petroleum coke particles, 20% pitch coke granule, 10% needle coke Granule and balance of graphite broken granule composition；
Described Colophonium is medium temperature coal pitch；
When described graphite cylinder body wall thickness is for 90mm, in the siccative described in step one particle diameter be more than 2mm siccative account for dry The 2% of material gross weight, particle diameter is that the siccative of 1～2mm accounts for the 11% of siccative gross weight, and particle diameter is that the siccative of 0.5～1mm accounts for siccative The 10% of gross weight, particle diameter is that the siccative of below 0.074mm accounts for the 57% of siccative gross weight, balance of particle diameter 0.075～ The siccative of 0.15mm；
In described petroleum coke particles, the mass content of ash is 0.42%, and the mass content of volatile matters is 0.8%, sulphur content Mass content be 0.8%, petroleum coke true density be 2.04g/cm2, oil resistivity is 429 μ Ω m；Described pitch coke In grain, the mass content of ash is 0.5%, and the mass content of volatile matters is 1.2%, and the mass content of sulphur content is 0.2%, Colophonium Coke powder end ratio resistance is 350 μ Ω mm2/m；In the broken granule of described graphite, the mass content of ash is 0.1%, the matter of volatile matters Amount content is 0.2%, and the mass content of sulphur content is 0.2%, and graphite comminuted powder ratio resistance is 350 μ Ω mm2/m；Described needle-like Burnt granule is super premium needle coke granule；The coefficient of expansion of described super premium needle coke granule is 2.0 × 10-6Mm/ DEG C, sulfur quality hundred Content is divided to be 0.5%, true density is 2.12g/cm3, vanadium weight/mass percentage composition is 10ppm, and nickel content weight/mass percentage composition is 30%；
Step 2, blank molding
Siccative and Colophonium mix homogeneously are obtained compound, pours compound in mould under mould vibrations, keep mould Tool vibrations, are 2kg/cm in pressure2Pressure under compound in mould is densified to the graphite cylinder body blank of 700mm；Described mould Frequency of vibration during tool vibrations is 2700 beats/min；
Step 3, graphite cylinder body blank roasting
Graphite cylinder body is placed in roaster and carries out roasting；
When described graphite cylinder body wall thickness is 90mm, the roasting of graphite cylinder body blank described in step 3 is entered according to the following steps OK：
The furnace temperature of roaster is warming up to 350 DEG C with the programming rate of 4.4 DEG C/h and is incubated after 50h, then with 1.7 DEG C/h's Programming rate is warming up to 400 DEG C and is incubated 30h, then is warming up to 500 DEG C with the programming rate of 1.4 DEG C/h and is incubated 70h, then with The programming rate of 2.0 DEG C/h is warming up to 600 DEG C and is incubated 50h, then is warming up to 700 DEG C with the programming rate of 4.0 DEG C/h and is incubated 25h, then be warming up to 800 DEG C with the programming rate of 5.0 DEG C/h and be incubated 20h, then it is warming up to 1000 DEG C with the programming rate of 8 DEG C/h And it is incubated 25h, then be warming up to 1300 DEG C with the programming rate of 10 DEG C/h and be incubated 30h, finally it is incubated 20h at 1300 DEG C；
Step 4, graphite cylinder body blank graphitization
Fill full resistance material into the graphite cylinder body blank after roasting, the insulation material parcel graphite tube being 500mm with thickness The upper bottom surface of body blank and bottom surface, wrap up the circumferential surface of graphite cylinder body blank, Ran Houyong with the resistance material that thickness is 150mm Thickness is the circumferential surface of the insulation material parcel resistance material of 400mm, the furnace burdening of the 500mm that tiles in graphitizing furnace bottom；Then Start graphitization；
Described graphited heating means are：
First graphitization in-furnace temperature was at the uniform velocity warming up to 1700 DEG C in 60 hours, then at the uniform velocity heated up in 22 hours To 2300 DEG C, finally it is warming up to 2500 DEG C in 5 hours, that is, completes；
Described resistance material is the compound of graphitized coke and green coke, and the mass ratio of the compound of graphitized coke and green coke is 7: 3, resistance material granularity is 10～25mm；Described insulation material is the mixture of metallurgical coke and quartz sand, metallurgical wherein in mixture The mass fraction of coke powder is 75%, and the granularity of insulation material is 2～6mm；Described furnace burdening bottom is that the bulk density after compacting is 1.039Kg/m3Quartz sand, top is quartz sand and the metallurgical coke compound after compacting, quartz sand in the compound of top Mass fraction is 40%, and in furnace burdening, the granularity of metallurgical coke is 2～10mm.
