CN103130208A - Method for producing carbon intermediate by using ball pressing process - Google Patents
Method for producing carbon intermediate by using ball pressing process Download PDFInfo
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- CN103130208A CN103130208A CN2013100900462A CN201310090046A CN103130208A CN 103130208 A CN103130208 A CN 103130208A CN 2013100900462 A CN2013100900462 A CN 2013100900462A CN 201310090046 A CN201310090046 A CN 201310090046A CN 103130208 A CN103130208 A CN 103130208A
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- element intermediate
- ball press
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- 238000000034 method Methods 0.000 title claims abstract description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 238000003825 pressing Methods 0.000 title abstract 3
- 239000000203 mixture Substances 0.000 claims abstract description 93
- 239000002994 raw material Substances 0.000 claims abstract description 55
- 239000000463 material Substances 0.000 claims abstract description 49
- 238000004898 kneading Methods 0.000 claims abstract description 39
- 238000002156 mixing Methods 0.000 claims abstract description 34
- 239000000571 coke Substances 0.000 claims abstract description 29
- 239000003245 coal Substances 0.000 claims abstract description 13
- 239000006253 pitch coke Substances 0.000 claims abstract description 7
- 229910021383 artificial graphite Inorganic materials 0.000 claims abstract description 6
- 229910021382 natural graphite Inorganic materials 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 162
- 239000003610 charcoal Substances 0.000 claims description 90
- 239000002006 petroleum coke Substances 0.000 claims description 29
- 239000011800 void material Substances 0.000 claims description 27
- 239000000758 substrate Substances 0.000 claims description 26
- 239000011294 coal tar pitch Substances 0.000 claims description 19
- 239000011341 hard coal tar pitch Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000002131 composite material Substances 0.000 claims description 13
- 239000000178 monomer Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 13
- 239000003575 carbonaceous material Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 10
- 238000005242 forging Methods 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 8
- 239000002699 waste material Substances 0.000 claims description 8
- 238000000280 densification Methods 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 239000011301 petroleum pitch Substances 0.000 claims description 6
- 229920003987 resole Polymers 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 5
- 239000011334 petroleum pitch coke Substances 0.000 claims description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 230000001413 cellular effect Effects 0.000 claims description 3
- 238000004939 coking Methods 0.000 claims description 3
- 238000002309 gasification Methods 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 abstract 3
- 239000002008 calcined petroleum coke Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 235000015895 biscuits Nutrition 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000005504 petroleum refining Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a method for producing a carbon intermediate by using a ball pressing process. The method is characterized in that at least one of calcined petroleum coke, pitch coke, electrically calcined coal, metallurgical coke, natural graphite, synthetic graphite, carbon product return scrap and carbon product reclaimed material is used as the material of the carbon intermediate. The production method comprises the steps of selecting raw materials, carrying out grain composition, selecting a binding agent, controlling the addition of the binding agent, mixing or kneading and pressing balls to obtain the carbon intermediate. The carbon intermediate has a shape of sphere, has uniformly and directionally arranged carbons, is a carbon green body of anisotropy, and has plasticity when the temperature is higher than the softening temperature of the binding agent, and the volume density is 1.65-1.80g/cm<3>. The high density and anisotropy of the carbon intermediate are realized with the granularity of the supplied materials maintained.
Description
Technical field
The invention belongs to chemical technology field, belong to the method for a kind of Carbon Materials and raw material production charcoal thereof element intermediate, particularly a kind of spongy, cellular, fine particulate, powdery; Flakey Carbon Materials and raw material thereof adopt ball press technique to produce the method for charcoal element intermediate.
Background technology
Refinery coke is last procedure surplus products of petroleum refining, along with the development of petroleum refining industry and the raising of fine chemical technology level, can extract more chemical products with high added-value in oil per ton, causes that in oil residuum refinery coke, useful component reduces in a large number.That is to say, petroleum chemical enterprise's scientific-technical progress is that petrochemical complex is created huge appreciation space, be social creativity multivalence value more, but what the carbon industry of giving the existence of dependence refinery coke raw material brought is difficulty and challenge, petroleum chemical enterprise unconditionally produces refinery coke, and charcoal element enterprise has ready conditions and selects the refinery coke raw material.At present, supply and marketing refinery coke market, the refinery coke quantity that can reach Carbon Materials, the technical requirements of carbon product raw material is fewer and feweri.Main Problems: the refinery coke pore increases, and pore quantity increases; Refinery coke loosen deliquescing, strength decreased; The refinery coke macrobead is fewer and feweri, and the fine-grained powder amount is more and more.For these problems, the scientific research personnel, through long-term and unremitting effort, research, tackling key problem are by the raw material pre-mixing; High-temperature calcination; Multiple stage material compounding; Increase powder and coal-tar pitch consumption; Add the means such as trace element, take simultaneously the vacuum kneading; High-pressure molding; The measures such as anaerobic roasting just make the problems referred to above be eased, but pay high strength, high energy consumption, and high pollution, expensive cost have been walked a road for development of curing the symptoms, not the disease, finally cause Chinese carbon material and goods in the world market long-term low price hover; 10 times of price differences of the refinery coke raw material the highest formation of refinery coke raw material similar with international most advanced level of China are in " inexpensive " state for a long time.
