US3761387A - Process for producing an electrode pitch which can be easily graphitized - Google Patents
Process for producing an electrode pitch which can be easily graphitized Download PDFInfo
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- US3761387A US3761387A US00199774A US3761387DA US3761387A US 3761387 A US3761387 A US 3761387A US 00199774 A US00199774 A US 00199774A US 3761387D A US3761387D A US 3761387DA US 3761387 A US3761387 A US 3761387A
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- pitch
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- oil
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- 238000000034 method Methods 0.000 title description 17
- 239000011347 resin Substances 0.000 abstract description 39
- 229920005989 resin Polymers 0.000 abstract description 39
- 239000000725 suspension Substances 0.000 abstract description 14
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 abstract description 12
- 239000011294 coal tar pitch Substances 0.000 abstract description 12
- 238000004821 distillation Methods 0.000 abstract description 10
- 238000009835 boiling Methods 0.000 abstract description 8
- 239000000706 filtrate Substances 0.000 abstract description 7
- 239000000047 product Substances 0.000 abstract description 7
- 239000002075 main ingredient Substances 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 3
- 239000011295 pitch Substances 0.000 description 50
- 239000003921 oil Substances 0.000 description 28
- 238000004939 coking Methods 0.000 description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 8
- 125000003118 aryl group Chemical group 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 7
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 239000000571 coke Substances 0.000 description 5
- QPUYECUOLPXSFR-UHFFFAOYSA-N 1-methylnaphthalene Chemical compound C1=CC=C2C(C)=CC=CC2=C1 QPUYECUOLPXSFR-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000011280 coal tar Substances 0.000 description 4
- 238000007701 flash-distillation Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QNLZIZAQLLYXTC-UHFFFAOYSA-N 1,2-dimethylnaphthalene Chemical compound C1=CC=CC2=C(C)C(C)=CC=C21 QNLZIZAQLLYXTC-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 208000001848 dysentery Diseases 0.000 description 2
- 239000002198 insoluble material Substances 0.000 description 2
- 230000008447 perception Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000011269 tar Substances 0.000 description 2
- 208000003251 Pruritus Diseases 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000003849 aromatic solvent Substances 0.000 description 1
- 239000011305 binder pitch Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000011883 electrode binding agent Substances 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 239000011312 pitch solution Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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
- C10C1/00—Working-up tar
- C10C1/005—Working-up tar by mixing two or more coaltar fractions
-
- 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
Definitions
- ABSTRACT OF THE DISCLOSURE Dissolving a coal tar pitch in an aromatic rich oil fraction containing naphthalene and its homologs as its main ingredients and having a boiling range of 200 to 300 C., in a weight ratio pitch to oil fraction of 1:1 to 1:4 to produce a suspension; separating the solid content from the suspension; distilling 01f said oil fraction from the filtrate at such a sump temperature and with such time of stay for the pitch forming the sump product of the distillation column that the content of fi-resins is increased without forming of additional a-resins.
- the object of the present invention is to provide a process for producing a pitch for electrodes which can be easily graphitized, as well as yield graphite electrodes having satisfactory mechanical strength.
- pitches having a high amount of a constituent of p-resins (defined as substances which are insoluble in benzene but are soluble in anthracene oil) form a strong framework of carbon during coking and-in addition to this-the B-resins-like the rat-resins, yield a high share to the coking residue of the pitch.
- p-resins defined as substances which are insoluble in benzene but are soluble in anthracene oil
- anthracene-oil has the disadvantage that its boiling range is extremely close to that of the pitch so that the exact separation of the solvent from the pitch solution is difficult; on the one hand, the solvent becomes pitchlike to a certain extent and on the other hand certain parts of it distill already off so that the pitch characteristics have changed after distilling off of the anthracene-oil in a uncontrolled manner.
- oil fractions with a boiling range of 200 to 300 C., preferably 220 to 250 C. containing naphthalene and its homologs as its main ingredients for separating the u-resins.
- these oil fractions may be used in comparatively low amounts, generally in a small excess and preferably in a ratio (pitchzoil fraction) of from 1:1 to 1:4, more preferably about 1:2.
- the suspension can easily be filtered and about of the undesired a-resins are separated off by the filtration.
- Particularly preferred oil fractions are those obtained from the residual oils of benzine pyrolysis to ethylene; such oil fractions have a lower viscosity than corresponding fractions from coal tar.
- the subject matter of this invention is a process for producing an electrode pitch which can be easily graphitized and is characterized by the following steps: A coal tar pitch is dissolved in an aromatic rich oil fraction of a boiling range of 200 to 300 C., preferably 220 to 250 C.