The present embodiment possesses following beneficial effect：
1st, pass through scientific algorithm before the present embodiment preparation, then carry out graphite cylinder body material preparation again, so the present embodiment The graphite cylinder body reasonable in design of method preparation, reliable in quality；Graphite cylinder body outer surface prepared by the present embodiment method is no Crackle, no hole, even structure, wall thickness reduction amount is ± 1mm, the both ends of the surface depth of parallelism 0.15%, perpendicularity franchise ± 0.1%, Crack side between the teeth and fall rib length and be not more than 30mm, crack side between the teeth and fall rib depth and be not more than 3mm；Product bending strength 18MPa, comprcssive strength 28MPa, Bulk density 1.68g/cm3, ratio resistance 6.2～7.5 μ Ω mm2/ m, ash be less than 0.5%, linear expansion coefficient be not more than 2.4 × 10-6Mm/ DEG C (between 100 DEG C～600 DEG C), elastic modelling quantity is 11Gpa；
2nd, graphite cylinder body is prepared using the present embodiment method, raw material can save 17% than traditional processing technology, and original The method first preparing real core cylinder compares, and can save roasting time 100 hours on calcining process, saves coal-fired 360Kg/ ton, stone Blackization process in product per ton can economize on electricity more than 300 degree, mechanical processing process with splicing circle make production technology compared with, every Graphite cylinder body can save man-hour 56 hours, saves binding resin 6Kg/m2, therefore the present embodiment possesses the effect of energy-saving and environmental protection；
3rd, the present embodiment method adopts vibration moulding technology, makes graphite cylinder body compact structure, intensity index directivity gap Little, it is preferable graphite inhibition and generation construction equipment the selection of material, and the product longtime running of the present embodiment method preparation is non-directional Strength Changes.
4th, the graphite cylinder body heat transfer property of the present embodiment method preparation is stainless 4 times, and heat stability is high, chemically stable Property is good；
5th, the graphite cylinder body that the present embodiment method obtains can be widely used in absorption tower, Analytic Tower, vacuum drying oven, chlorination hydrido Become stove, the main element of tail gas absorber, can be in heating, the different process production process of cooling, its main element has resistance to Pressure, decay resistance, so that be employed equipment more energy-saving and environmental protection；
6th, in the present embodiment preparation process, vibro-moulding process is a kind of new graphite cylinder body blank moulding process, in height Under the vibration of frequency, the blanking in vibration, hot gas can be made to discharge, be always maintained at grinding tool vibrations during preparing blank, The inside and outside wall of blank again by frictional force counteracting force so as to surfaces externally and internally fineness and internal density improve, make final products Mechanical strength directional difference little, so vibro-moulding process is reasonable in design.

Claims (10)

1. a kind of preparation method of graphite cylinder body is it is characterised in that the method is carried out according to the following steps：
Step one, weigh raw material
It is that 74%～78% siccative and balance of Colophonium weigh raw material by mass percentage；
Described siccative by mass percentage by 60% petroleum coke particles, 20% pitch coke granule, 5%～10% needle coke Granule and balance of graphite broken granule composition；
Step 2, blank molding
Siccative and Colophonium mix homogeneously are obtained compound, pours compound in mould under mould vibrations, keep mould shake Dynamic, it is 1.12～2kg/cm in pressure2Pressure under compound in mould is densified to the graphite cylinder body blank of object height；Institute State frequency of vibration during mould vibrations and be 2300～2700 beats/min；
Step 3, graphite cylinder body blank roasting
Graphite cylinder body is placed in roasting burnt furnace and carries out roasting；
Step 4, graphite cylinder body blank graphitization
Fill full resistance material into the graphite cylinder body blank after roasting, the insulation material parcel graphite tube being 500～800mm with thickness The upper bottom surface of body blank and bottom surface, wrap up the circumferential surface of graphite cylinder body blank with the resistance material that thickness is 100～150mm, Then with thickness be 350～400mm insulation material wrap up resistance material circumferential surface, graphitizing furnace bottom tile 500～ The furnace burdening of 1000mm；Then start graphitization；
Described graphited heating means are：
First graphitization in-furnace temperature was at the uniform velocity warming up to 1650～1750 DEG C in 58～62 hours, then at 20～24 hours Inside at the uniform velocity it is warming up to 2250～2350 DEG C, be finally warming up to 2500 DEG C in 5～6 hours, that is, complete；
Described resistance material is the compound of graphitized coke and green coke, and the mass ratio of the compound of graphitized coke and green coke is 7:3, electricity Resistance material granularity is 10～25mm；Described insulation material is the mixture of metallurgical coke and quartz sand, wherein metallurgical coke in mixture Mass fraction be 65%～75%, the granularity of insulation material is 0～6mm；Described furnace burdening bottom is the bulk density after compacting For 0.850～1.039Kg/m3Quartz sand, top is quartz sand and the metallurgical coke compound after compacting, in the compound of top The mass fraction of quartz sand is 30%～40%, and in furnace burdening, the granularity of metallurgical coke is 0～10mm.
