CA1305591C - Binder for carbon and process for producing same - Google Patents
Binder for carbon and process for producing sameInfo
- Publication number
- CA1305591C CA1305591C CA 557508 CA557508A CA1305591C CA 1305591 C CA1305591 C CA 1305591C CA 557508 CA557508 CA 557508 CA 557508 A CA557508 A CA 557508A CA 1305591 C CA1305591 C CA 1305591C
- Authority
- CA
- Canada
- Prior art keywords
- binder
- precursor
- carbon
- boron oxide
- blnder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/023—Working-up pitch, asphalt, bitumen by chemical means reaction with inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/528—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 obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—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 obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Ceramic Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Civil Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Solid Fuels And Fuel-Associated Substances (AREA)
- Electrolytic Production Of Metals (AREA)
- Working-Up Tar And Pitch (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
A binder for carbon with reduced calcination is obtained by addition of approximately 0.1% by weight of B203 to the binder precursor from a coal tar distillation residue. The efficiency of the Inhibitor thus is approximately trebled as com-pared with the addition to the finished binder.
A binder for carbon with reduced calcination is obtained by addition of approximately 0.1% by weight of B203 to the binder precursor from a coal tar distillation residue. The efficiency of the Inhibitor thus is approximately trebled as com-pared with the addition to the finished binder.
Description
The present Inven~lon relates to a blnder based on coal tar, whlch has Improved propertles and Is Intended for carbon materlal. The present Inventlon also relates to a process for produclng sald blnder.
Carbon materlals for the productlon of carbon mouldlngs such as anodes, electrodes and ilnlngs conslst oF a mlxture of solId carbon such as anthraclte, pltch coke, petrol coke and car-bon black, and a carbon-petroleum-orlglnatlng bltumlnous blnder.
The materlals preferably contaln petrol co~e and coai tar pltch.
They are used prlmarlly for the productlon o~ precalclned or self-calclnlng (Soderberg) anodes for the alumlnlum electrolysls.
~ecause of the slde-reactlons (oxldatlon) and the anode decompo-: sltlon (sandlng) the consumptlon of anode materlals Is hlgher than Is requlred solely for the reductlon of the alumlnlum oxlde.
It Is known that speclflc Impurltles In both the cokeand the blnder, such as sodlum, calclum and vanadlum compounds, accelerate the oxldatlon and that the addltlons of boron and phosphorus compounds show Inhlbltlng effects (Llght Metals, 1982, ~ Page 713).
: ;:
:`
US-PS ~,188,279 Proposes the productlon of carbon mouldlngs from carbon materlals wlth 15 to 35% by welght of blnder and 0.1 to 3% by welght of boron compounds or 0.5 to 5% by welght of phosphorus compounds as oxldatlon Inhl b Itor, the Inhlbltor belng added to the homogenlzed mlxture or It Is admlxed wlth the blnder component prlor to the addltlon of the carbon materlal.
It Is also posslble to add all the three components i slmultaneously and to homogenlze them, as descrlbed In the Example. The calclnatlon Is reduced by 15% by an addltlon of 8%
by welght of borlc acld, relatlve to the coal-tar pltch blnder.
It has now been ~ound that the addltlon of borlc acld In the speclfled amounts causes the formatlon of VB and TB, whlch crystalllze out In the alumlnlum melt and, In the further pro-cesslng of the alumlnlum to form folls, they cause the formatlon of holes In the folls.
Phosphorus compounds, such as P205, also are less sult-able Inhlbltors slnce they reduce the current yleld In the elec-trolytlc process.
Therefore, the present Inventlon reduces the amount of Inhlbltors In the blnder and In the carbon whlle slmultaneously Improvlng thelr efflclency.
Accordlng to the present Inventlon, a blnder Is used whlch contalns maxlmally 0.3% by welght of boron oxlde and Is obtalned by addlng the boron oxlde to the blnder precursor and by subsequently further processlng the precursor to a carbon blnder.
Topped-off coal tar or dlstlllatlon residues of thls tar havlng a lower softenlng polnt than the blnder are used as blnder precursor. On addlng the boron oxlde (B203) the precursor Is processed to the deslred blnder by vacuum dlstlllatlon or/and carrler gas dlstlllatlon In one or several stages.
