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US4454019A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for producing optically anisotropic carbonaceous pitch

Assignee: Tonen General Sekiyu KK
•
Filing: 1982-01-11
•
Granted: 1984-06-12
•
Expires: 2002-01-11
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Abstract

Abstract A homogeneous, optically anisotropic pitch used for the production of carbon materials is prepared from a starting oil comprising a substantially chloroform-insoluble matter-free oily or tarry substance. The starting oil is subjected to thermal cracking and polycondensation to form approximately 20-80% of optically anisotropic phase pitch.

Inventors

  • 👤 Takayuki Izumi
  • 👤 Tsutomu Naito
  • 👤 Tomoo Nakamura
  • 👤 Hisao Tanaka

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-25 03:44
CPC Classifications
D; D01; D01F; D01F9/00; D01F9/08; D01F9/12; D01F9/14; D01F9/145; D01F9/15; C; C10; C10C; C10C3/00; C10C3/002

Claims Analysis

Total Claims: 44
Claim 1
Independent Claim 295 words
A process for producing a homogeneous, optically anisotropic carbonaceous pitch having a softening point in the range from about 230° C. to about 320° C. and an optically anisotropic phase content of about 90% to about 100% comprising: providing a carbonaceous material selected from oils and tars capable of forming a pitch when heated at elevated temperatures, said carbonaceous material having a boiling point in the range of about 250° C. to about 540° C. and being substantially free of chloroform and of n-heptane insoluble matter and containing a n-heptane-soluble material, said n-heptane-soluble material consisting essentially of an aromatic oil and resin, each of which has an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1000 and a maximum molecular weight of up to 2000; heating said carbonaceous material at a temperature in the range of about 380° C. to about 440° C. for a time sufficient to about 20% to about 80% of an optically anisotropic phase; maintaining said heated carbonaceous material at a temperature in the range from about 360° C. to about 380° C. for a time sufficient to form two layers, an upper layer containing a relatively low optically anisotropic phase content and a lower layer containing relatively high optically anisotropic phase content; separating said lower layer from said upper layer; thereafter heating said separated lower layer at a temperature in the range of 380° C. to about 440° C. for a time sufficient to increase the optically anisotropic phase content of said lower layer to at least 90% whereby a homogeneous optically anisotrophic carbonaceous pitch having a softening point in the range of about 230° C. to about 320° C. and an optically anisotropic phase content of about 90% to about 100% is obtained.
Claim 2
Dependent Claim 295 words
A process for producing a homogeneous, optically anisotropic carbonaceous pitch having a softening point in the range from about 230° C. to about 320° C. and an optically anisotropic phase content of about 90% to about 100% comprising: providing a carbonaceous material selected from oils and tars capable of forming a pitch when heated at elevated temperatures, said carbonaceous material having a boiling point in the range of about 250° C. to about 540° C. and being substantially free of chloroform and of n-heptane insoluble matter and containing a n-heptane-soluble material, said n-heptane-soluble material consisting essentially of an aromatic oil and resin, each of which has an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1000 and a maximum molecular weight of up to 2000; heating said carbonaceous material at a temperature in the range of about 380° C. to about 440° C. for a time sufficient to about 20% to about 80% of an optically anisotropic phase; maintaining said heated carbonaceous material at a temperature in the range from about 360° C. to about 380° C. for a time sufficient to form two layers, an upper layer containing a relatively low optically anisotropic phase content and a lower layer containing relatively high optically anisotropic phase content; separating said lower layer from said upper layer; thereafter heating said separated lower layer at a temperature in the range of 380° C. to about 440° C. for a time sufficient to increase the optically anisotropic phase content of said lower layer to at least 90% whereby a homogeneous optically anisotrophic carbonaceous pitch having a softening point in the range of about 230° C. to about 320° C. and an optically anisotropic phase content of about 90% to about 100% is obtained.
Claim 3
Dependent Claim 82 words
The process of claim 1 wherein said carbonaceous material is heated at temperatures in the range of 380° C. to 440° C. at pressures in the range of about 2 to about 50 kg/cm 2 until the optically anisotropic phase in said heated carbonaceous material is in the range of about 20% to 80% and thereafter said heated carbonaceous material is sparged with nitrogen for a time sufficient to remove components of the heated carbonaceous material which are volatile under sparging conditions.
