CA1165095A - Process for manufacture of battery carbon black - Google Patents
Process for manufacture of battery carbon blackInfo
- Publication number
- CA1165095A CA1165095A CA000347118A CA347118A CA1165095A CA 1165095 A CA1165095 A CA 1165095A CA 000347118 A CA000347118 A CA 000347118A CA 347118 A CA347118 A CA 347118A CA 1165095 A CA1165095 A CA 1165095A
- Authority
- CA
- Canada
- Prior art keywords
- ranging
- carbon black
- millimicrons
- particle size
- size distribution
- 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
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
DLT:lw PROCESS FOR THE MANUFACTIJRE OF BATTERY CARBON BLACK
ABSTRACT
Furnace carbon black process useful for the production of a carbon black used as an ingredient in dry cell battery compositions is disclosed which comprises heating a carbon black feedstock having a DPB ranging from 200 to 250 cc/l00g and a particle size distribution ranging from 55 to 130 millimicrons to a temperature ranging from 1400°C to 2400°C under an inert atmos-phere, thereby producing a carbon black having a mean particle size distribution ranging from about 50 to about 120 millimicrons a dibutylphalate absorption (DBP) ranging from about 210 to about 270cc/l00g, a nitrogen surface area ranging from about 30 to about 60m2/g and an interplanar crystal lattice spacing (LC) ranging from about 2.7 to about 3.7 millimicrons.
ABSTRACT
Furnace carbon black process useful for the production of a carbon black used as an ingredient in dry cell battery compositions is disclosed which comprises heating a carbon black feedstock having a DPB ranging from 200 to 250 cc/l00g and a particle size distribution ranging from 55 to 130 millimicrons to a temperature ranging from 1400°C to 2400°C under an inert atmos-phere, thereby producing a carbon black having a mean particle size distribution ranging from about 50 to about 120 millimicrons a dibutylphalate absorption (DBP) ranging from about 210 to about 270cc/l00g, a nitrogen surface area ranging from about 30 to about 60m2/g and an interplanar crystal lattice spacing (LC) ranging from about 2.7 to about 3.7 millimicrons.
Description
5~2Z
~ I~LT: lw ~27/7~3 BA~CKGROUND OF THE INVENTION
The present invention pertains to the production o~
........ . .
carbon black and more particularly pertains to ~he productior} of carbon black which can be used as an ingredient in dry cell .........
battery compositions. It is well known that carbon blacks are . .. _ .
included in dry cell hattery compositions in order to ~npa increased electrolyte capacity, improved dischar~Fe ch~act~
istics, and other desirable properties to battery compositions. `---In the past, acetylene-type blacks were the carbon blacks choice for battery formulations since they imparted the best balance of properties to battery compositions which contain them.
Acetylene black is produced by decomposing the acetylene at - -temperatures higher than 2300C in an oxygen-con~aininy atmos-phere .
Prior art also includes W. V. Kotlensky and P. I..
Walker, Proceedings Fourth Conference for Carb~n" 1960, page 423, where it is disclosed that carbon blacks hav~ng mean par-ticle sizes ranging from about 10 to about 560 mill}microns and a `
DPB ranging from 35 to 65cc/lOOg is heated to temperatures ranging from 500 to 3000C in an inert atmosphere . An inner
~ I~LT: lw ~27/7~3 BA~CKGROUND OF THE INVENTION
The present invention pertains to the production o~
........ . .
carbon black and more particularly pertains to ~he productior} of carbon black which can be used as an ingredient in dry cell .........
battery compositions. It is well known that carbon blacks are . .. _ .
included in dry cell hattery compositions in order to ~npa increased electrolyte capacity, improved dischar~Fe ch~act~
istics, and other desirable properties to battery compositions. `---In the past, acetylene-type blacks were the carbon blacks choice for battery formulations since they imparted the best balance of properties to battery compositions which contain them.
Acetylene black is produced by decomposing the acetylene at - -temperatures higher than 2300C in an oxygen-con~aininy atmos-phere .
Prior art also includes W. V. Kotlensky and P. I..
Walker, Proceedings Fourth Conference for Carb~n" 1960, page 423, where it is disclosed that carbon blacks hav~ng mean par-ticle sizes ranging from about 10 to about 560 mill}microns and a `
DPB ranging from 35 to 65cc/lOOg is heated to temperatures ranging from 500 to 3000C in an inert atmosphere . An inner
2 ~, .