- the weight ratio of pitch to said oil fraction being from 1:1 to 1:4 preferably about 1:2; the resulting suspension is filtered in the heat or separated; theadded oil fraction is distilled off again at such a sump temperature and with such a time of stay for the pitch forming the sump product of the distillation column that the B-resin content in said pitch is increased without forming additional a-resins.
- the coal tar pitch used is a pitch obtained by continuous flash distillation of coking tars from the Ruhr-area the sump temperature at which the formation of [Si-resins occurs is 300 to 400 C. preferably 320 to 360 C., the time of stay is 0.25 to 5 hours preferably 1 to 2 hours.
- the B-resins of the charged pitch the portion of which lies generally between 15 and 20% may be increased by 25-50% or more to produce an easily graphitizable electrode pitch having a fl-resin content of more than 24%, e.g. about 26%.
- the coking residues of the obtained electrode pitches are higher than 50% (according to Conradson). On coking a firm carbon framework is obtained.
- Graphite electrodes manufactured from these pitches have in addition to good electrical and thermal properties a high mechanical strength.
- the present process can be applied also to thermally after-treated coal tar pitches which are used as electrode pitches for non-graphitized carbon electrodes e.g. for aluminiu m smelting.
- these pitches are treated according to the process of invention also up to 90% of the undesired a-resins are removed.
- the additional formation of fl-resins takes place in small amount only since in the case of these thermally treated electrode pitches the condensation process has already partially taken place.
- these pitches have before being subjected to the process of invention, already got a fi-resins content of more than 20% it is easy to obtain at the end electrode pitches containing more than 24% of Q-resins. It is true, of course, that a small decrease of the coking residue occurs.
- Example I 5000 parts by weight coal tar pitch obtained by continuous flash distillation, were dissolved in 10,000 parts by weight of a residual oil fraction, rich in aromatics of the benzine pyrolyse to ethylene and the suspension thus obtained at 80 C. to 100 C. sucked off over a vacuum filter.
- the coal tar pitch had the following characteristics:
- the oil fraction rich in aromatic had the following properties:
- Example II In a manner analogous to Example I, another coaltar pitch also prepared by continuous flash distillation was dissolved in the ratio 1:2 in the described oil fraction rich in aromatic, the resulting suspension was filtered and the oil distilled, so that a sump temperature of 320 C. was more than 2 hours maintained.
- the properties of the charged and of the pitch obtained in a yield of 83% were as follows:
- the amount of the anthracene-insoluble has been reduced by 90% and the amount of fi-resins more than 50% increased.
- Example III Special Pitch electrode charged pitch Softening point (K.-S.), 0.... 83. 0 84. 5 Benzolinsoluble, percent 25. 4 25. 6 Anthraceneoil-insoluble, percent. 9.1 1. 3 fi-Resins, percent 16. 3 24. 3 Coking residue (Conradson), percent 53. 9 53. 2
- This treatment reduced the content of substances insoluble in anthraceneoil by about 85% and increased the fi-resins content by 50%.
- Example IV As described in Example I a normal electrode pitch obtained by thermal aftertreatment of a coal tar pitch was dissolved in a aromatic rich oil-fraction in the weight ratio of 1:2 and the suspension thus obtained was filtered and the oil distilled off in a manner that the sump temperature was maintained at 360 C. for 2 hours.
- the properties of the charged pitch and the yield of 85 produced itch were:
- the pitch to solvent weight ratio being at least 1:1
- the filtration is carried out at 80-110 C.
- distillation is carried out at 0.13 atmospheres and reaches a final sump temperature of 320-360 C.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
DISSOLVING A COAL TAR PITCH IN AN AROMATIC RICH OIL FRACTION CONTAINING NAPHTHALENE AND ITS HOMOLOGS AS ITS MAIN INGREDIENTS AND HAVING A BOILING RNAGE OF 200 TO 300*C., IN A WEIGHT RATIO PITCH TO OIL FRACTION OF 1:1 TO 1:4 TO. PRODUCE A SUSPENSION; SEPARATING THE SOLID CONTENT FROM THE SUSPENSION; DISTILLING OFF SAID OIL FRACTION FROM THE FILTRATE AT SUCH A SUMP TEMPERATURE AND WITH SUCH TIME OF STAY FOR THE PITCH FORMING THE SUMP PRODUCT OF THE DISTILLATION COLUMN THAT THE CONTENT OF B-RESINS IS INCREASED WITHOUT FORMING OF ADDITIONAL A-RESINS.