Claim 4
Dependent Claim 24 words
The process according to claim 2, wherein the aromatic carbon fraction of each of the aromatic oil and resin components is at least 0.7.
Claim 5
Dependent Claim 30 words
The process according to claim 2, wherein the aromatic oil and resin have a number-average molecular weight of up to 750 and a maximum molecular weight of up to 1,500.
Claim 6
Dependent Claim 31 words
The process according to claim 3, wherein the aromatic oil and resin have a number-average molecular weight in the range of 250-750 and a maximum molecular weight of up to 1,500.
Claim 7
Dependent Claim 264 words
The process for producing a homogeneous, optically anisotropic carbonaceous pitch having a softening point in the range of about 230° C. to about 320° C. and an optically anisotropic phase content of about 90% to about 100% comprising: providing a carbonaceous material selected from oils and tars capable of forming a pitch when heated at elevated temperatures, said carbonaceous material being substantially free of chloroform insoluble materials, having up to 1 wt. % of asphaltene as a n-heptane insoluble component and including a mixture of compounds consisting mainly of carbon and hydrogen having a boiling point in the range of about 250° C. to about 540° C. and containing n-heptane-soluble components consisting essentially of an aromatic oil and resin, said aromatic oil and resin each having an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1000 and a maximum molecular weight of up to 2000; heating said carbonaceous material at temperatures in the range from about 380° C. to about 440° C. for a time sufficient to 20% to about 80% of an optically anisotrophic phase; maintaining said heated carbonaceous material at temperatures in the range from about 360° C. to about 380° C. for a time sufficient for said heated carbonaceous material to form an upper layer and a lower layer; separation said lower layer from said upper layer; and heating said lower layer at a temperature in the range from about 380° C. to about 440° C. for a time sufficient to increase the optical anisotropic phase content of said lower layer to at least 90%.
Claim 8
Dependent Claim 264 words
The process for producing a homogeneous, optically anisotropic carbonaceous pitch having a softening point in the range of about 230° C. to about 320° C. and an optically anisotropic phase content of about 90% to about 100% comprising: providing a carbonaceous material selected from oils and tars capable of forming a pitch when heated at elevated temperatures, said carbonaceous material being substantially free of chloroform insoluble materials, having up to 1 wt. % of asphaltene as a n-heptane insoluble component and including a mixture of compounds consisting mainly of carbon and hydrogen having a boiling point in the range of about 250° C. to about 540° C. and containing n-heptane-soluble components consisting essentially of an aromatic oil and resin, said aromatic oil and resin each having an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1000 and a maximum molecular weight of up to 2000; heating said carbonaceous material at temperatures in the range from about 380° C. to about 440° C. for a time sufficient to 20% to about 80% of an optically anisotrophic phase; maintaining said heated carbonaceous material at temperatures in the range from about 360° C. to about 380° C. for a time sufficient for said heated carbonaceous material to form an upper layer and a lower layer; separation said lower layer from said upper layer; and heating said lower layer at a temperature in the range from about 380° C. to about 440° C. for a time sufficient to increase the optical anisotropic phase content of said lower layer to at least 90%.
Claim 9
Dependent Claim 33 words
The process according to claim 6, wherein asphaltene has an aromatic carbon fraction of at least 0.6, number-average molecular weight of up to 1,000 and a maximum molecular weight of up to 2,000.
Claim 10
Dependent Claim 23 words
The process according to claim 7, wherein the aromatic oil, resin and asphaltene each have an aromatic carbon fraction of at least 0.7.
Claim 11
Dependent Claim 32 words
The process according to claim 7, wherein the aromatic oil, resin and asphaltene each have a number-average molecular weight of up to 750 and a maximum molecular weight of up to 1,500.
Claim 12
Dependent Claim 34 words
The process according to claim 9, wherein the aromatic oil, resin and asphaltene each have a number-average molecular weight in the approximate range of 250-750 and a maximum molecular weight of up to 1,500.