D:LT: Iw ~/~7/7 ~ S'~S I ' !
planar crystal spacing of between 12 and 42 mil~microns w~s .. -.-.-.-.. -.-... .-............
attained .
The prior art further includes U. S . Patent No. .-. ....... -. -.... ..
4,061,719 which discloses a process for the production of carbon .~
. .. :
....
black useful in dipolari2ation masses of dry cell batteries~ The -.. ----process includes the mixing of an aqueous suspension of a car~
:.-: -.-..-::.-. .
bon black having an absorption stiffness number higher than 15 . - .
, . .
and having been obtained by subjecting liquid hydrocarbons to .. -~ermal conversion at temperatures of 1200C to 2000C and .-`-. -. . - .-.-.-.-.....
pressures of 1 to 80 atmospheres in the presence of oxy~n- --.... .
containing gases, water scrubbing the resulting carbon black .. -containing reaction gas, mixing the resultant carbon-black-cont~ining .... ..
solution with 0 5 to 10g of a liquid vaporizable aliphatic or - --.... .
:.-: -::.-.-.-..-cycloaliphatic hydrocarbons per gram of carbon bla~k, sepalr~ting .. ` -. . ..
:,.: ... -.
the resulting carbon black from the liquid phase, heating the -,..... :
carbon black to free the black from the hydrocar~ons and the t'' ' ' water heating the black to 1100C to 2200C over a period of ~ ~
up to 30 minutes. The black produced by this process has a ... -.-....
nitrogen surface area of between 100 and 1000 square meters per ......
,..........
gram and a mean particle size of 25 to 65 microns, sic. ~-t is ~
:-:: ::..---believed that the mean particle size is 25 to 65 millimicrolls. .....
iSQ~5 ~ his invenkion provides a process for making a carbon black usef'ul as an in-gredient in dry cell battery composition which comprises: -a. heating, in an inert atmosphere, for a time period ranging from 9 to 21 seconds and at a rate of between about 100C/sec and 150C/sec, a carbon black ~eed-stock having a dibut~lphthalate absorption (DBP) ranging from 200 to 250cc/lOOg, a mean particle size distribution ranging from 55 to 130 millimicrons, a nitrogen s-urface area of between 30 and 60 m2/g, and a bimodal particle size distribution ranging from about 52 to 58 millimicrons and ~rom about 112 to 118 millimicrons, to a temp-erature ranging from 1400C to 2400C, and 4 _ 3L~6S(l ~
b. cooling said heated carbon black to a temperature below 325C in an inert atmosphere.
The process of this invention is useful for the production of a carbon black used as an ingredient in dry cell battery compositions.
The carbon black produced generally has a particle size distribution ranging from about 50 to about 120 millimicrons, a DBP of between about 210 and 270cc/lOOg, a nitrogen surface area between 30 and 60 meter /g and an interplanar crystal lattice spacing (Lc) between about 2.7 and 3.7 millimIcrons.
~l - 5 -a5 Preferably, the carbon blaek has a bimodal mean particle size distribution wherein the modes range from about 52 to 58 millimicrons and 112 to 118 millimierons, and a DBP of about 250ec/lOOg, and a nitrogen surfaee area of between 40 and 50 m /g.
A earbon blaek feedstock used i.n the process of thi.s invention has a partiele size distribution ranging from about 55 to 130 millimicrons and a DBP ranging from 200 to 250ce/lOOg.
Preferably the feedstock has a L of 1.1 to 1.2 millimierons and a pereent volatile eontent below about 3Ø More preferably the feedstock has a water eonten~ of below about 0.5~.
Though not restrieted thereto, a earbon black feed-stoek having sueh eharaeteristics can be produced in a vertical, eireular cross-seetion furnaee of the general type deseribed in United States Patent No. 2,779,665, by a proeess generally deseribed and illustrated in United States Patent No. 3~253,390.
The earbon black feedstoek produeed thereby is fed with inert earrier into a heating zone where it is heated to a temperature ranging from 1400C to 2400C.