Summary of the invention
The objective of the invention is the defective for above-mentioned existence, adopt the pressure ball production technique, by ball press roller rubber-insulated wire pressure, under wedding agent, powder coordinated, gross blow hole flattened it is diminished with carbon feedstock, and pore quantity reduces; Loose soft carbon structure, densification, compacting, intensity improves; Fine particle, powder are bonded to one; Reduce void content, intensity, granulometric composition fluctuation variation; Charcoal biscuit body after pressure ball is the formed coke charcoal through roasting, thermal treatment; For the production of Carbon Materials, carbon product, be equivalent to that Carbonaceous material to be formed is called charcoal element intermediate after kneading, a kind of method that adopts ball press technique to produce charcoal element intermediate is provided.
The present invention adopts ball press technique to produce the method content Description of charcoal element intermediate:
The present invention adopts ball press technique to produce the method for charcoal element intermediate, it is characterized in that: charcoal element intermediate is to select after-smithing petroleum coke or pitch coke or electric forging coal or metallurgical coke or natural graphite or synthetic graphite or carbon product production returns or carbon product reclaimed materials, wherein more than one mixtures are raw material, adopt the pressure ball production technique, control wedding agent add-on 7～16%, under higher than 60 ℃ of conditions of wedding agent softening point temperature, mixing, kneading are through adjusting ball press roller rubber-insulated wire speed 0.5～5m/min; Line pressure is than 0.3～1.5t/mm, with spongy or cellular, loose shape, fine particulate, powdery, flakey Carbon Materials and raw material, be pressed into carbonaceous evenly, align, anisotropisation, volume density 1.65～1.80 g/cm
3Charcoal element intermediate;
Its production method: adopt material choice → grain composition, wedding agent selection, wedding agent add-on to control → mixing or kneading → pressure ball → charcoal element intermediate feature:
(1) material choice
Adopt after-smithing petroleum coke or pitch coke or electric forging coal or metallurgical coke or natural graphite or synthetic graphite or carbon product to produce returns or carbon product reclaimed materials, wherein more than one mixtures are raw material;
Grain composition, wedding agent are selected, the wedding agent add-on is controlled
Calculate by mass percentage grain composition material+wedding agent=100%;
Grain composition: two kinds of methods are arranged;
1. produce carbon product grain composition method: take production dense char material, carbon product as the purpose grain composition, can satisfy the grain composition requirement that the present invention produces charcoal element intermediate at Carbon Materials, carbon product production line;
2. low-cost grain composition method: less than the natural particle size material 64 ~ 93% below 50mm, less than 0.1mm powder 0～20%;
(2) wedding agent is selected:
Petroleum pitch and modification derived product or coal-tar pitch and modification derived product or resol, wherein more than one mixtures are wedding agent, require the coking value of wedding agent greater than 40%;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled between 7～16%, when containing wedding agent in the raw material that adopts, calculate already contg wedding agent quantity in raw material;
(3) mixing or kneading
Adopt hot mixing or kneading mode, change according to wedding agent viscosity under differing temps, when the selection coal-tar pitch, when petroleum pitch is wedding agent, with heating raw materials to 130 after grain composition～200 ℃, when selecting resol to be wedding agent, with heating raw materials to 40 after grain composition～100 ℃, after adding wedding agent, be mixed together or kneading 1～60min;
(4) pressure ball
Mix or the good raw material of kneading, keeping under mixing or kneading temperature condition, deliver to the ball press charging tank, the feeding coal of feeding device below adjustment and control charging tank, continuous and quantitative is to the ball press feed, ball press roller rubber-insulated wire speed is controlled at 0.5～5m/min according to wedding agent kind, softening point temperature, volatilization temperature, gasification temperature, ignition temperature variation, ball press normal operation line pressure is than 0.3～1.5t/mm, base substrate after pressure ball sieves by grate, the grid section pitch-row be controlled at base substrate three-dimensional dimension minimum size 4/5～1/2 between; Minus mesh has two kinds of selections: when 1. keeping pressure ball, temperature turns back to the ball press charging tank, and feed carries out pressure ball again; 2. turn back in mixing or kneading equipment and again mix or kneading, oversize is charcoal element intermediate;
(5) charcoal element intermediate feature
Charcoal element intermediate is spherical or the unequal oval-shaped ball of three-dimensional dimension, and length direction sphere size is less than 80mm; The two different three states that occur of roller skin spacing during with the ball press pressure ball according to pressure ball material wedding agent content: 1. when wedding agent content less than 10%, ball press pressure ball two roller skin spacings are during less than 1mm, what suppress out from ball press roller skin is independence, separation, monomer ball; 2. when wedding agent content 10～12%; During ball press pressure ball two roller skin spacing 1～3 mm, from ball press roller micromicro to suppress two disjunctor balls that link together by ball-and-socket edge 1～3 thick densification material of mm more than ball; 3. work as wedding agent content greater than 12%; Ball press pressure ball two roller skin spacings to suppress, are pressed the band shape that roller skin width forms from ball press roller micromicro during greater than 3 mm; Ball and ball-and-socket edge are greater than the 3 complete disjunctor balls that link together of the thick densification material of mm; Charcoal element intermediate wedding agent content 7～16%; Has plasticity-higher than the wedding agent softening temperature; Volume density 1.65～1.80g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 10%, and the internal porosity rate is less than 25%; Has anisotropisation carbonaceous characteristic.