Claim 13
Dependent Claim 184 words
A homogeneous, optically anisotropic carbonaceous pitch having a softening point in the approximate range of 230°-320° C. and an optically anisotropic phase content of approximately 90-100%, and used for the production of carbon materials derived from a starting material comprising a substantially chloroform-insoluble matter-free oily or tarry substance including a mixture of compounds consisting mainly of carbon and hydrogen having a boiling point in the approximate range of 250°-540° C. and containing an aromatic oil and resin as the main n-heptane-soluble components, in which the aromatic oil and resin each have an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1000 and a maximum molecular weight of up to 2000 wherein said starting material is subjected to a thermal cracking and polycondensation reaction to form approximately 20-80% of optically anisotropic phase pitch and comprising the additional process steps of allowing the pitch to settle at a temperature of approximately 350°-400° C. in order to deposit an optically aniostropic phase in a bottom layer and separating said optically anisotropic phase from an upper layer containing an optically isotropic phase.
Claim 14
Dependent Claim 184 words
A homogeneous, optically anisotropic carbonaceous pitch having a softening point in the approximate range of 230°-320° C. and an optically anisotropic phase content of approximately 90-100%, and used for the production of carbon materials derived from a starting material comprising a substantially chloroform-insoluble matter-free oily or tarry substance including a mixture of compounds consisting mainly of carbon and hydrogen having a boiling point in the approximate range of 250°-540° C. and containing an aromatic oil and resin as the main n-heptane-soluble components, in which the aromatic oil and resin each have an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1000 and a maximum molecular weight of up to 2000 wherein said starting material is subjected to a thermal cracking and polycondensation reaction to form approximately 20-80% of optically anisotropic phase pitch and comprising the additional process steps of allowing the pitch to settle at a temperature of approximately 350°-400° C. in order to deposit an optically aniostropic phase in a bottom layer and separating said optically anisotropic phase from an upper layer containing an optically isotropic phase.
Claim 15
Dependent Claim 23 words
The optically anisotropic pitch of claim 11, wherein said aromatic oil and resin each have an aromatic carbon fraction of at least 0.7.
Claim 16
Dependent Claim 32 words
The optically anisotropic pitch of claim 11, wherein the aromatic oil and resin each have a number-average molecular weight of up to 750 and a maximum molecular weight of up to 1,500.
Claim 17
Dependent Claim 34 words
The optically anisotropic pitch of claim 13, wherein the aromatic oil and resin each have a number-average molecular weight in the approximate range of 250-750 and a maximum molecular weight of up to 1,500.
Claim 18
Dependent Claim 27 words
The optically anisotropic pitch of claim 11, wherein the thermal cracking and polycondensation reaction are carried out at a temperature in the approximate range of 380°-460° C.
Claim 19
Dependent Claim 197 words
A process for producing a homogeneous, optically anisotropic carbonaceous pitch having a softening point in the approximate range of 230°-320° C. and an optically anisotropic phase content of approximately 90-100%, and used for the production of carbon materials comprising the steps of: subjecting a starting material to a thermal cracking and polycondensation reaction to form approximately 20-80% of optically anisotropic phase pitch said starting material including a substantially chloroform-insoluble matter-free oily or tarry substance comprising a mixture of compounds consisting mainly of carbon and hydrogen having a boiling point in the approximate range of 250°-540° C. and containing an aromatic oil and resin as main n-heptane-soluble components, in which the aromatic oil and resin each have an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1,000 and a maximum molecular weight of up to 2,000; allowing said pitch to settle at a temperature of up to 400° C. to deposit an optically anisotropic phase in a bottom layer; separating said bottom layer from an upper layer containing optically isotropic phase; and heat-treating said bottom layer containing said optically anisotropic phase to obtain an optically anisotropic phase content of more than 90%.
Claim 20
Dependent Claim 197 words
A process for producing a homogeneous, optically anisotropic carbonaceous pitch having a softening point in the approximate range of 230°-320° C. and an optically anisotropic phase content of approximately 90-100%, and used for the production of carbon materials comprising the steps of: subjecting a starting material to a thermal cracking and polycondensation reaction to form approximately 20-80% of optically anisotropic phase pitch said starting material including a substantially chloroform-insoluble matter-free oily or tarry substance comprising a mixture of compounds consisting mainly of carbon and hydrogen having a boiling point in the approximate range of 250°-540° C. and containing an aromatic oil and resin as main n-heptane-soluble components, in which the aromatic oil and resin each have an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1,000 and a maximum molecular weight of up to 2,000; allowing said pitch to settle at a temperature of up to 400° C. to deposit an optically anisotropic phase in a bottom layer; separating said bottom layer from an upper layer containing optically isotropic phase; and heat-treating said bottom layer containing said optically anisotropic phase to obtain an optically anisotropic phase content of more than 90%.