Description
United States Patent 3,761,387 PROCESS FOR PRODUCING AN ELECTRODE PITCH WHICH CAN BE EASILY GRAPHITIZED Otto Wegener, Mulheim-Speldorf, Heinrich Louis, Duisburg-Hamborn, and Rudolf Oberkobusch and Gerd Collin, Duisburg-Meiderich, Germany, assignors to Rutgerswerke Aktiengesellschaft, Frankfurt am Main, Germany No Drawing. Filed Nov. 17, 1971, Ser. No. 199,774 Claims priority, application Germany, Nov. 30, 1970, P 20 58 751.3 Int. Cl. Cc 3/02 U.S. Cl. 208-45 7 Claims ABSTRACT OF THE DISCLOSURE Dissolving a coal tar pitch in an aromatic rich oil fraction containing naphthalene and its homologs as its main ingredients and having a boiling range of 200 to 300 C., in a weight ratio pitch to oil fraction of 1:1 to 1:4 to produce a suspension; separating the solid content from the suspension; distilling 01f said oil fraction from the filtrate at such a sump temperature and with such time of stay for the pitch forming the sump product of the distillation column that the content of fi-resins is increased without forming of additional a-resins.
BACKGROUND OF THE INVENTION Processes have been known to produce anisotropic,
easily graphitizable cokes which can be used for the production of graphite electrodes. However, according to the present state of the art, binding agents which are suitable for these cokes have not been known; following the production methods of easily graphitizable cokes, it could be concluded that, fundamentally, coal tar pitches having a low content of highest molecular, sootlike substances which are insoluble in quinoline and also insoluble in anthracene-oil, the so-called oz-resins can be easily graphitized. However, pitches of this type yield, according to the state of the art, in mixture with easily graphitizable cokes, graphite electrodes of low mechanical strength and high consumption. For this reason, the specifications of the graphite electrode producers require in the pitch used as binding agent, normally a relatively high minimum-content of or-resins. These or-resins cause namely during coking and graphitizing, the formation of a very strong framework of carbon and this means electrodes with satisfactory mechanical strength and low consumption.
The object of the present invention is to provide a process for producing a pitch for electrodes which can be easily graphitized, as well as yield graphite electrodes having satisfactory mechanical strength.
SUMMARY OF THE INVENTION The solution of this problem is based in part on the perception that pitches having a high amount of a constituent of p-resins (defined as substances which are insoluble in benzene but are soluble in anthracene oil) form a strong framework of carbon during coking and-in addition to this-the B-resins-like the rat-resins, yield a high share to the coking residue of the pitch. According to this perception it had to be the aim to remove the oc-l'BSil'lS from a pitch as far as possible quantitatively, and simultaneously to increase the amount of fi-resins, if possible.
By dissolving the pitch in quinoline or anthracene-oil, and filtering off the insoluble ingredients, the rot-resins will of course be quantitatively removed, but the amount of B-resins will not be increased. Filtration of a pitch suspension in these solvents is rather diflicult due to the high viscosity of the solvents. This is true particularly in the ice case of quinoline. Practically the solvents must be used in a large excess, in order to guarantee a technically good separation of the soluble and insoluble material at all. In addition anthracene-oil has the disadvantage that its boiling range is extremely close to that of the pitch so that the exact separation of the solvent from the pitch solution is difficult; on the one hand, the solvent becomes pitchlike to a certain extent and on the other hand certain parts of it distill already off so that the pitch characteristics have changed after distilling off of the anthracene-oil in a uncontrolled manner.
It has now been found advantageous to use instead of quinoline or anthracene-oil as solvents for the pitch an aromatic-rich oil fraction with a boiling range of 200 to 300 C., preferably 220 to 250 C. containing naphthalene and its homologs as its main ingredients for separating the u-resins. In view of their low viscosity and good coagulating action, these oil fractions may be used in comparatively low amounts, generally in a small excess and preferably in a ratio (pitchzoil fraction) of from 1:1 to 1:4, more preferably about 1:2. The suspension can easily be filtered and about of the undesired a-resins are separated off by the filtration. Particularly preferred oil fractions are those obtained from the residual oils of benzine pyrolysis to ethylene; such oil fractions have a lower viscosity than corresponding fractions from coal tar.