2. a kind of graphite cylinder body according to claim 1 preparation method it is characterised in that：During described in step one, Colophonium is Warm coal tar pitch.
3. a kind of graphite cylinder body according to claim 1 preparation method it is characterised in that：When described graphite tube body wall When thickness is less than 100mm, in the siccative described in step one, the siccative more than 2mm for the particle diameter accounts for less than the 2% of siccative gross weight, and particle diameter is The siccative of 1～2mm accounts for the 8%～14% of siccative gross weight, particle diameter be 0.5～1mm siccative account for siccative gross weight 7%～ 13%, particle diameter is that the siccative of below 0.074mm accounts for the 54%～60% of siccative gross weight, balance of particle diameter 0.075～0.15mm Siccative.
4. a kind of graphite cylinder body according to claim 1 preparation method it is characterised in that：When described graphite tube body wall When thickness is more than 100mm, in the siccative described in step one, the siccative more than 1mm for the particle diameter accounts for less than the 2% of siccative gross weight, and particle diameter is The siccative of 0.5～1mm accounts for the 10%～16% of siccative gross weight, and particle diameter is that the siccative of 0.2～0.5mm accounts for siccative gross weight 7%～13%, particle diameter is that the siccative of below 0.074mm accounts for the 53%～59% of siccative gross weight, balance of particle diameter 0.075～ The siccative of 0.15mm.
5. a kind of graphite cylinder body according to claim 1 preparation method it is characterised in that：When described graphite tube body wall When thickness is more than 100mm, the roasting of graphite cylinder body blank described in step 3 is carried out according to the following steps：
The furnace temperature of roaster is warming up to 130～350 DEG C with the programming rate of 4.4 DEG C/h and is incubated after 50h, then with 1.7 DEG C/h Programming rate be warming up to 350～400 DEG C and be incubated 30h, then be warming up to 400～500 DEG C with the programming rate of 1.1 DEG C/h and protect Warm 90h, then be warming up to 500～600 DEG C with the programming rate of 1.7 DEG C/h and be incubated 60h, then the programming rate liter with 3.3 DEG C/h Temperature to 600～700 DEG C and is incubated 30h, then is warming up to 700～800 DEG C with the programming rate of 5.0 DEG C/h and is incubated 20h, then with The programming rate of 6.7 DEG C/h is warming up to 800～1000 DEG C and is incubated 30h, then it is warming up to 1000 with the programming rate of 10 DEG C/h～ 1300 DEG C and be incubated 30h, finally it is incubated 20h at 1275～1325 DEG C.
