US3775289A - Method for producing bituminous substance such as a coal tar pitch - Google Patents

Method for producing bituminous substance such as a coal tar pitch Download PDF

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Publication number
US3775289A
US3775289A US00196096A US3775289DA US3775289A US 3775289 A US3775289 A US 3775289A US 00196096 A US00196096 A US 00196096A US 3775289D A US3775289D A US 3775289DA US 3775289 A US3775289 A US 3775289A
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United States
Prior art keywords
pitch
oil
percent
coal tar
component
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Expired - Lifetime
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US00196096A
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English (en)
Inventor
C Kishi
M Tatsuta
M Nago
K Kibuishi
Y Hatakeyama
K Miyakawa
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Nippon Steel Corp
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Nippon Steel Corp
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Publication date
Priority claimed from JP45098979A external-priority patent/JPS4918451B1/ja
Priority claimed from JP45102970A external-priority patent/JPS4918769B1/ja
Application filed by Nippon Steel Corp filed Critical Nippon Steel Corp
Application granted granted Critical
Publication of US3775289A publication Critical patent/US3775289A/en
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    • 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
    • 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
    • C10C1/20—Refining by chemical means inorganic or organic compounds

Definitions

  • ABSTRACT A method for producing bituminous substance such as coal tar pitch which comprises adding sulfuric acid to coal tar produced by a high temperature dry distillation of coal and a bituminous substance produced from the coal tar, then adding petroleum heavy oil to the mixture to precipitate and separate pitch component.
  • bituminous substance such as pitch from coal tar
  • low boiling point aromatic components are removed by distillation or steaming, and if necessary polycondensation reaction is caused by a heating treatment or by blowing in the air to a certain desired degree, or distillated oil from creosote oil and the like is cut back to obtain bituminous substance of desired properties (viscosity and softening point).
  • air blowing-in or the addition of sulfur can promote the poly-condensation and increase benzole-insoluble component, these measures are nothing more than auxiliary means for the heating treatment since they are effective only under a heated condition between 300 to 400C due to their reaction temperature.
  • waste sulfuric acid (waste sulfuric acid produced in the washing step with concentrated sulfuric acid of crude benzole and petroleum products and is called merely as waste sulfuric acid hereinafter) composed mainly of sulfonic acid and organic compounds of sulfuric acid, or concentrated sulfuric acid is used as catalyst for the polymerization improvement of pitches, and this method can achieve the object at a lower reaction temperature.
  • the present inventors have completed a method which overcomes completely the above defect by an extraction treatment using petroleum heavy oils.
  • this method just mentioned has a problem in separation of the precipitating pitch component and the extracted petroleum solution, and under a certain condition a small amount of the petroleum heavy oil mingles into the precipitating pitch component.
  • the quality of pitch is shown by an excessive lowering of the fixed carbon content, and it is necessary to carefully establish the conditions such as the temperature, the mixing and extracting ratio, etc.
  • the present invention has also overcome this problem completely and makes it possible to produce pitches of good quality under a wide range of conditions in spite of differences in the quality of coal tar and properties of heavy oils.
  • the present invention is to provide a method which can maximize the extractability of lowmolecular components and the separability of pitch component by using petroleum hydrocarbons containing or mixed with a small amount of low boiling point saturated hydrocarbon oil in addition to high boiling point petroleum heavy oil as extracting agent for removing low-molecular low-boiling point components in the coal tar.
  • the petroleum solvents used in the present invention have the following properties.
  • the aniline point more than 20C (desirably more than 40C).
  • the petroleum solvents within the above range include light oil, heavy oil, mixtures of light oil and heavy oil, mixtures of heavy oil with light oil, kerosene and gasoline, etc., and various crude oils.
  • the extracting agent contains a low boiling point saturated hydrocarbon in addition to the high boiling point heavy oil, the separability is improved due to the lowering of viscosity at the time of extraction, and part of paraffin or naphthene hydrocarbon oil which dissolves into the pitch layer in a very small amount is converted into a low boiling point hydrocarbon and thus distillation separation for final adjustment of softening point is easily attained.
  • the present invention has eliminated the both defects and makes it possible to produce pitches of good quality from coal tar components with a simplified equipment.
  • FIG. 1 is a graph showing the relation between the temperature and the viscosity of pitch produced 'by the present invention in comparison with that by a conventional method.
  • FIG. 2 is a graph showing the relation between the temperature and the viscosity of road tar produced by the present invention in comparison with that by a conventional method.