~ 25 A coal tar pltch Is preferably used as precursor so ; ~ that the processIng can be carrled out In one stage, for example, in an agltator retort or In a thln-fllm evaporator, under con-trolled condltlons.
In order to avold reduclng the reslstance of the blnder ~;~ to aglng, the dlstl~latlon should be carrled out at bottom tem--peratures of lower than 380C. Thls applles partlcularly to the productlon of blnders for Soderberg materlals. In the last dls-tlllatlon stage the maxlmal bottom temperature should not be below 350C slnce otherwlse an op~lmal homogenlzatlon wlll not be attalned.
Carbon materlals for the productlon of carbon mouldlngs such as anodes, electrodes and ilnlngs conslst oF a mlxture of solId carbon such as anthraclte, pltch coke, petrol coke and car-bon black, and a carbon-petroleum-orlglnatlng bltumlnous blnder.
The materlals preferably contaln petrol co~e and coai tar pltch.
They are used prlmarlly for the productlon o~ precalclned or self-calclnlng (Soderberg) anodes for the alumlnlum electrolysls.
~ecause of the slde-reactlons (oxldatlon) and the anode decompo-: sltlon (sandlng) the consumptlon of anode materlals Is hlgher than Is requlred solely for the reductlon of the alumlnlum oxlde.
It Is known that speclflc Impurltles In both the cokeand the blnder, such as sodlum, calclum and vanadlum compounds, accelerate the oxldatlon and that the addltlons of boron and phosphorus compounds show Inhlbltlng effects (Llght Metals, 1982, ~ Page 713).
: ;:
:`
US-PS ~,188,279 Proposes the productlon of carbon mouldlngs from carbon materlals wlth 15 to 35% by welght of blnder and 0.1 to 3% by welght of boron compounds or 0.5 to 5% by welght of phosphorus compounds as oxldatlon Inhl b Itor, the Inhlbltor belng added to the homogenlzed mlxture or It Is admlxed wlth the blnder component prlor to the addltlon of the carbon materlal.
It Is also posslble to add all the three components i slmultaneously and to homogenlze them, as descrlbed In the Example. The calclnatlon Is reduced by 15% by an addltlon of 8%
by welght of borlc acld, relatlve to the coal-tar pltch blnder.
It has now been ~ound that the addltlon of borlc acld In the speclfled amounts causes the formatlon of VB and TB, whlch crystalllze out In the alumlnlum melt and, In the further pro-cesslng of the alumlnlum to form folls, they cause the formatlon of holes In the folls.
Phosphorus compounds, such as P205, also are less sult-able Inhlbltors slnce they reduce the current yleld In the elec-trolytlc process.
Therefore, the present Inventlon reduces the amount of Inhlbltors In the blnder and In the carbon whlle slmultaneously Improvlng thelr efflclency.
Accordlng to the present Inventlon, a blnder Is used whlch contalns maxlmally 0.3% by welght of boron oxlde and Is obtalned by addlng the boron oxlde to the blnder precursor and by subsequently further processlng the precursor to a carbon blnder.
Topped-off coal tar or dlstlllatlon residues of thls tar havlng a lower softenlng polnt than the blnder are used as blnder precursor. On addlng the boron oxlde (B203) the precursor Is processed to the deslred blnder by vacuum dlstlllatlon or/and carrler gas dlstlllatlon In one or several stages.
~ 25 A coal tar pltch Is preferably used as precursor so ; ~ that the processIng can be carrled out In one stage, for example, in an agltator retort or In a thln-fllm evaporator, under con-trolled condltlons.
In order to avold reduclng the reslstance of the blnder ~;~ to aglng, the dlstl~latlon should be carrled out at bottom tem--peratures of lower than 380C. Thls applles partlcularly to the productlon of blnders for Soderberg materlals. In the last dls-tlllatlon stage the maxlmal bottom temperature should not be below 350C slnce otherwlse an op~lmal homogenlzatlon wlll not be attalned.
:
5~
The boron oxlde content in the blnder Is In the range of 0.03 to 0 3% by welght, preferably at approxlmately 0.1% by welght. In thls range the addltlon of B~03 has no negatlve effect on the wettlng propertles of the blnder or on the coklng properties of pltch-coke mlxtures.