The charcoal element intermediate that the present invention obtains contains 7～16% wedding agents, has spheroid form, carbonaceous evenly, align, be the charcoal biscuit body of anisotropisation, have plasticity-higher than the wedding agent softening temperature, volume density 1.65～1.80 g/cm
3, keep under raw material supplied materials granularity condition as far as possible, realize charcoal element intermediate high-density, anisotropisation.
Embodiment
The method that the present invention adopts ball press technique to produce charcoal element intermediate is to realize like this, the below does and illustrates, and the present invention adopts ball press technique to produce the concrete implementation step of method of charcoal element intermediate: material choice → grain composition, wedding agent are selected, the wedding agent add-on controls → mixes or kneading → pressure ball → charcoal element intermediate feature.
Its production method comprises:
(1) material choice
Adopt after-smithing petroleum coke or pitch coke or electric forging coal or metallurgical coke or natural graphite or synthetic graphite or carbon product to produce returns or carbon product reclaimed materials, wherein more than one mixtures are raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate by mass percentage grain composition material+wedding agent=100%.
Grain composition: two kinds of methods are arranged;
1. produce carbon product grain composition method: existing Carbon Materials, carbon product production line, any production dense char material, carbon product are the purpose grain composition, all can satisfy the grain composition requirement that the present invention produces charcoal element intermediate.Advantage: take full advantage of existing Carbon Materials, carbon product production-line technique, the charcoal of producing element intermediate volume density is high.Shortcoming: the raw material macrobead destroys serious; The raw material ratio surface-area increases; Wedding agent consumption and production cost increase; The oxidation-resistance of charcoal element intermediate, anti-thermal shock stability, electroconductibility reduce;
2. low-cost grain composition method: less than the natural particle size material 64 ~ 93% below 50mm, less than 0.1mm powder 0～20%; Advantage: keep feed particles to form; Simplification of flowsheet has reduced raw material ratio surface-area, wedding agent consumption, production cost.Shortcoming: the charcoal element intermediate volume density of producing is lower slightly.
Wedding agent is selected:
Petroleum pitch and modification derived product or coal-tar pitch and modification derived product or resol, wherein more than one mixtures are wedding agent, require the coking value of wedding agent greater than 40%.
The wedding agent add-on is controlled:
The wedding agent add-on is controlled between 7～16%, when containing wedding agent in the raw material that adopts, calculate already contg wedding agent quantity in raw material.
(3) mixing or kneading
Adopt hot mixing or kneading mode, change according to wedding agent viscosity under differing temps, when the selection coal-tar pitch, when petroleum pitch is wedding agent, with heating raw materials to 130 after grain composition～200 ℃, when selecting resol to be wedding agent, with heating raw materials to 40 after grain composition～100 ℃, after adding wedding agent, be mixed together or kneading 1～60min.
(4) pressure ball
Mix or the good raw material of kneading, keep mixing or the kneading temperature condition under, deliver to the ball press charging tank, adjust and control the feeding coal of feeding device below charging tank, continuous and quantitative is to the ball press feed.Ball press roller rubber-insulated wire speed is controlled at 0.5～5m/min according to wedding agent kind, softening point temperature, volatilization temperature, gasification temperature, ignition temperature variation, and ball press normal operation line pressure is than 0.3～1.5t/mm.Base substrate after pressure ball sieves by grate, the grid section pitch-row be controlled at base substrate three-dimensional dimension minimum size 4/5～1/2 between.Minus mesh has two kinds of selections: when 1. keeping pressure ball, temperature turns back to the ball press charging tank, and feed carries out pressure ball again; 2. turn back in mixing or kneading equipment and again mix or kneading.Oversize is charcoal element intermediate.
(5) charcoal element intermediate feature
Charcoal element intermediate is spherical or the unequal oval-shaped ball of three-dimensional dimension, and length direction sphere size is less than 80mm.The two different three states that occur of roller skin spacing during with the ball press pressure ball according to pressure ball material wedding agent content: 1. when wedding agent content less than 10%; Ball press pressure ball two roller skin spacings are during less than 1mm, and what suppress out from ball press roller skin is independence, separation, monomer ball; 2. when wedding agent content 10～12%; During ball press pressure ball two roller skin spacing 1～3 mm, from ball press roller micromicro to suppress two disjunctor balls that link together by ball-and-socket edge 1～3 thick densification material of mm more than ball; 3. work as wedding agent content greater than 12%; Ball press pressure ball two roller skin spacings to suppress, are pressed the band shape that roller skin width forms from ball press roller micromicro during greater than 3 mm; Ball and ball-and-socket edge are greater than the 3 complete disjunctor balls that link together of the thick densification material of mm.Charcoal element intermediate wedding agent content 7～16%; Has plasticity-higher than the wedding agent softening temperature; Volume density 1.65～1.80g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 10%, and the internal porosity rate is less than 25%; Has anisotropisation carbonaceous characteristic.