Claim 21
Dependent Claim 40 words
The process according to claim 16, wherein said thermal decomposition and polycondensation reaction are carried out at a temperature of at least 380° C. and said heat treatment is carried out also at a temperature of at least 380° C.
Claim 22
Dependent Claim 26 words
The process according to claim 16, wherein said thermal decomposition and polycondensation reaction are carried out at a temperature in the approximate range of 400°-440° C.
Claim 23
Dependent Claim 32 words
The process according to claim 16, wherein said lower layer separates out at a temperature in the approximate range of 360°-380° C. and has an optically anisotropic phase content of about 70-90%.
Claim 24
Dependent Claim 17 words
The process according to claim 16, wherein said heat treatment is carried out at approximately 390°-440° C.
Claim 25
Dependent Claim 22 words
The process according to claim 16, wherein the aromatic oil and resin each have an aromatic carbon fraction of at least 0.7.
Claim 26
Dependent Claim 31 words
The process according to claim 16, wherein said aromatic oil and resin each have a number-average molecular weight of up to 750 and a maximum molecular weight of up to 1,500.
Claim 27
Dependent Claim 33 words
The process according to claim 21, wherein the aromatic oil and resin each have a number-average molecular weight in the approximate range of 250-750 and a maximum molecular weight of up to 1,500.
Claim 28
Dependent Claim 201 words
The process for producing a homogeneous, optically anisotropic carbonaceous pitch having a softening point in the approximate range of 230°-320° C. and an optically anisotropic phase content of approximately 90-100%, and used for the production of carbon materials using as a starting oil a substantially chloroform-insoluble matter-free oily or tarry substance comprising a mixture of compounds consisting mainly of carbon and hydrogen having a boiling point in the approximate range of 250°-540° C. and containing an aromatic oil and resin as n-heptane-soluble components and asphaltene as a n-heptane-insoluble component, in which the aromatic oil and resin each have an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1,000 and a maximum molecular weight of up to 2,000; the process comprising the steps of: subjecting said starting oil to a thermal cracking and polycondensation reaction to form approximately 20-80% of optically anisotropic phase pitch; allowing said pitch to settle at a temperature of approximately 350°-400° C. to deposit an optically anisotropic phase in a bottom layer; and separating said bottom layer from an upper layer containing an optically isotropic phase and heat-treating said bottom layer to obtain an optically anisotropic phase content of more than 90%.
Claim 29
Dependent Claim 201 words
The process for producing a homogeneous, optically anisotropic carbonaceous pitch having a softening point in the approximate range of 230°-320° C. and an optically anisotropic phase content of approximately 90-100%, and used for the production of carbon materials using as a starting oil a substantially chloroform-insoluble matter-free oily or tarry substance comprising a mixture of compounds consisting mainly of carbon and hydrogen having a boiling point in the approximate range of 250°-540° C. and containing an aromatic oil and resin as n-heptane-soluble components and asphaltene as a n-heptane-insoluble component, in which the aromatic oil and resin each have an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1,000 and a maximum molecular weight of up to 2,000; the process comprising the steps of: subjecting said starting oil to a thermal cracking and polycondensation reaction to form approximately 20-80% of optically anisotropic phase pitch; allowing said pitch to settle at a temperature of approximately 350°-400° C. to deposit an optically anisotropic phase in a bottom layer; and separating said bottom layer from an upper layer containing an optically isotropic phase and heat-treating said bottom layer to obtain an optically anisotropic phase content of more than 90%.
Claim 30
Dependent Claim 35 words
The process according to claim 24, wherein the asphaltene has an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1,000 and a maximum molecular weight of up to 2,000.
Claim 31
Dependent Claim 23 words
The process according to claim 24, wherein the aromatic oil, resin and asphaltene each have an aromatic carbon fraction of at least 0.7.