The present Inventlon wlll be further Illustrated by way of Example 1 and the Comparlson Examples 2 and 3 hereafter.
Example 1 1000 parts by welght of a normal coal tar pltch, char-acterlzed by the analytlcal values llsted In Table 1, are melted down under an Inert gas, heated to 180C and then mlxed wlth 1 part by welght of B203 for 2 hours whlle stlrrlng. The mlxture Is then disillled In an agltator retort under a pressure of 100 mbars up to a bottom temperatwre of 360C. A blnder havlng the ; analytlcal data llsted In Table 2 Is thus obtalned wlth a yleld ~; Of 9~%.
~ 22 parts by welght of thls blnder are mlxed wlth 78 ;~ parts by welght of petroleum coi~e of defIned granulometry and then moulded to mouldlngs. The mouldlngs, calclned at 960C, are oxldlzed at 960C In a C02 current In order to measure the C02 z5 reactlvlty.
:~
The C02 reactlvlty Is a crlterlon of the anode consump-tlon In the alumlnlum electrolysls. The entlre calclnatlon Is composed of the dlrect calclnatlon and the dust formed, the lat-ter belng a ~unctlon of the granulometry of the petroleum col<e.
Furthermore, the denslty, the specl~lc electrlcal resistance and the bendlng strength of the test speclmens were determlned. The results have been llsted In Table 3.
5~
The boron oxlde content in the blnder Is In the range of 0.03 to 0 3% by welght, preferably at approxlmately 0.1% by welght. In thls range the addltlon of B~03 has no negatlve effect on the wettlng propertles of the blnder or on the coklng properties of pltch-coke mlxtures.
The present Inventlon wlll be further Illustrated by way of Example 1 and the Comparlson Examples 2 and 3 hereafter.
Example 1 1000 parts by welght of a normal coal tar pltch, char-acterlzed by the analytlcal values llsted In Table 1, are melted down under an Inert gas, heated to 180C and then mlxed wlth 1 part by welght of B203 for 2 hours whlle stlrrlng. The mlxture Is then disillled In an agltator retort under a pressure of 100 mbars up to a bottom temperatwre of 360C. A blnder havlng the ; analytlcal data llsted In Table 2 Is thus obtalned wlth a yleld ~; Of 9~%.
~ 22 parts by welght of thls blnder are mlxed wlth 78 ;~ parts by welght of petroleum coi~e of defIned granulometry and then moulded to mouldlngs. The mouldlngs, calclned at 960C, are oxldlzed at 960C In a C02 current In order to measure the C02 z5 reactlvlty.
:~
The C02 reactlvlty Is a crlterlon of the anode consump-tlon In the alumlnlum electrolysls. The entlre calclnatlon Is composed of the dlrect calclnatlon and the dust formed, the lat-ter belng a ~unctlon of the granulometry of the petroleum col<e.
Furthermore, the denslty, the specl~lc electrlcal resistance and the bendlng strength of the test speclmens were determlned. The results have been llsted In Table 3.
Example 2 corresponds to Example 1, but the boron oxlde Is added to the blnder (cooled to 200C) only after the dlstilla-tlon. Thls does not affect the yleld oF blnder. The propertles of the blnder have been llsted In Table 2 and the results of mea-surements on the test specImens In Table 3.
Table 3 ~Com~arlson) Example 3 corresponds to Example 2 but wlthout the addltlon of B203. The analytlcal values of the blnder have been llsted In Table 2 and the results of measurements on t~e test speclmens In Table 3.
Tab ! e 1 Anal~tical Data of the 81nder Precursor 20 softenlng polnt (Kraemer-Sarnow) 68C
Insoluble In toluene (Tl)26.3% by welght Insoluble In qulnolIne (Ql)6.2% by welght coklng resldue (Alcan) 51.4% by welght ash formers 0. 23% by welght _ ~I
.
~35~
Table 2 Analytlcal Data of the B Inder _ ~ _ 3 softenlng polnt tK.-S.) (C) 95 94 95 TI (% by welght)30.~ 30.0 30.4 QI (% by wei~h~) 7.0 7.1 7.0 coklng resldue (Alcan) ~ ~ 6~hj~__________gg,~____ Tab!e 3 Values Measured on the Test SpecImen - -. .