Embodiment 1
The production method of low-cost charcoal element intermediate
(1), material choice: the employing after-smithing petroleum coke is raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate according to the mass fraction grain composition material+wedding agent=100%;
Grain composition: adopt low-cost grain composition method;
40～0mm natural particle size refinery coke 92%;
Wedding agent is selected:
Selecting 106 ℃ of hard coal-tar pitch of softening point temperature is wedding agent;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled at 8%;
(3) mix
Adopt hot hybrid mode, 40～0mm natural particle size refinery coke is dropped in mixing machine, heating makes temperature of charge reach 150 ~ 175 ℃, then adds 106 ℃ of hard coal-tar pitch wedding agents of softening point temperature, is mixed together 2～30min;
(4) pressure ball
Adjust ball press linear pressure 0.5～1.2t/mm, control ball press roller rubber-insulated wire speed 0.8～3.0m/min.Mix raw material, send into the ball press charging tank, keep under the condition of 150 ~ 175 ℃ of temperature, continuous feeder is to the ball press continuous dosing of very below the ball press charging tank.Suppress oval base substrate size Φ 40 * 32 * 25, after pressure ball, base substrate sieves by grate, grid section pitch-row 13mm, and the minus mesh insulation turns back to ball press charging tank pressure ball again, and oversize is charcoal element intermediate;
(5) charcoal element intermediate feature
After pressure ball, charcoal element intermediate, be independence, separation, monomer ball, coal-tar pitch content 8%; Volume density 〉=1.65g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 12%, and the internal porosity rate is less than 25%; Has anisotropisation carbonaceous characteristic.
Embodiment 2
The prebaked anode production method of charcoal element intermediate
(1), material choice: adopt and produce the prebaked anode after-smithing petroleum coke; The waste product of graphitized electrode or anode scrap are raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate according to the mass fraction grain composition material+wedding agent=100%;
Grain composition: adopt low-cost grain composition method;
The natural particle size refinery coke 72% of 35～0mm;
0.1 the waste product of～0mm graphitized electrode or anode scrap powder 1%;
0.1～0mm refinery coke powder 15%;
Wedding agent is selected:
Selecting 105 ℃ of hard coal-tar pitch of softening point temperature is wedding agent;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled at 12%;
(3) mix
Adopt hot hybrid mode, the material after grain composition is dropped in mixing machine, heating makes temperature of charge reach 150 ~ 175 ℃, then adds 105 ℃ of hard coal-tar pitch wedding agents of softening point temperature, is mixed together 2～50min;
(4) pressure ball
Adjust ball press linear pressure 0.4～1.2t/mm, control ball press roller rubber-insulated wire speed 0.5～2.5m/min.Mix raw material, send into the ball press charging tank, under the condition that keeps 150 ~ 175 ℃ of temperature, the belted electronic balance below the ball press charging tank is to the ball press continuous dosing of very.Suppress oval base substrate size Φ 36 * 28 * 22, the base substrate after pressure ball sieves by grate, grid section pitch-row 12mm, and minus mesh turns back to mixing machine and reheats mixing, and oversize is charcoal element intermediate;
(5) charcoal element intermediate feature
Charcoal element intermediate after pressure ball, for independence, separation, monomer ball and two disjunctor balls that connect together more than ball exist simultaneously, coal-tar pitch content 12%; Volume density 〉=1.68g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 8%, and the internal porosity rate is less than 20%; Has anisotropisation carbonaceous characteristic.
Embodiment 3
The graphitized electrode production method of charcoal element intermediate
(1), material choice: adopt graphitized electrode to produce and use after-smithing petroleum coke; The graphitized electrode moulding base (containing 23% coal-tar pitch wedding agent) that gives up; The graphitized electrode anode scrap; Natural flake graphite is raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate according to the mass fraction grain composition material+wedding agent=100%;
Grain composition: adopt low-cost grain composition method;
35～0mm after-smithing petroleum coke 62%;
35～0mm graphitized electrode moulding base (containing 23% coal-tar pitch wedding agent) 10% that gives up;
2～0mm natural flake graphite 3%;
0.1～0mm graphitized electrode anode scrap powder 3%;
0.1～0mm after-smithing petroleum coke powder 12%;
Wedding agent is selected:
Selecting 110 ℃ of hard coal-tar pitch of softening point temperature is wedding agent;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled at 10%;
(3) mix
Adopt hot hybrid mode, the material after grain composition is dropped in mixing machine, heating makes temperature of charge reach 160 ~ 185 ℃, then adds 110 ℃ of hard coal-tar pitch wedding agents of softening point temperature, is mixed together 5～60min;
(4) pressure ball
Adjust ball press linear pressure 0.4～1.2t t/mm, control ball press roller rubber-insulated wire speed 0.5～3.5m/min.The raw material that mixes is sent into the ball press charging tank, and under the condition that keeps 160 ~ 185 ℃ of temperature, the belted electronic balance below the ball press charging tank or other feeding device are to the ball press continuous dosing of very.Suppress oval base substrate size Φ 32 * 25 * 18, the base substrate after pressure ball sieves by grate, grid section pitch-row 10mm, and the minus mesh insulation turns back to the ball press charging tank and continues pressure ball, and oversize is charcoal element intermediate;
(5) charcoal element intermediate feature
Charcoal element intermediate after pressure ball, for independence, separation, monomer ball and two disjunctor balls that connect together more than ball exist simultaneously, coal-tar pitch content 12.3%; Volume density 〉=1.70g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 7%, and the internal porosity rate is less than 18%; Has anisotropisation carbonaceous characteristic.