Claim 32
Dependent Claim 32 words
The process according to claim 24, wherein the aromatic oil, resin and asphaltene each have a number-average molecular weight of up to 750 and a maximum molecular weight of up to 1,500.
Claim 33
Dependent Claim 34 words
The process according to claim 27, wherein the aromatic oil, resin and asphaltene each have a number-average molecular weight in the approximate range of 250-750 and a maximum molecular weight of up to 1,500.
Claim 34
Dependent Claim 26 words
The process according to claim 24, wherein said thermal cracking and polycondensation reaction are carried out at a temperature in the approximate range of 380°-460° C.
Claim 35
Dependent Claim 203 words
The process for producing a homogeneous, optically anisotropic carbonaceous pitch having a softening point in the approximate range of 230°-320° C. and an optically anisotropic phase content of approximately 90-100%, and used for the production of carbon materials using as a starting oil a substantially chloroform-insoluble matter-free oily or tarry substance comprising a mixture of compounds consisting mainly of carbon and hydrogen having a boiling point in the approximate range of 250°-540° C., and containing an aromatic oil and resin as n-heptane-soluble components and asphaltene as a n-heptane-insoluble component, in which the aromatic oil and resin each have an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1,000 and a maximum molecular weight of up to 2,000; the process comprising the steps of: subjecting said starting material to a thermal cracking and polycondensation reaction to form approximately 20-80% of optically anisotropic phase pitch; allowing said pitch to settle at a temperature of up to 400° C. in order to deposit an optically anisotropic phase in a bottom layer; separating said bottom layer from said upper level containing an optically isotropic phase; and heat-treating said bottom layer to obtain an optically anisotropic phase content of more than 90%.
Claim 36
Dependent Claim 203 words
The process for producing a homogeneous, optically anisotropic carbonaceous pitch having a softening point in the approximate range of 230°-320° C. and an optically anisotropic phase content of approximately 90-100%, and used for the production of carbon materials using as a starting oil a substantially chloroform-insoluble matter-free oily or tarry substance comprising a mixture of compounds consisting mainly of carbon and hydrogen having a boiling point in the approximate range of 250°-540° C., and containing an aromatic oil and resin as n-heptane-soluble components and asphaltene as a n-heptane-insoluble component, in which the aromatic oil and resin each have an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1,000 and a maximum molecular weight of up to 2,000; the process comprising the steps of: subjecting said starting material to a thermal cracking and polycondensation reaction to form approximately 20-80% of optically anisotropic phase pitch; allowing said pitch to settle at a temperature of up to 400° C. in order to deposit an optically anisotropic phase in a bottom layer; separating said bottom layer from said upper level containing an optically isotropic phase; and heat-treating said bottom layer to obtain an optically anisotropic phase content of more than 90%.
Claim 37
Dependent Claim 40 words
The process according to claim 30, wherein said thermal cracking and polycondensation reaction are carried out at a temperature of at least 380° C. and said heat treatment is carried out also at a temperature of at least 380° C.
Claim 38
Dependent Claim 26 words
The process according to claim 30, wherein said thermal cracking and polycondensation reaction are carried out at a temperature in the approximate range of 400°-440° C.
Claim 39
Dependent Claim 31 words
The process according to claim 30, wherein the lower layer separated out at a temperature in the approximate range of 360°-380° C. having an optically anisotropic phase content of about 70-90%.
Claim 40
Dependent Claim 17 words
The process according to claim 30, wherein said heat treatment is carried out at approximately 390°-440° C.
Claim 41
Dependent Claim 35 words
The process according to claim 30, wherein the asphaltene has an aromatic carbon fraction of at least 0.6, a number-average molecular weight of up to 1,000 and a maximum molecular weight of up to 2,000.
Claim 42
Dependent Claim 23 words
The process according to claim 35, wherein said aromatic oil, resin and asphaltene each have an aromatic carbon fraction of at least 0.7.
Claim 43
Dependent Claim 32 words
The process according to claim 35, wherein the aromatic oil, resin and asphaltene each have a number-average molecular weight of up to 750 and a maximum molecular weight of up to 1,500.
Claim 44
Dependent Claim 34 words
The process according to claim 36, wherein the aromatic oil, resin and asphaltene each have a number-average molecular weight in the approximate range of 250-750 and a maximum molecular weight of up to 1,500.

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