  • EXAMPLE 1 Petroleum heavy oil of C grade was added to coal tar in a ratio of l l and the mixture was stirred at 50C and 100C respectively and left still at the above tem- Heavy oil of C grade was added to soft pitch and the mixture was stirred at 80C and 150C respectively. Pitches thus separated show the following properties.
  • the pitch produced by the treatment at 50C in Example l was further treated at 150C with addition of heavy oil of C grade in a ratio of l l. Pitch thus separated shows the following properties.
  • Hard pitch Modified Stirring temperature by heat 87 35. 2 10. 0 57. 1 Amount of Inventive method: of addition, Middle pitch (Exampercent Analysis 50 C. 80 C. 120 C. p e 2) 67 23. 2 a. 1 50. 0
  • the pitch of the present invenggggl mmwnent tion shows lowered temperature-sensitivity as com- Q g scomponent, pared with that of the pitch produced by the convenlgxedear bogg, ercent 33.4 33.9 .5 tional method.
  • This tendency is also observed in road Scoslty (5 cp 720 tar produced by the present invention, thus overcoming 45 6 the d f t of conventional road an TABLE 14.
  • FIG. 2 shows measurements of the temperature- Am Stirring temperature viscosity relation.
  • the temperature is preferably 50 to 150C in case of tar and 100 to 250C in case of middle pitch.
  • Pitch properties Amount Heavy of added oil Percent waste Tar treatsulfuric heavy Grade of ment Yield of Softening Benzole- Quinolinc- Experiment acid, oil heavy temp., pitch, point, insoluble insoluble Fixed No. percent ratio 0 0. percent component component carbon 1.. 0 1/1 C 80 25 88 29.3 9.2 57.8 1. 5 1/1 C 80 95 34. 5 0.5 59. 9 1. 5 1/0. 5 G 80 28 88 36. 5 9. 6 59. 6 1. 5 1/0. 5 A 80 30 91 36. 9 9. 4 62. 7 1.5 1/0. 5 B 80 88 35.2 8.8 58. 6 5.0 1/1 C 120 46 1 83 1 58.2 8.6 l 51.
  • Bananas-Separated substance (precipitate) after the heavy oil treatment was analysed as road tar and distillation or oil addition for adjustment of viscosity was not conducted.
  • the amount of EXAMPLE 13 added waste sulfuric acid or concentrated sulfuric acid has direct connection with increase and decrease of the benzole-insoluble component, and the proportion of heavy oil and the treatment temperature control the softening point, the fixed carbon content and separation from heavy oil.
  • heavy oil is preferably from 30 200 percent to the tar for good separation and accessibility Extraction by petroleum light oil alone or mixed Oil Petroleum light oil, heavy oil or mixed oil was added in various ratios to 10kg of coal tar, the mixtures were heated under stirring, left still and the pitch component which precipitated in the lower layer was analysed.
  • the present inventors have completed a method for producing pitch of very good quality by conducting poly-condensation after the addition of a small amount of waste sulfuric acid or concentrated sulfuric acid to coal tar at a low temperain Table 24. ture.
  • One example of this method is set forth under.
  • the mixed oil is a mixture of C grade oil, light oil,
  • Table 26 shows the analysis 5 method to a soft pitch and a middle pitch as well as to of the waste sulfuric acid used in this example. the coal tar. This is shown in the following example.
  • raw material coal tar having low contents of fixed carbon and solvent-insoluble components.
  • the solvent after the extraction is a mixture of crude oil and low-molecular aromatic component of the coal tar, and thus can be readily used for production of petroleum products (gasoline, light oil, heavy oil and asphalt) by distillation.
  • gasoline shows increase octane rating
  • asphalt shows improved mixability with aggregate materials and improved permeability when used for road pavement.
  • waste sulfuric acid or sulfuric acid serves to prevent colouration of distilled oil and formation of gum substance at the time of distillation refinement of the separated extraction solvent and contributes for desulfurization, thus improving the quality of distilled products.
  • the object of the present invention is to provide a method for producing and improving coal tar, it is possible to produce unique petroleum products and low-sulfur fuel oil when coal tar is used as fuel or when the present invention is applied to the refining step of petroleum without heat decomposition and contact decomposition as conventionally done.
  • a method for producing coal tar pitch comprising adding sulfuric acid to coal tar produced by the high temperature, dry distillation of coal and then adding a petroleum hydrocarbon oil to the mixture, said oil having an aniline point above 20C and consisting of 0-30 percent of a fraction having a boiling point up to 200C, 20 to 98 percent of a fraction having a boiling point between 200 and 360C and 0 to percent of a fraction having a boiling point above 360C, the ratio of coal tar to said oil being from 110.3 to 2.0, and maintaining the temperature between 50 and 250C to precipitate and separate the pitch component.
  • a method for improving coal tar pitch by extraction comprising adding to the pitch a hydrocarbon oil having an aniline point above 20C and consisting of 0-30 percent of a fraction having a boiling point up to 200C, 20 to 98 percent of a fraction having a boiling point between 200 and 360C and 0 to 80 percent of a fraction having a boiling point above 360C, the ratio of coal tar to said oil being from 110.3 to 2.0, and maintaining the temperature between 50 and 250C to precipitate and separate the pitch component.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Working-Up Tar And Pitch (AREA)
  • Detergent Compositions (AREA)
US00196096A 1970-11-10 1971-11-05 Method for producing bituminous substance such as a coal tar pitch Expired - Lifetime US3775289A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP45098979A JPS4918451B1 (enrdf_load_stackoverflow) 1970-11-10 1970-11-10
JP9898070 1970-11-10
JP45102970A JPS4918769B1 (enrdf_load_stackoverflow) 1970-11-21 1970-11-21