It has been futher found when using coal tar pitches produced by continuous flash distillation, that the desired fl-resins can be increased still further without forming of any additional a-resins if, during distilling oif again the solvent from the filtrate of the pitch suspension such a pressure is maintained that the pitch forming the sump product of the distillation column is maintained for a controlled period of time at a controlled sump temperature. The two controlled values--the sump temperature and the dwell timevary somewhat for pitches of different sources but they can be easily determined by simple laboratory tests. The sump temperature, therefore, must be high enough that tit-resins may be formed but it must not be so high that additional u-resins will be formed.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENT OF THE INVENTION Thus the subject matter of this invention is a process for producing an electrode pitch which can be easily graphitized and is characterized by the following steps: A coal tar pitch is dissolved in an aromatic rich oil fraction of a boiling range of 200 to 300 C., preferably 220 to 250 C. which contain as main ingredients naphthalene and its homologs to produce a suspension, the weight ratio of pitch to said oil fraction being from 1:1 to 1:4 preferably about 1:2; the resulting suspension is filtered in the heat or separated; theadded oil fraction is distilled off again at such a sump temperature and with such a time of stay for the pitch forming the sump product of the distillation column that the B-resin content in said pitch is increased without forming additional a-resins.
When the coal tar pitch used is a pitch obtained by continuous flash distillation of coking tars from the Ruhr-area the sump temperature at which the formation of [Si-resins occurs is 300 to 400 C. preferably 320 to 360 C., the time of stay is 0.25 to 5 hours preferably 1 to 2 hours. By the process of this invention the B-resins of the charged pitch the portion of which lies generally between 15 and 20% may be increased by 25-50% or more to produce an easily graphitizable electrode pitch having a fl-resin content of more than 24%, e.g. about 26%. The coking residues of the obtained electrode pitches are higher than 50% (according to Conradson). On coking a firm carbon framework is obtained. Graphite electrodes manufactured from these pitches have in addition to good electrical and thermal properties a high mechanical strength.
The present process can be applied also to thermally after-treated coal tar pitches which are used as electrode pitches for non-graphitized carbon electrodes e.g. for aluminiu m smelting. When these pitches are treated according to the process of invention also up to 90% of the undesired a-resins are removed. However the additional formation of fl-resins takes place in small amount only since in the case of these thermally treated electrode pitches the condensation process has already partially taken place. However as these pitches have before being subjected to the process of invention, already got a fi-resins content of more than 20% it is easy to obtain at the end electrode pitches containing more than 24% of Q-resins. It is true, of course, that a small decrease of the coking residue occurs.
The invention is further explained by the following nonlimiting examples:
Example I 5000 parts by weight coal tar pitch obtained by continuous flash distillation, were dissolved in 10,000 parts by weight of a residual oil fraction, rich in aromatics of the benzine pyrolyse to ethylene and the suspension thus obtained at 80 C. to 100 C. sucked off over a vacuum filter. The coal tar pitch had the following characteristics:
Softening point Kramer-Sarnow C '70 Benzol insoluble percent 27.3 Anthracene oil insoluble do 7.4 fl-resins do 19.9 Coking residue (Conradson) do 60.0
The oil fraction rich in aromatic had the following properties:
Density at 20 C. 1.008 Analysis by fractional distillation:
Start of boiling: C 226 10% C 228 50% C..- 234 90% C 247 Gaschromatogramm: Naphthalene percent 31 Methylnaphthalene do 41 Dimethylennaphthalene do 13 Diphenyl do 5 Other aromatic hydrocarbons do In the filtration step 1050 parts by weight filter-residue and 13,950 parts by weight filtrate were obtained. From the filtrate by distillation under a pressure of 100 torr, 9,650 parts by weight of oil were distilled off so, that in the sump of the distillation apparatus a final temperature of 350 C. was obtained. This temperature was more than 1 hour maintained in order to maintain a thermal aftercondensation. The special electrode-pitch (4,250 parts by weight corresponding 85% yield) had the following properties:
Softening point Kramer-Sarnow C 86 Benzol-insoluble percent 25.4 Anthracene oil-insoluble do 0.9 St-resins do 24.5 Coking residue according Conradson do 50.1
The comparison with the pitch used shows that due to the treatment according to the invention not only almost 90% of the anthracene-insoluble material-which hinders the graphitizingis removed, but at the same time the 8- resins content being essential for the solidity of the coke residue has been increased by almost 25%. The use of the special electrode-pitch made it possible to manufacture a graphite electrode having good electric and thermal properties and high mechanical strength.