DLT:lw 4/27~79 Suitable inert gases include nitrogen, helium and hydrogen w~th minimal concentrations of oxygen and water. - -Preferably, the carrier is nitrogen. : -~ .. ~ .
Preferably, the black is heated to about 2200~C at a rate between fOOC/second and 150C/second for a heating time ~~~
. . .:
ranging from 9 seconds to 21 seconds.
Since it is generally impossible to attain an ox~gen-~ree .-or water-free atmosphere and since the linings of hig~ tem~
perature furnaces are preferably constructed of graphite, a two zone heating furnace is preferred. In the initial zone, the black .- -is heated to a temperature in excess of 925C thereby cc nverting ---any oxygen present into CO, CO~ or S02. The zone is con~
-structed of a material such as RA-330 pipe. The heated carbon ~
black at a temperature between 565C to 760C is fed ~to the --graphite lined second zone and heated to 2200C. The abnosphere, --following the discharge of the black from the furnace and while --the black is at temperatures in excess of 315C is maintained free of oxygen and water so as to prevent oxidal:ion of the black. L'.'~
7 , --~s~
- DLT:lw ~/~7/7 With regards to the production of a suitable carbon black feedstock, it will be apparant to ~hose skilled in the art --~
that such properties as DBP and interplanar crystal lattice .. . .
spacing of the present carbon black products can be fully reg~
.. , _ .
lated over the limits of the claimed ranges by means of known techniques, e.g. crystal lattices can be regulated by v~g ~e heating rate within the heating furnace and the maximum tem~
perature attained by the carbon black. DBP can be regulated by introduction of alkali metal salts in varied amounts int~ the . . .
make oil feedstock. Surface area can be regulated by va~rying the flow rate of water into the furnace process a~d by regulation - -of temperature within the reaction chamber of the vertic~l furnace. - -The relatively low volatile content of t e feedstock carbon blacks - -of this invention is incidental to their surface characteristics and - -the high temperature at which they are formed and to which they are reheated.
In the following is set forth an example of the inven- ~
tion which is given hy way of illustration and ~ot limitation. ---The specific concentrations, tempera tures times, ratios, etc . set -. . . ,-.-forth in these examples are not to be construed to unduly limitthe scope of the invention.
DLT; lw 4/~7/79 EXAMPLE I . .
. -:.:....:.-..-.-....-..-50 grams/second of a carbon black feedstock exhibiting ... -.-.-....... ..
the following properties~
... . . -..
.. --Mean Particle Size Distribution,Millimicrons 55-1~5 ...........
._ ....
DBP, cc/lOOg 225 ---.
..
:.......
Surface Area,BET,m2/g 40 .. -.-.-Volatile Content ,% 6 . O . ~
.....
....... : -:-Oxygen Content,% 0.1 ,..................
:-:-,:-.-.- :.
L ,millimicrons 1.2 -:.-.-:.-.-.--.-c -.:.:--::.--:.-:
-.-. ..
were fed with a nitrogen carrier at velocity of 1 .~
,..........
meter/sec through a high temperature treating furnace measuring - --13 meters in length and 0.1 meters in diameter. A pressure of 1.1 atm was maintained and the carbon black was discharged at ~ .-. . ....
temperature of 1425C. ... ~
.;
: .... ... -.-.. :
The heat treated carbon black was a~owed to cool --... .......
under an inert atmosphere following recovery thereof and on-. :-:.--.--.:
.- .
. ...-.
testing was found to have the following properties~
..:::.-:....
Mean Particle Size Distribution,millimicrons 50-115 ...
, ~ .
DBP, cc/g 250 ~ .-t-,-.-.,-.--.-,:
g ~:''.',.':.
i"''''' 5~2~
DLT: Iw ~/27/79 ~"5~
Surface area,BET,m2/g 45 , ......................................................... :
Volatile Content,% 2.0 .. . . ..
L , millimicrons 2 . 8 -- ~
c , Iodine Number,cc/lOOg 62 .. ~
:.. -.. :
--.. -. -.- -ABC color 89 .~
, ...-.-.-... _ r.::..-:::::.-Tinting Strength, % of 60 r,.,.'''~'''-' Acetylene black, (Shawingen, Inc.) which ha~ pre- ~
.... ..
viously been the dry cell battery black of choice was uti~i2ed in -- -. . . .
preparation sf a standard dry cell battery composition. This ---.
acetylene black was characterized by the follow~ng prope~ties ~
.- .-: -.......