Embodiment 4
Low conduction charcoal element intermediate production method
(1), material choice: adopt after-smithing petroleum coke; Pitch coke; Electric forging coal; Or metallurgical coke is raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate according to the mass fraction grain composition material+wedding agent=100%;
Grain composition: adopt low-cost grain composition method;
30～0mm after-smithing petroleum coke 25%;
30～0mm pitch coke 40%;
3～0mm electric forging coal 12%;
0.1～0mm pitch coke or metallurgical coke powder 15%;
Wedding agent is selected:
Selecting the heat-reactive phenolic resin of fixed carbon 70% is wedding agent;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled at 8%;
(3) mix
Adopt the heating hybrid mode, the material after grain composition is dropped in mixing machine, make temperature of charge reach 50 ~ 70 ℃, then add the heat-reactive phenolic resin wedding agent of fixed carbon 70%, be mixed together 10～60min;
(4) pressure ball
Adjust ball press linear pressure 0.5～1.5t/mm, control ball press roller rubber-insulated wire speed 0.5～4.0m/min.The raw material that mixes is sent into the ball press charging tank, and under the condition that keeps 50 ~ 70 ℃ of temperature, the belted electronic balance below the ball press charging tank or other feeding machine are to the ball press continuous dosing of very.Suppress spherical base substrate size Φ 30, the base substrate after pressure ball sieves by grate, grid section pitch-row 15mm, and the minus mesh insulation turns back to the ball press charging tank and continues pressure ball, and oversize is charcoal element intermediate.Charcoal element intermediate is under 150 ~ 200 ℃ of temperature condition, and insulation greater than 48h, just becomes the formed coke charcoal continuously;
(5) charcoal element intermediate feature
After pressure ball, charcoal element intermediate, be independence, separation, monomer ball; Volume density 〉=1.68g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 10%, and the internal porosity rate is less than 20%; Has anisotropisation carbonaceous characteristic.
Embodiment 5
The high-density electrode production method of charcoal element intermediate
(1), material choice: adopt the electrode after-smithing petroleum coke; Graphitized electrode waste product or anode scrap are raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate according to the mass fraction grain composition material+wedding agent=100%;
Grain composition: adopt the carbon product grain composition method of producing;
10～5mm after-smithing petroleum coke 20%;
5～2mm after-smithing petroleum coke 25%;
2～0mm after-smithing petroleum coke 20%;
0.1～0mm after-smithing petroleum coke powder 20%;
0.1～0mm graphitized electrode waste product or anode scrap powder 2%.
Wedding agent is selected:
Selecting 108 ℃ of hard coal-tar pitch of softening point temperature is wedding agent;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled at 13%;
(3) kneading
Adopt hot kneading mode, the material after grain composition is dropped in kneading machine, heating makes temperature of charge reach 155 ~ 180 ℃, then adds softening point temperature 108 ℃ of hard coal-tar pitch wedding agents, kneading 5～60min together;
(4) pressure ball
Adjust ball press linear pressure 0.4～1.2t/mm, control ball press roller rubber-insulated wire speed 0.5～3.0m/min.The raw material that kneading is good is sent into the ball press charging tank, and under the condition that keeps 155 ~ 180 ℃ of temperature, the belted electronic balance below the ball press charging tank or other feeding machine are to the ball press continuous dosing of very.Suppress oval base substrate size Φ 32 * 25 * 20, the base substrate after pressure ball sieves by grate, grid section pitch-row 12mm, and minus mesh turns back to mixing machine and reheats mixing, and oversize is charcoal element intermediate;
(5) charcoal element intermediate feature
Charcoal element intermediate after pressure ball, for independence, separation, monomer ball and two disjunctor balls that connect together more than ball exist simultaneously, coal-tar pitch content 13%; Volume density 〉=1.70g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 7%, and the internal porosity rate is less than 18%; Has anisotropisation carbonaceous characteristic.