6. a kind of graphite cylinder body according to claim 1 preparation method it is characterised in that：When described graphite tube body wall When thickness is less than 100mm, the roasting of graphite cylinder body blank described in step 3 is carried out according to the following steps：
The furnace temperature of roaster is warming up to 130～350 DEG C with the programming rate of 4.4 DEG C/h and is incubated after 50h, then with 1.7 DEG C/h Programming rate be warming up to 350～400 DEG C and be incubated 30h, then be warming up to 400～500 DEG C with the programming rate of 1.4 DEG C/h and protect Warm 70h, then be warming up to 500～600 DEG C with the programming rate of 2.0 DEG C/h and be incubated 50h, then the programming rate liter with 4.0 DEG C/h Temperature is to 600～700 DEG C and be incubated 25h, then is warming up to 700～800 DEG C with the programming rate of 5.0 DEG C/h and is incubated 20h, then with 8 DEG C/programming rate of h is warming up to 800～1000 DEG C and is incubated 25h, then be warming up to 1000～1300 with the programming rate of 10 DEG C/h DEG C and be incubated 30h, finally 1275～1325 DEG C be incubated 20h.
7. a kind of graphite cylinder body according to claim 1 preparation method it is characterised in that：Petroleum coke described in step one In grain, the mass content of ash is not more than 0.42%, and the mass content of volatile matters is not more than 0.8%, and the mass content of sulphur content is not More than 0.8%, petroleum coke true density is not less than 2.04g/cm2, oil resistivity no more than 429 μ Ω m.
8. a kind of graphite cylinder body according to claim 1 preparation method it is characterised in that：Pitch coke described in step one In grain, the mass content of ash is not more than 0.5%, and the mass content of volatile matters is not more than 1.2%, and the mass content of sulphur content is little In 0.2%, pitch coke powder ratio resistance is not more than 350 μ Ω mm2/m.
9. a kind of graphite cylinder body according to claim 1 preparation method it is characterised in that：Broken of graphite described in step one In grain, the mass content of ash is not more than 0.1%, and the mass content of volatile matters is not more than 0.2%, and the mass content of sulphur content is little In 0.2%, graphite comminuted powder ratio resistance is not more than 350 μ Ω mm2/m.
10. a kind of graphite cylinder body according to claim 1 preparation method it is characterised in that：Needle coke described in step one Granule is super premium needle coke granule, senior needle coke particles or one-level needle coke particles；The expansion of described super premium needle coke granule Coefficient is not more than 2.0 × 10-6Mm/ DEG C, sulfur weight/mass percentage composition is 0.5%, and true density is 2.12g/cm3, vanadium percent mass Content is 10ppm, and nickel content weight/mass percentage composition is 30%；The coefficient of expansion of described senior needle coke particles is 2.0 × 10- 6Mm/ DEG C～3.0 × 10-6Mm/ DEG C, sulfur weight/mass percentage composition is 0.6%, and true density is 2.10g/cm3, vanadium percent mass contains Measure as 10ppm, nickel content weight/mass percentage composition is 30%；The coefficient of expansion of described one-level needle coke particles is 3.0 × 10-6mm/ DEG C～4.0 × 10-6Mm/ DEG C, sulfur weight/mass percentage composition is 0.8%, and true density is 2.10g/cm3, vanadium weight/mass percentage composition is 10ppm, nickel content weight/mass percentage composition is 30%.
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CN1951805A (en) * 2006-11-20 2007-04-25 彭绍权 Production method of large diameter tubular semi-graphite carbon electrode
CN101948675A (en) * 2010-08-26 2011-01-19 大同市新成特炭有限公司 Heat accumulation and energy storage graphite material for solar thermal power generation and preparation method thereof
CN102206080A (en) * 2011-05-05 2011-10-05 大同市新成特炭有限公司 Graphite material for monocrystalline silicon growth thermal field in solar photovoltaic industry and production method thereof
CN102158999A (en) * 2011-05-16 2011-08-17 方大炭素新材料科技股份有限公司 Phi 800mm general power graphite electrode and production method thereof
CN103553617A (en) * 2013-10-29 2014-02-05 大同新成新材料股份有限公司 Graphite material for continuous casting mold and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
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CN108545735A (en) * 2018-06-27 2018-09-18 湖北红业建材科技开发有限公司 A kind of turntable continous way graphite tube graphitizing furnace and graphitizing method is carried out to graphite tube
CN111483171A (en) * 2020-04-22 2020-08-04 四川士达特种炭材有限公司 Isostatic pressing graphite barrel material forming die and isostatic pressing cylindrical graphite processing method
CN111483171B (en) * 2020-04-22 2021-04-23 四川士达特种炭材有限公司 Processing method for producing isostatic pressing cylindrical graphite by using isostatic pressing graphite barrel material forming die

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