Particle size,millimicrons 42 .-.- .
. .
DBP, cc/100g 235 .
Surface Area,BET,m2/g 54 Lc,millimicrons 2. 58 - -A second dry cell battery composition was pre~ared .--::.
substituting the heat treated black of this Example in place of .... ....
the acetylene black. The compositions were identical exc~ept for ......
::::::::::
the carbon black constituent. . .
,... .
The properties of the two battery comp~sitions were ~ -.-.- .-.-.-..-tested using ANSI specification C18.1-1972 for Light In-te~mittent ~
~'.`.'-.'.',-,' 10r~
!
f 552Z
OLT: lw a,/z7/7g ~65~s Test (Lift) amperage output, and Heavy Intermittent Test ~Hift), initially and after 12 weeks at 45C. The following results for a 2D cells were found to be the following:
.....
Initial 12 wks @ 45C -~
..........
Acet Applicant's Acet hpplicant's --.-~
2.25 ohm Lift 100% 108% 100% 107% .... -2.25 ohm Cont. 100% 108% 100% 101% .-2.25 ohm HIFT 100% 107% 100% 109%
4 ohm LIFT 100% 110% 100% 113%
4 ohm HIFT 100% 110% 100% 104%
ohm 4H/D 105% 105% 100% 102%
.-.. - .. : .
It can thus be seen that the presently cla~med heat .. . =
treated black is found to impart superior properties t~ b~ttery compositions containing Applicant's black over compositions .
....-containing ace~ylene black. . .-. ~
Therefore, carbon black products have been developed which were heretofore unknown and unobvious in that they are .~
characterized by such a different combination of properties as . -,... ..
11 , .. ,... _ ` " ~LI':lw ~/Z7/7~
~;5~95 would have previously caused one skilled in the art to doubt . ...
that they could have utility. More particularly, these new blacks are different in being characterized by interplanar crystal .
, .. .
lattice spacing- ~
_=, ....
.. ....
.......
.....
12 ~ ~
D:LT: Iw ~/~7/7 ~ S'~S I ' !
planar crystal spacing of between 12 and 42 mil~microns w~s .. -.-.-.-.. -.-... .-............
attained .
The prior art further includes U. S . Patent No. .-. ....... -. -.... ..
4,061,719 which discloses a process for the production of carbon .~
. .. :
....
black useful in dipolari2ation masses of dry cell batteries~ The -.. ----process includes the mixing of an aqueous suspension of a car~
:.-: -.-..-::.-. .
bon black having an absorption stiffness number higher than 15 . - .
, . .
and having been obtained by subjecting liquid hydrocarbons to .. -~ermal conversion at temperatures of 1200C to 2000C and .-`-. -. . - .-.-.-.-.....
pressures of 1 to 80 atmospheres in the presence of oxy~n- --.... .
containing gases, water scrubbing the resulting carbon black .. -containing reaction gas, mixing the resultant carbon-black-cont~ining .... ..
solution with 0 5 to 10g of a liquid vaporizable aliphatic or - --.... .
:.-: -::.-.-.-..-cycloaliphatic hydrocarbons per gram of carbon bla~k, sepalr~ting .. ` -. . ..
:,.: ... -.
the resulting carbon black from the liquid phase, heating the -,..... :
carbon black to free the black from the hydrocar~ons and the t'' ' ' water heating the black to 1100C to 2200C over a period of ~ ~
up to 30 minutes. The black produced by this process has a ... -.-....
nitrogen surface area of between 100 and 1000 square meters per ......
,..........
gram and a mean particle size of 25 to 65 microns, sic. ~-t is ~
:-:: ::..---believed that the mean particle size is 25 to 65 millimicrolls. .....
iSQ~5 ~ his invenkion provides a process for making a carbon black usef'ul as an in-gredient in dry cell battery composition which comprises: -a. heating, in an inert atmosphere, for a time period ranging from 9 to 21 seconds and at a rate of between about 100C/sec and 150C/sec, a carbon black ~eed-stock having a dibut~lphthalate absorption (DBP) ranging from 200 to 250cc/lOOg, a mean particle size distribution ranging from 55 to 130 millimicrons, a nitrogen s-urface area of between 30 and 60 m2/g, and a bimodal particle size distribution ranging from about 52 to 58 millimicrons and ~rom about 112 to 118 millimicrons, to a temp-erature ranging from 1400C to 2400C, and 4 _ 3L~6S(l ~
b. cooling said heated carbon black to a temperature below 325C in an inert atmosphere.