~_~ ~_ _~
C2 r~actlvlty:
dlrect calclnatlon (mg/sq.cm h) 16.1 17.8 18.7 20 dust formed (mgtsq.cm h) 4.5 6.7 6.4 ; total calclnatlon (mg/sq.cm h) 19.6 23.5 26.1 denslty (kg/dm3)1.48 1.47 1.47 - speclflc electrlca~ resl-slstance ( ~ m) 68 67 67 bendlng strength ~
(1Q5 N/sq.m) 261 251 243 As the Tables 2 and 3 show the addltlon of the boron oxlde before or a~ter the dlstlllatlon ca~ser nelther a change of ; the analytlcal data of the blnder nor a chan~e of the electrlcal or mechanlcal propertles of the test speclmens produced there-from, wlthln the llmlts of accuracy of measurement.
~' _ ~ 5~
Thus, for an addltlon of B203 after the dlstlllatlon the entlre calclnatlon decreases by approxImately 7% by welght and In the addltlon before the dlstlllatlon accordlng to the pre-sent Inventlon It decreases by approxlmately 22% by welght. Both the dlrect calclnatlon and the formatlon of dust show slmllar results.
It has thus been shown that by the addltlon of boron oxlde to the blnder precursor, accordlng to the present Inven-tlon, rather than to the fInlshed blnder or to the carbon mate-rlal, Its Inhlbltlng effect can be Increased by a multlple. It Is thus posslble to reduce substantlally the consumptlon of anodes wlth small amounts of Inhlbltor that are tolerable for the alumlnlum Industry.
: 16 ~: ~ 25 : . `
: ~ :
~:~ 3~
.
~`~ - 6 -\
, ,
Table 3 ~Com~arlson) Example 3 corresponds to Example 2 but wlthout the addltlon of B203. The analytlcal values of the blnder have been llsted In Table 2 and the results of measurements on t~e test speclmens In Table 3.
Tab ! e 1 Anal~tical Data of the 81nder Precursor 20 softenlng polnt (Kraemer-Sarnow) 68C
Insoluble In toluene (Tl)26.3% by welght Insoluble In qulnolIne (Ql)6.2% by welght coklng resldue (Alcan) 51.4% by welght ash formers 0. 23% by welght _ ~I
.
~35~
Table 2 Analytlcal Data of the B Inder _ ~ _ 3 softenlng polnt tK.-S.) (C) 95 94 95 TI (% by welght)30.~ 30.0 30.4 QI (% by wei~h~) 7.0 7.1 7.0 coklng resldue (Alcan) ~ ~ 6~hj~__________gg,~____ Tab!e 3 Values Measured on the Test SpecImen - -. .
~_~ ~_ _~
C2 r~actlvlty:
dlrect calclnatlon (mg/sq.cm h) 16.1 17.8 18.7 20 dust formed (mgtsq.cm h) 4.5 6.7 6.4 ; total calclnatlon (mg/sq.cm h) 19.6 23.5 26.1 denslty (kg/dm3)1.48 1.47 1.47 - speclflc electrlca~ resl-slstance ( ~ m) 68 67 67 bendlng strength ~
(1Q5 N/sq.m) 261 251 243 As the Tables 2 and 3 show the addltlon of the boron oxlde before or a~ter the dlstlllatlon ca~ser nelther a change of ; the analytlcal data of the blnder nor a chan~e of the electrlcal or mechanlcal propertles of the test speclmens produced there-from, wlthln the llmlts of accuracy of measurement.
~' _ ~ 5~
Thus, for an addltlon of B203 after the dlstlllatlon the entlre calclnatlon decreases by approxImately 7% by welght and In the addltlon before the dlstlllatlon accordlng to the pre-sent Inventlon It decreases by approxlmately 22% by welght. Both the dlrect calclnatlon and the formatlon of dust show slmllar results.
It has thus been shown that by the addltlon of boron oxlde to the blnder precursor, accordlng to the present Inven-tlon, rather than to the fInlshed blnder or to the carbon mate-rlal, Its Inhlbltlng effect can be Increased by a multlple. It Is thus posslble to reduce substantlally the consumptlon of anodes wlth small amounts of Inhlbltor that are tolerable for the alumlnlum Industry.