Claims (6)
1. method that adopts ball press technique to produce charcoal element intermediate, it is characterized in that: charcoal element intermediate is to select after-smithing petroleum coke or pitch coke or electric forging coal or metallurgical coke or natural graphite or synthetic graphite or carbon product production returns or carbon product reclaimed materials, wherein more than one mixtures are raw material, adopt the pressure ball production technique, control wedding agent add-on 7～16%, under higher than 60 ℃ of conditions of wedding agent softening point temperature, mixing, kneading are adjusted ball press roller rubber-insulated wire speed 0.5～5m/min; Line pressure is than 0.3～1.5t/mm, with spongy or cellular, loose shape, fine particulate, powdery, flakey Carbon Materials and raw material, be pressed into carbonaceous evenly, align, anisotropisation, volume density 1.65～1.80 g/cm
3Charcoal element intermediate;
Its production method: adopt material choice → grain composition, wedding agent selection, wedding agent add-on to control → mixing or kneading → pressure ball → charcoal element intermediate feature:
(1) material choice
Adopt after-smithing petroleum coke or pitch coke or electric forging coal or metallurgical coke or natural graphite or synthetic graphite or carbon product to produce returns or carbon product reclaimed materials, wherein more than one mixtures are raw material;
Grain composition, wedding agent are selected, the wedding agent add-on is controlled
Calculate by mass percentage grain composition material+wedding agent=100%;
Grain composition: two kinds of methods are arranged;
1. produce carbon product grain composition method: take production dense char material, carbon product as the purpose grain composition, satisfy the grain composition requirement of producing charcoal element intermediate at Carbon Materials, carbon product production line;
2. low-cost grain composition method: less than the natural particle size material 64 ~ 93% below 50mm, less than 0.1mm powder 0～20%;
(2) wedding agent is selected:
Petroleum pitch and modification derived product or coal-tar pitch and modification derived product or resol, wherein more than one mixtures are wedding agent, require the coking value of wedding agent greater than 40%;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled between 7～16%, when containing wedding agent in the raw material that adopts, calculate already contg wedding agent quantity in raw material;
(3) mixing or kneading
Adopt hot mixing or kneading mode, change according to wedding agent viscosity under differing temps, when the selection coal-tar pitch, when petroleum pitch is wedding agent, with heating raw materials to 130 after grain composition～200 ℃, when selecting resol to be wedding agent, with heating raw materials to 40 after grain composition～100 ℃, after adding wedding agent, be mixed together or kneading 1～60min;
(4) pressure ball
Mix or the good raw material of kneading, keeping under mixing or kneading temperature condition, deliver to the ball press charging tank, the feeding coal of feeding device below adjustment and control charging tank, continuous and quantitative is to the ball press feed, ball press roller rubber-insulated wire speed is controlled at 0.5～5m/min according to wedding agent kind, softening point temperature, volatilization temperature, gasification temperature, ignition temperature variation, ball press normal operation line pressure is than 0.3～1.5t/mm, base substrate after pressure ball sieves by grate, the grid section pitch-row be controlled at base substrate three-dimensional dimension minimum size 4/5～1/2 between; Minus mesh has two kinds of selections: when 1. keeping pressure ball, temperature turns back to the ball press charging tank, and feed carries out pressure ball again; 2. turn back in mixing or kneading equipment and again mix or kneading, oversize is charcoal element intermediate;
(5) charcoal element intermediate feature
Charcoal element intermediate is spherical or the unequal oval-shaped ball of three-dimensional dimension, and length direction sphere size is less than 80mm; The two different three states that occur of roller skin spacing during with the ball press pressure ball according to pressure ball material wedding agent content: 1. when wedding agent content less than 10%, ball press pressure ball two roller skin spacings are during less than 1mm, what suppress out from ball press roller skin is independence, separation, monomer ball; 2. when wedding agent content 10～12%; During ball press pressure ball two roller skin spacing 1～3 mm, from ball press roller micromicro to suppress two disjunctor balls that link together by ball-and-socket edge 1～3 thick densification material of mm more than ball; 3. work as wedding agent content greater than 12%; Ball press pressure ball two roller skin spacings to suppress, are pressed the band shape that roller skin width forms from ball press roller micromicro during greater than 3 mm; Ball and ball-and-socket edge are greater than the 3 complete disjunctor balls that link together of the thick densification material of mm; Charcoal element intermediate wedding agent content 7～16%; Has plasticity-higher than the wedding agent softening temperature; Volume density 1.65～1.80g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 10%, and the internal porosity rate is less than 25%; Has anisotropisation carbonaceous characteristic.
2. employing ball press technique according to claim 1 is produced the method for charcoal element intermediate, it is characterized in that: the production method of low-cost charcoal element intermediate is:
(1), material choice: the employing after-smithing petroleum coke is raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate by mass percentage grain composition material+wedding agent=100%;
Grain composition: adopt low-cost grain composition method;
40～0mm natural particle size refinery coke 92%;
Wedding agent is selected:
Selecting 106 ℃ of hard coal-tar pitch of softening point temperature is wedding agent;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled at 8%;
(3) mix
Adopt hot hybrid mode, 30～0mm natural particle size refinery coke is dropped in mixing machine, heating makes temperature of charge reach 150 ~ 175 ℃, then adds 106 ℃ of hard coal-tar pitch wedding agents of softening point temperature, is mixed together 2～30min;
(4) pressure ball
Adjust ball press linear pressure 0.5～1.2t/mm, control ball press roller rubber-insulated wire speed 0.8～3.0m/min;
Mix raw material, send into the ball press charging tank, keep under the condition of 150 ~ 175 ℃ of temperature, continuous feeder is to the ball press continuous dosing of very below the ball press charging tank;
Suppress oval base substrate size Φ 40 * 32 * 25, after pressure ball, base substrate sieves by grate, grid section pitch-row 13mm, and the minus mesh insulation turns back to ball press charging tank pressure ball again, and oversize is charcoal element intermediate;
(5) charcoal element intermediate feature
After pressure ball, charcoal element intermediate, be independence, separation, monomer ball, coal-tar pitch content 8%; Volume density 〉=1.65g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 12%, and the internal porosity rate is less than 25%; Has anisotropisation carbonaceous characteristic.