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US3775289A true US3775289A (en) 1973-11-27

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US (1) US3775289A (enrdf_load_stackoverflow)
CA (1) CA985650A (enrdf_load_stackoverflow)
DE (1) DE2155530A1 (enrdf_load_stackoverflow)
FR (1) FR2113716A1 (enrdf_load_stackoverflow)
GB (1) GB1376341A (enrdf_load_stackoverflow)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3865713A (en) * 1972-06-12 1975-02-11 Kureha Chemical Ind Co Ltd Carbonaceous reagent for carbonaceous binder used in the manufacture of fired carbon articles and carbon-bonded refractories
US3970542A (en) * 1971-09-10 1976-07-20 Cindu N.V. Method of preparing electrode pitches
US5605618A (en) * 1994-09-09 1997-02-25 Petoca, Ltd. Process for preparing nitrogen-containing isotropic pitch and nitrogen-containing isotropic pitch
RU2178441C1 (ru) * 2000-07-20 2002-01-20 Томских Светлана Сергеевна Способ получения битумного связующего

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3025612C2 (de) * 1980-07-05 1985-11-14 Rütgerswerke AG, 6000 Frankfurt Pechartige Produkte und Verfahren zu ihrer Herstellung
US4744882A (en) * 1987-01-02 1988-05-17 Domtar Inc Polycondensates of sulfonated coal tar fractions

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1722872A (en) * 1923-12-27 1929-07-30 Zeche Mathias Stinnes Process for separating oil from coal tar
US2299469A (en) * 1935-07-26 1942-10-20 Universal Process Parent Compa Treatment of bitumina and allied substances
US2560642A (en) * 1946-06-19 1951-07-17 C D Patents Ltd Treatment of pitches or tars and the manufacture of molded articles therefrom
US3490586A (en) * 1966-08-22 1970-01-20 Schill & Seilacher Chem Fab Method of working up coal tar pitch
US3692663A (en) * 1971-03-19 1972-09-19 Osaka Gas Co Ltd Process for treating tars

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1722872A (en) * 1923-12-27 1929-07-30 Zeche Mathias Stinnes Process for separating oil from coal tar
US2299469A (en) * 1935-07-26 1942-10-20 Universal Process Parent Compa Treatment of bitumina and allied substances
US2560642A (en) * 1946-06-19 1951-07-17 C D Patents Ltd Treatment of pitches or tars and the manufacture of molded articles therefrom
US3490586A (en) * 1966-08-22 1970-01-20 Schill & Seilacher Chem Fab Method of working up coal tar pitch
US3692663A (en) * 1971-03-19 1972-09-19 Osaka Gas Co Ltd Process for treating tars

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3970542A (en) * 1971-09-10 1976-07-20 Cindu N.V. Method of preparing electrode pitches
US3865713A (en) * 1972-06-12 1975-02-11 Kureha Chemical Ind Co Ltd Carbonaceous reagent for carbonaceous binder used in the manufacture of fired carbon articles and carbon-bonded refractories
US5605618A (en) * 1994-09-09 1997-02-25 Petoca, Ltd. Process for preparing nitrogen-containing isotropic pitch and nitrogen-containing isotropic pitch
RU2178441C1 (ru) * 2000-07-20 2002-01-20 Томских Светлана Сергеевна Способ получения битумного связующего

Also Published As

Publication number Publication date
DE2155530A1 (enrdf_load_stackoverflow) 1972-05-25
CA985650A (en) 1976-03-16
FR2113716A1 (enrdf_load_stackoverflow) 1972-06-23
GB1376341A (en) 1974-12-04

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