The process of this invention is useful for the production of a carbon black used as an ingredient in dry cell battery compositions.
The carbon black produced generally has a particle size distribution ranging from about 50 to about 120 millimicrons, a DBP of between about 210 and 270cc/lOOg, a nitrogen surface area between 30 and 60 meter /g and an interplanar crystal lattice spacing (Lc) between about 2.7 and 3.7 millimIcrons.
~l - 5 -a5 Preferably, the carbon blaek has a bimodal mean particle size distribution wherein the modes range from about 52 to 58 millimicrons and 112 to 118 millimierons, and a DBP of about 250ec/lOOg, and a nitrogen surfaee area of between 40 and 50 m /g.
A earbon blaek feedstock used i.n the process of thi.s invention has a partiele size distribution ranging from about 55 to 130 millimicrons and a DBP ranging from 200 to 250ce/lOOg.
Preferably the feedstock has a L of 1.1 to 1.2 millimierons and a pereent volatile eontent below about 3Ø More preferably the feedstock has a water eonten~ of below about 0.5~.
Though not restrieted thereto, a earbon black feed-stoek having sueh eharaeteristics can be produced in a vertical, eireular cross-seetion furnaee of the general type deseribed in United States Patent No. 2,779,665, by a proeess generally deseribed and illustrated in United States Patent No. 3~253,390.
The earbon black feedstoek produeed thereby is fed with inert earrier into a heating zone where it is heated to a temperature ranging from 1400C to 2400C.
DLT:lw 4/27~79 Suitable inert gases include nitrogen, helium and hydrogen w~th minimal concentrations of oxygen and water. - -Preferably, the carrier is nitrogen. : -~ .. ~ .
Preferably, the black is heated to about 2200~C at a rate between fOOC/second and 150C/second for a heating time ~~~
. . .:
ranging from 9 seconds to 21 seconds.
Since it is generally impossible to attain an ox~gen-~ree .-or water-free atmosphere and since the linings of hig~ tem~
perature furnaces are preferably constructed of graphite, a two zone heating furnace is preferred. In the initial zone, the black .- -is heated to a temperature in excess of 925C thereby cc nverting ---any oxygen present into CO, CO~ or S02. The zone is con~
-structed of a material such as RA-330 pipe. The heated carbon ~
black at a temperature between 565C to 760C is fed ~to the --graphite lined second zone and heated to 2200C. The abnosphere, --following the discharge of the black from the furnace and while --the black is at temperatures in excess of 315C is maintained free of oxygen and water so as to prevent oxidal:ion of the black. L'.'~
7 , --~s~
- DLT:lw ~/~7/7 With regards to the production of a suitable carbon black feedstock, it will be apparant to ~hose skilled in the art --~
that such properties as DBP and interplanar crystal lattice .. . .
spacing of the present carbon black products can be fully reg~
.. , _ .
lated over the limits of the claimed ranges by means of known techniques, e.g. crystal lattices can be regulated by v~g ~e heating rate within the heating furnace and the maximum tem~
perature attained by the carbon black. DBP can be regulated by introduction of alkali metal salts in varied amounts int~ the . . .
make oil feedstock. Surface area can be regulated by va~rying the flow rate of water into the furnace process a~d by regulation - -of temperature within the reaction chamber of the vertic~l furnace. - -The relatively low volatile content of t e feedstock carbon blacks - -of this invention is incidental to their surface characteristics and - -the high temperature at which they are formed and to which they are reheated.
In the following is set forth an example of the inven- ~
tion which is given hy way of illustration and ~ot limitation. ---The specific concentrations, tempera tures times, ratios, etc . set -. . . ,-.-forth in these examples are not to be construed to unduly limitthe scope of the invention.
DLT; lw 4/~7/79 EXAMPLE I . .