Example II In a manner analogous to Example I, another coaltar pitch also prepared by continuous flash distillation was dissolved in the ratio 1:2 in the described oil fraction rich in aromatic, the resulting suspension was filtered and the oil distilled, so that a sump temperature of 320 C. was more than 2 hours maintained. The properties of the charged and of the pitch obtained in a yield of 83% were as follows:
Special Pitch electrode charged pitch Softening point (K.-S.), C 75.5 90 Benzol-insoluble, percent 25. 1 2G. 8 Anthraceneoil-insoluble, percent 8. 1 0.8 B-Resins, percent 17.0 26. 0 Coking residue (Conradson), percen 50. 8 53. 0
Thus, due to this treatment, the amount of the anthracene-insoluble has been reduced by 90% and the amount of fi-resins more than 50% increased.
Example III Special Pitch electrode charged pitch Softening point (K.-S.), 0.... 83. 0 84. 5 Benzolinsoluble, percent 25. 4 25. 6 Anthraceneoil-insoluble, percent. 9.1 1. 3 fi-Resins, percent 16. 3 24. 3 Coking residue (Conradson), percent 53. 9 53. 2
This treatment reduced the content of substances insoluble in anthraceneoil by about 85% and increased the fi-resins content by 50%.
Example IV As described in Example I a normal electrode pitch obtained by thermal aftertreatment of a coal tar pitch was dissolved in a aromatic rich oil-fraction in the weight ratio of 1:2 and the suspension thus obtained was filtered and the oil distilled off in a manner that the sump temperature was maintained at 360 C. for 2 hours. The properties of the charged pitch and the yield of 85 produced itch were:
Charged Final pitch product Softening point (K.-S.), C 85 80 Benzol insoluble, percent 32. 7 26. 4 Anthraceneoil-insoluble, percent 10. 5 1. 2 fi-Resins, percent 22. 2 25. 2 Coking residue (Conradson), percent. 54. 1 5 1 By the treatment of the already precondensed pitch, the anthraceneoil-insoluble material was by almost reduced, but the amount of [i-resins was increased only by 14%.
What is claimed is: 1. Process for producing an electrode binder pitch in high yield from coal tar pitch starting material, which binder pitch can be easily graphitized comprising the steps of heating and dissolving the coal tar pitch in an aromatic solvent comprising as main ingredients one or more n-methylnaphthalene materials where n is from Zero to 3 and having a boiling range of 200 to 300 C.,
the pitch to solvent weight ratio being at least 1:1
and no greater than 1:4,
to produce a suspension,
hot filtering the solid content from said suspension to produce a filtrate of reduced alpha-resin content compared to the starting pitch,
distilling olf said oil fraction from the filtrate at subatmospheric pressure in a distillation column,
and treating distillation sump product of the distillation column at such a sump temperature and with such a time of stay that the amount of beta-resins in the sump product is increased without formation of additional alpha-resins therein.
2. Process according to claim in which said aromatic rich oil fraction has a boiling range of 220 to 250 C.
3. Process according to claim 1 in which the said coal tar pitch is dissolved in the said aromatic rich oil fraction in a weight ratio of 1:2.
4. Process in accordance with claim 3 wherein the oil comprises 31% naphthalene, 41% methylnaphthalene and 13% dimethylnaphthalene,
the filtration is carried out at 80-110 C.,
the distillation is carried out at 0.13 atmospheres and reaches a final sump temperature of 320-360 C., and
wherein the final sump temperature is maintained for 1-2 hours.
5. Process in accordance with claim 4 wherein the final sump temperature is 350 C. and is held for one hour.
6. Process according to claim 1 in which coal tar pitch of the coking tars from the Ruhr-area are used and the sump temperature is maintained from 300-400 C., with a time of stay for the pitch of 0.25 to 5 hours.