3. employing ball press technique according to claim 1 is produced the method for charcoal element intermediate, it is characterized in that: prebaked anode with the production method of charcoal element intermediate is:
(1), material choice: adopt and produce the prebaked anode after-smithing petroleum coke; The waste product of graphitized electrode or anode scrap are raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate according to the mass fraction grain composition material+wedding agent=100%;
Grain composition: adopt low-cost grain composition method;
The natural particle size refinery coke 72% of 35～0mm;
0.1 the waste product of～0mm graphitized electrode or anode scrap powder 1%;
0.1～0mm refinery coke powder 15%;
Wedding agent is selected:
Selecting 105 ℃ of hard coal-tar pitch of softening point temperature is wedding agent;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled at 12%;
(3) mix
Adopt hot hybrid mode, the material after grain composition is dropped in mixing machine, heating makes temperature of charge reach 150 ~ 175 ℃, then adds 105 ℃ of hard coal-tar pitch wedding agents of softening point temperature, is mixed together 2～50min;
(4) pressure ball
Adjust ball press linear pressure 0.4～1.2t/mm, control ball press roller rubber-insulated wire speed 0.5～2.5m/min;
Mix raw material, send into the ball press charging tank, under the condition that keeps 150 ~ 175 ℃ of temperature, the belted electronic balance below the ball press charging tank is to the ball press continuous dosing of very;
Suppress oval base substrate size Φ 36 * 28 * 22, the base substrate after pressure ball sieves by grate, grid section pitch-row 12mm, and minus mesh turns back to mixing machine and reheats mixing, and oversize is charcoal element intermediate;
(5) charcoal element intermediate feature
Charcoal element intermediate after pressure ball, for independence, separation, monomer ball and two disjunctor balls that connect together more than ball exist simultaneously, coal-tar pitch content 12%; Volume density 〉=1.68g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 8%, and the internal porosity rate is less than 20%; Has anisotropisation carbonaceous characteristic.
4. employing ball press technique according to claim 1 is produced the method for charcoal element intermediate, it is characterized in that: graphitized electrode with the production method of charcoal element intermediate is:
(1), material choice: adopt graphitized electrode to produce and use after-smithing petroleum coke; The graphitized electrode moulding base (containing 23% coal-tar pitch wedding agent) that gives up; The graphitized electrode anode scrap; Natural flake graphite is raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate according to the mass fraction grain composition material+wedding agent=100%;
Grain composition: adopt low-cost grain composition method;
35～0mm after-smithing petroleum coke 62%;
35～0mm graphitized electrode moulding base (containing 23% coal-tar pitch wedding agent) 10% that gives up;
2～0mm natural flake graphite 3%;
0.1～0mm graphitized electrode anode scrap powder 3%;
0.1～0mm after-smithing petroleum coke powder 12%;
Wedding agent is selected:
Selecting 110 ℃ of hard coal-tar pitch of softening point temperature is wedding agent;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled at 10%;
(3) mix
Adopt hot hybrid mode, the material after grain composition is dropped in mixing machine, heating makes temperature of charge reach 160 ~ 185 ℃, then adds 110 ℃ of hard coal-tar pitch wedding agents of softening point temperature, is mixed together 5～60min;
(4) pressure ball
Adjust ball press linear pressure 0.4～1.2t t/mm, control ball press roller rubber-insulated wire speed 0.5～3.5m/min;
The raw material that mixes is sent into the ball press charging tank, and under the condition that keeps 160 ~ 185 ℃ of temperature, the belted electronic balance below the ball press charging tank or other feeding device are to the ball press continuous dosing of very;
Suppress oval base substrate size Φ 32 * 25 * 18, the base substrate after pressure ball sieves by grate, grid section pitch-row 10mm, and the minus mesh insulation turns back to the ball press charging tank and continues pressure ball, and oversize is charcoal element intermediate;
(5) charcoal element intermediate feature
Charcoal element intermediate after pressure ball, for independence, separation, monomer ball and two disjunctor balls that connect together more than ball exist simultaneously, coal-tar pitch content 12.3%; Volume density 〉=1.70g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 7%, and the internal porosity rate is less than 18%; Has anisotropisation carbonaceous characteristic.
5. employing ball press technique according to claim 1 is produced the method for charcoal element intermediate, it is characterized in that: low conduction charcoal element intermediate production method is
(1), material choice: adopt after-smithing petroleum coke; Pitch coke; Electric forging coal; Or metallurgical coke is raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate according to the mass fraction grain composition material+wedding agent=100%;
Grain composition: adopt low-cost grain composition method;
30～0mm after-smithing petroleum coke 25%;
30～0mm pitch coke 40%;
3～0mm electric forging coal 12%;
0.1～0mm pitch coke or metallurgical coke powder 15%;
Wedding agent is selected:
Selecting the heat-reactive phenolic resin of fixed carbon 70% is wedding agent;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled at 8%;
(3) mix
Adopt the heating hybrid mode, the material after grain composition is dropped in mixing machine, make temperature of charge reach 50 ~ 70 ℃, then add the heat-reactive phenolic resin wedding agent of fixed carbon 70%, be mixed together 10～60min;
(4) pressure ball
Adjust ball press linear pressure 0.5～1.5t/mm, control ball press roller rubber-insulated wire speed 0.5～4.0m/min;
The raw material that mixes is sent into the ball press charging tank, and under the condition that keeps 50 ~ 70 ℃ of temperature, the belted electronic balance below the ball press charging tank or other feeding machine are to the ball press continuous dosing of very;
Suppress spherical base substrate size Φ 30, the base substrate after pressure ball sieves by grate, grid section pitch-row 15mm, and the minus mesh insulation turns back to the ball press charging tank and continues pressure ball, and oversize is charcoal element intermediate;
Charcoal element intermediate is under 150 ~ 200 ℃ of temperature condition, and insulation greater than 48h, just becomes the formed coke charcoal continuously;
(5) charcoal element intermediate feature
After pressure ball, charcoal element intermediate, be independence, separation, monomer ball; Volume density 〉=1.68g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 10%, and the internal porosity rate is less than 20%; Has anisotropisation carbonaceous characteristic.