. -:.:....:.-..-.-....-..-50 grams/second of a carbon black feedstock exhibiting ... -.-.-....... ..
the following properties~
... . . -..
.. --Mean Particle Size Distribution,Millimicrons 55-1~5 ...........
._ ....
DBP, cc/lOOg 225 ---.
..
:.......
Surface Area,BET,m2/g 40 .. -.-.-Volatile Content ,% 6 . O . ~
.....
....... : -:-Oxygen Content,% 0.1 ,..................
:-:-,:-.-.- :.
L ,millimicrons 1.2 -:.-.-:.-.-.--.-c -.:.:--::.--:.-:
-.-. ..
were fed with a nitrogen carrier at velocity of 1 .~
,..........
meter/sec through a high temperature treating furnace measuring - --13 meters in length and 0.1 meters in diameter. A pressure of 1.1 atm was maintained and the carbon black was discharged at ~ .-. . ....
temperature of 1425C. ... ~
.;
: .... ... -.-.. :
The heat treated carbon black was a~owed to cool --... .......
under an inert atmosphere following recovery thereof and on-. :-:.--.--.:
.- .
. ...-.
testing was found to have the following properties~
..:::.-:....
Mean Particle Size Distribution,millimicrons 50-115 ...
, ~ .
DBP, cc/g 250 ~ .-t-,-.-.,-.--.-,:
g ~:''.',.':.
i"''''' 5~2~
DLT: Iw ~/27/79 ~"5~
Surface area,BET,m2/g 45 , ......................................................... :
Volatile Content,% 2.0 .. . . ..
L , millimicrons 2 . 8 -- ~
c , Iodine Number,cc/lOOg 62 .. ~
:.. -.. :
--.. -. -.- -ABC color 89 .~
, ...-.-.-... _ r.::..-:::::.-Tinting Strength, % of 60 r,.,.'''~'''-' Acetylene black, (Shawingen, Inc.) which ha~ pre- ~
.... ..
viously been the dry cell battery black of choice was uti~i2ed in -- -. . . .
preparation sf a standard dry cell battery composition. This ---.
acetylene black was characterized by the follow~ng prope~ties ~
.- .-: -.......
Particle size,millimicrons 42 .-.- .
. .
DBP, cc/100g 235 .
Surface Area,BET,m2/g 54 Lc,millimicrons 2. 58 - -A second dry cell battery composition was pre~ared .--::.
substituting the heat treated black of this Example in place of .... ....
the acetylene black. The compositions were identical exc~ept for ......
::::::::::
the carbon black constituent. . .
,... .
The properties of the two battery comp~sitions were ~ -.-.- .-.-.-..-tested using ANSI specification C18.1-1972 for Light In-te~mittent ~
~'.`.'-.'.',-,' 10r~
!
f 552Z
OLT: lw a,/z7/7g ~65~s Test (Lift) amperage output, and Heavy Intermittent Test ~Hift), initially and after 12 weeks at 45C. The following results for a 2D cells were found to be the following:
.....
Initial 12 wks @ 45C -~
..........
Acet Applicant's Acet hpplicant's --.-~
2.25 ohm Lift 100% 108% 100% 107% .... -2.25 ohm Cont. 100% 108% 100% 101% .-2.25 ohm HIFT 100% 107% 100% 109%
4 ohm LIFT 100% 110% 100% 113%
4 ohm HIFT 100% 110% 100% 104%
ohm 4H/D 105% 105% 100% 102%
.-.. - .. : .
It can thus be seen that the presently cla~med heat .. . =
treated black is found to impart superior properties t~ b~ttery compositions containing Applicant's black over compositions .
....-containing ace~ylene black. . .-. ~
Therefore, carbon black products have been developed which were heretofore unknown and unobvious in that they are .~
characterized by such a different combination of properties as . -,... ..
11 , .. ,... _ ` " ~LI':lw ~/Z7/7~
~;5~95 would have previously caused one skilled in the art to doubt . ...
that they could have utility. More particularly, these new blacks are different in being characterized by interplanar crystal .
, .. .
lattice spacing- ~
_=, ....
.. ....
.......
.....