: 16 ~: ~ 25 : . `
: ~ :
~:~ 3~
.
~`~ - 6 -\
, ,
Claims (7)
1. A binder for carbon based on coal tar with additions of boron oxide as oxidation inhibitor, in which the binder maximally contains 0.3% by weight of boron oxide and is obtained by adding the boron oxide to a precursor of the binder and by subsequently further processing the precursor to the carbon binder, the precursor of the binder being selected from topped-off coal tar or its distillation residues having a lower softening point than the binder.
2. A binder as in claim 1, wherein the precursor is a distillation residue of coal tar.
3. A binder as in claim 2, in which the precursor is a normal coal tar pitch.
4. A binder as in claim 1, 2 or 3, which contains 0.03 to 0.3% by weight of boron oxide.
5. A binder as in claim 1, 2 or 3, which contains approximately 0.1% by weight of boron oxide.
6. A process for producing the binder as in claim 1, wherein the boron oxide is mixed with the precursor in liquid form and the mixture is further processed to the carbon binder by at least one of vacuum distillation and carrier gas distillation in one or several stages, wherein the maximal bottom temperature in the last distillation stage is above 200°C.
7. A process as in claim 6, wherein the maximal bottom temperature is the last distillation stage is in the range of 350 to 380°C.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEP3702950.9 | 1987-01-31 | ||
| DE19873702950 DE3702950A1 (en) | 1987-01-31 | 1987-01-31 | BINDING AGENTS FOR CARBON MATERIALS AND METHOD FOR THE PRODUCTION THEREOF |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1305591C true CA1305591C (en) | 1992-07-28 |
Family
ID=6319982
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA 557508 Expired - Fee Related CA1305591C (en) | 1987-01-31 | 1988-01-27 | Binder for carbon and process for producing same |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP0277284B1 (en) |
| CA (1) | CA1305591C (en) |
| DE (2) | DE3702950A1 (en) |
| ES (1) | ES2002714T3 (en) |
| NO (1) | NO175375C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19534363A1 (en) * | 1995-09-15 | 1997-03-20 | Schunk Kohlenstofftechnik Gmbh | Additives for the production of boron-containing polyaromatic mesophase pitches, polyaromatic mesophases and carbons by liquid phase pyrolysis |
| CN112978725A (en) * | 2021-02-07 | 2021-06-18 | 大连宏光锂业股份有限公司 | Modified artificial graphite cathode material of power lithium ion battery and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1289081A (en) * | 1970-01-02 | 1972-09-13 | ||
| US4188279A (en) * | 1976-10-26 | 1980-02-12 | Mobil Oil Corporation | Shaped carbon articles |
| EP0163597A1 (en) * | 1984-04-27 | 1985-12-04 | Schweizerische Aluminium Ag | Process for diminution of the tendency towards oxidation at increased temperatures of carbon powders or of shaped carbon articles fabricated by using the afore-mentioned carbon powder |
-
1987
- 1987-01-31 DE DE19873702950 patent/DE3702950A1/en not_active Withdrawn
- 1987-10-31 EP EP19870116043 patent/EP0277284B1/en not_active Expired - Lifetime
- 1987-10-31 ES ES198787116043T patent/ES2002714T3/en not_active Expired - Lifetime
- 1987-10-31 DE DE8787116043T patent/DE3775917D1/en not_active Expired - Fee Related
-
1988
- 1988-01-27 CA CA 557508 patent/CA1305591C/en not_active Expired - Fee Related
- 1988-01-29 NO NO880411A patent/NO175375C/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| ES2002714T3 (en) | 1993-07-16 |
| DE3775917D1 (en) | 1992-02-20 |
| NO880411D0 (en) | 1988-01-29 |
| ES2002714A4 (en) | 1988-10-01 |
| DE3702950A1 (en) | 1988-08-11 |
| EP0277284B1 (en) | 1992-01-08 |
| NO880411L (en) | 1988-08-01 |
| NO175375C (en) | 1994-10-05 |
| EP0277284A3 (en) | 1989-09-13 |
| NO175375B (en) | 1994-06-27 |
| EP0277284A2 (en) | 1988-08-10 |
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| MKLA | Lapsed |