6. employing ball press technique according to claim 1 is produced the method for charcoal element intermediate, it is characterized in that: high-density electrode with the production method of charcoal element intermediate is
(1), material choice: adopt the electrode after-smithing petroleum coke; Graphitized electrode waste product or anode scrap are raw material;
(2) grain composition, wedding agent selection, wedding agent add-on are controlled
Calculate according to the mass fraction grain composition material+wedding agent=100%;
Grain composition: adopt the carbon product grain composition method of producing;
10～5mm after-smithing petroleum coke 20%;
5～2mm after-smithing petroleum coke 25%;
2～0mm after-smithing petroleum coke 20%;
0.1～0mm after-smithing petroleum coke powder 20%;
0.1～0mm graphitized electrode waste product or anode scrap powder 2%;
Wedding agent is selected:
Selecting 108 ℃ of hard coal-tar pitch of softening point temperature is wedding agent;
The wedding agent add-on is controlled:
The wedding agent add-on is controlled at 13%;
(3) kneading
Adopt hot kneading mode, the material after grain composition is dropped in kneading machine, heating makes temperature of charge reach 155 ~ 180 ℃, then adds softening point temperature 108 ℃ of hard coal-tar pitch wedding agents, kneading 5～60min together;
(4) pressure ball
Adjust ball press linear pressure 0.4～1.2t/mm, control ball press roller rubber-insulated wire speed 0.5～3.0m/min;
The raw material that kneading is good is sent into the ball press charging tank, and under the condition that keeps 155 ~ 180 ℃ of temperature, the belted electronic balance below the ball press charging tank or other feeding machine are to the ball press continuous dosing of very;
Suppress oval base substrate size Φ 32 * 25 * 20, the base substrate after pressure ball sieves by grate, grid section pitch-row 12mm, and minus mesh turns back to mixing machine and reheats mixing, and oversize is charcoal element intermediate;
(5) charcoal element intermediate feature
Charcoal element intermediate after pressure ball, for independence, separation, monomer ball and two disjunctor balls that connect together more than ball exist simultaneously, coal-tar pitch content 13%; Volume density 〉=1.70g/cm
3The load face void content is less than pressurized vertical surface void content; Apparent porosity is less than 7%, and the internal porosity rate is less than 18%; Has anisotropisation carbonaceous characteristic.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647913A (en) * | 2020-05-22 | 2020-09-11 | 国家电投集团黄河上游水电开发有限责任公司 | Carbon high-density anode for aluminum |
| CN115521144A (en) * | 2022-08-17 | 2022-12-27 | 山东大学 | Prebaked anode using phenolic resin as adhesive and manufacturing method thereof |
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| WO1980001683A1 (en) * | 1979-02-09 | 1980-08-21 | Maruzen Petrochem Co Ltd | Process for producing high-density,high-strength carbon and graphite material |
| JPS5673612A (en) * | 1979-11-14 | 1981-06-18 | Hitachi Chem Co Ltd | Manufacture of carbon material |
| JPH0214877A (en) * | 1988-06-30 | 1990-01-18 | Hitachi Chem Co Ltd | Production of carbon material |
| CN101723353A (en) * | 2009-11-19 | 2010-06-09 | 任利华 | Production method of high density carbon coke |
| CN102963879A (en) * | 2008-08-27 | 2013-03-13 | 任利华 | Formed coke produced by ball pressing technology and production method thereof |
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2013
- 2013-03-21 CN CN201310090046.2A patent/CN103130208B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1980001683A1 (en) * | 1979-02-09 | 1980-08-21 | Maruzen Petrochem Co Ltd | Process for producing high-density,high-strength carbon and graphite material |
| JPS5673612A (en) * | 1979-11-14 | 1981-06-18 | Hitachi Chem Co Ltd | Manufacture of carbon material |
| JPH0214877A (en) * | 1988-06-30 | 1990-01-18 | Hitachi Chem Co Ltd | Production of carbon material |
| CN102963879A (en) * | 2008-08-27 | 2013-03-13 | 任利华 | Formed coke produced by ball pressing technology and production method thereof |
| CN101723353A (en) * | 2009-11-19 | 2010-06-09 | 任利华 | Production method of high density carbon coke |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647913A (en) * | 2020-05-22 | 2020-09-11 | 国家电投集团黄河上游水电开发有限责任公司 | Carbon high-density anode for aluminum |
| CN115521144A (en) * | 2022-08-17 | 2022-12-27 | 山东大学 | Prebaked anode using phenolic resin as adhesive and manufacturing method thereof |
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