12 ~ ~
Claims (5)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process for making a carbon black useful as an ingredient in dry cell battery compositions which comprises:
a. heating, in an inert atmosphere, for a time period ranging from 9 to 21 seconds and at a rate of between about 100°c/sec and 150°C/sec, a carbon black feedstock having a dibutylphthalate absorption (DBP) ranging from 200 to 250cc/l00g, a mean particle size distribution ranging from 55 to 130 millimicrons, a nitrogen surface area of between 30 and 60m2/g, and a bimodal particle size distribution ranging from about 52 to 58 millimicrons and from about 112 to 118 millimicrons, to a temperature ranging from 1400°C to 2400°C, and b. cooling said heated carbon black to a temperature below 325°C in an inert atmosphere.
a. heating, in an inert atmosphere, for a time period ranging from 9 to 21 seconds and at a rate of between about 100°c/sec and 150°C/sec, a carbon black feedstock having a dibutylphthalate absorption (DBP) ranging from 200 to 250cc/l00g, a mean particle size distribution ranging from 55 to 130 millimicrons, a nitrogen surface area of between 30 and 60m2/g, and a bimodal particle size distribution ranging from about 52 to 58 millimicrons and from about 112 to 118 millimicrons, to a temperature ranging from 1400°C to 2400°C, and b. cooling said heated carbon black to a temperature below 325°C in an inert atmosphere.
2. The process of claim 1 wherein the carbon black is heated to about 2200°C.
3. A process of claim 1, wherein the resulting carbon black has a) a mean particle size distribution ranging from about 50 to about 120 millimicrons, b) a dibutylphthalate absorption (DBP) ranging from about 210 to about 270cc/l00g, c) a nitrogen surface area ranging from about 30 to about 60m2/g, and d) an interplanar crystal lattice spacing (Lc) ranging from about 2.7 to about 3.7 millimicrons.
4. A process of claim 3 wherein the carbon black feedstock has an interplanar crystal lattice spacing (Lc) ranging 1.1 to 1.2 millimicrons and a percent volatile content below about 3Ø
5. A process of claim 3 wherein the carbon black feed-stock is heated in nitroyen atmosphere.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US5236579A | 1979-06-27 | 1979-06-27 | |
US052,365 | 1979-06-27 |
Publications (1)
Publication Number | Publication Date |
---|---|
CA1165095A true CA1165095A (en) | 1984-04-10 |
Family
ID=21977142
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA000347118A Expired CA1165095A (en) | 1979-06-27 | 1980-03-06 | Process for manufacture of battery carbon black |
Country Status (5)
Country | Link |
---|---|
JP (1) | JPS568461A (en) |
BR (1) | BR8002311A (en) |
CA (1) | CA1165095A (en) |
DE (1) | DE3002555A1 (en) |
IT (1) | IT1130211B (en) |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS591572A (en) * | 1982-06-25 | 1984-01-06 | Asahi Carbon Kk | High-structure carbon black |
JPS5971367A (en) * | 1982-10-14 | 1984-04-23 | Asahi Carbon Kk | High-structure carbon black |
JPS59109562A (en) * | 1982-12-16 | 1984-06-25 | Denki Kagaku Kogyo Kk | Carbon black and electrically conductive composition containing the same |
JPS60190469A (en) * | 1984-03-13 | 1985-09-27 | Tokai Carbon Co Ltd | Production of conductive carbon black |
JP2889326B2 (en) * | 1989-09-14 | 1999-05-10 | 昭和キャボット株式会社 | Carbon black and rubber composition |
US5958623A (en) * | 1996-12-13 | 1999-09-28 | Kozawa; Akiya | Electrochemical cell employing a fine carbon additive |
-
1980
- 1980-01-08 IT IT19094/80A patent/IT1130211B/en active
- 1980-01-25 DE DE19803002555 patent/DE3002555A1/en not_active Ceased
- 1980-02-19 JP JP1861680A patent/JPS568461A/en active Pending
- 1980-03-06 CA CA000347118A patent/CA1165095A/en not_active Expired
- 1980-04-14 BR BR8002311A patent/BR8002311A/en unknown
Also Published As
Publication number | Publication date |
---|---|
IT8019094A0 (en) | 1980-01-08 |
JPS568461A (en) | 1981-01-28 |
IT1130211B (en) | 1986-06-11 |
BR8002311A (en) | 1981-11-24 |
DE3002555A1 (en) | 1981-01-08 |
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