7. The process of claim 6 wherein the stay time is 1-2 hours and the sump temperature is maintained from 320- 60 C.
References Cited UNITED STATES PATENTS 3,558,468 1/1971 Wise 208-8 1,722,872 7/ 1929 Weindel 20845 3,490,586 1/1970 Jaisle 208-45 3,147,205 9/1964 Ohsol 208-45 FOREIGN PATENTS 1,080,866 8/ 1967 Great Britain 20844 DELBERT E. GANTZ, Primary Examiner V. OKEEFE, Assistant Examiner
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19702058751 DE2058751A1 (en) | 1970-11-30 | 1970-11-30 | Process for the production of an easily graphitizable electrode pitch |
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US3761387A true US3761387A (en) | 1973-09-25 |
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Application Number | Title | Priority Date | Filing Date |
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US00199774A Expired - Lifetime US3761387A (en) | 1970-11-30 | 1971-11-17 | Process for producing an electrode pitch which can be easily graphitized |
Country Status (6)
Country | Link |
---|---|
US (1) | US3761387A (en) |
DE (1) | DE2058751A1 (en) |
ES (1) | ES395371A1 (en) |
FR (1) | FR2116183A5 (en) |
GB (1) | GB1357159A (en) |
NL (1) | NL171466C (en) |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3995014A (en) * | 1973-12-11 | 1976-11-30 | Union Carbide Corporation | Process for producing carbon fibers from mesophase pitch |
US4026788A (en) * | 1973-12-11 | 1977-05-31 | Union Carbide Corporation | Process for producing mesophase pitch |
US4032430A (en) * | 1973-12-11 | 1977-06-28 | Union Carbide Corporation | Process for producing carbon fibers from mesophase pitch |
US4089934A (en) * | 1974-12-28 | 1978-05-16 | Mitsubishi Chemical Industries Ltd. | Process for preparing carbon products |
US4405439A (en) * | 1979-07-25 | 1983-09-20 | The Lummus Company | Removal of quinoline insolubles from coal derived fractions |
US4517072A (en) * | 1981-05-18 | 1985-05-14 | Domtar Inc. | Process for modifying coal tar materials |
US4755278A (en) * | 1986-02-26 | 1988-07-05 | Institut Francais Du Petrole | Process for fractionating solid asphalts |
US4758326A (en) * | 1984-10-05 | 1988-07-19 | Kawasaki Steel Corporation | Method of producing precursor pitches for carbon fibers |
US9511663B2 (en) | 2013-05-29 | 2016-12-06 | Mcalister Technologies, Llc | Methods for fuel tank recycling and net hydrogen fuel and carbon goods production along with associated apparatus and systems |
US9534296B2 (en) | 2013-03-15 | 2017-01-03 | Mcalister Technologies, Llc | Methods of manufacture of engineered materials and devices |
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1970
- 1970-11-30 DE DE19702058751 patent/DE2058751A1/en active Pending
-
1971
- 1971-09-23 ES ES395371A patent/ES395371A1/en not_active Expired
- 1971-09-27 NL NLAANVRAGE7113231,A patent/NL171466C/en not_active IP Right Cessation
- 1971-11-08 GB GB5178971A patent/GB1357159A/en not_active Expired
- 1971-11-17 US US00199774A patent/US3761387A/en not_active Expired - Lifetime
- 1971-11-30 FR FR7142943A patent/FR2116183A5/fr not_active Expired
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3995014A (en) * | 1973-12-11 | 1976-11-30 | Union Carbide Corporation | Process for producing carbon fibers from mesophase pitch |
US4026788A (en) * | 1973-12-11 | 1977-05-31 | Union Carbide Corporation | Process for producing mesophase pitch |
US4032430A (en) * | 1973-12-11 | 1977-06-28 | Union Carbide Corporation | Process for producing carbon fibers from mesophase pitch |
US4089934A (en) * | 1974-12-28 | 1978-05-16 | Mitsubishi Chemical Industries Ltd. | Process for preparing carbon products |
US4405439A (en) * | 1979-07-25 | 1983-09-20 | The Lummus Company | Removal of quinoline insolubles from coal derived fractions |
US4517072A (en) * | 1981-05-18 | 1985-05-14 | Domtar Inc. | Process for modifying coal tar materials |
US4758326A (en) * | 1984-10-05 | 1988-07-19 | Kawasaki Steel Corporation | Method of producing precursor pitches for carbon fibers |
US4755278A (en) * | 1986-02-26 | 1988-07-05 | Institut Francais Du Petrole | Process for fractionating solid asphalts |
US9534296B2 (en) | 2013-03-15 | 2017-01-03 | Mcalister Technologies, Llc | Methods of manufacture of engineered materials and devices |
US9511663B2 (en) | 2013-05-29 | 2016-12-06 | Mcalister Technologies, Llc | Methods for fuel tank recycling and net hydrogen fuel and carbon goods production along with associated apparatus and systems |
Also Published As
Publication number | Publication date |
---|---|
DE2058751A1 (en) | 1972-06-29 |
FR2116183A5 (en) | 1972-07-07 |
NL7113231A (en) | 1972-06-01 |
NL171466B (en) | 1982-11-01 |
GB1357159A (en) | 1974-06-19 |
ES395371A1 (en) | 1973-12-01 |
NL171466C (en) | 1983-04-05 |
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