EP0768362A1 - Procédé et appareil de séparation de bitume d'asphalte - Google Patents

Procédé et appareil de séparation de bitume d'asphalte Download PDF

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Publication number
EP0768362A1
EP0768362A1 EP95116320A EP95116320A EP0768362A1 EP 0768362 A1 EP0768362 A1 EP 0768362A1 EP 95116320 A EP95116320 A EP 95116320A EP 95116320 A EP95116320 A EP 95116320A EP 0768362 A1 EP0768362 A1 EP 0768362A1
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EP
European Patent Office
Prior art keywords
water
bitumen
asphalt
sample
vessel
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.)
Granted
Application number
EP95116320A
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German (de)
English (en)
Other versions
EP0768362B1 (fr
Inventor
Gerd Prof. Dr.-Ing. Brunner
Manuel Dipl.-Ing. Budich
Stanislaus Dipl.-Ing. Jung
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Individual
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Individual
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Priority to DE59505852T priority Critical patent/DE59505852D1/de
Priority to EP19950116320 priority patent/EP0768362B1/fr
Publication of EP0768362A1 publication Critical patent/EP0768362A1/fr
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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
    • C10C3/007—Working-up pitch, asphalt, bitumen winning and separation of asphalt from mixtures with aggregates, fillers and other products, e.g. winning from natural asphalt and regeneration of waste asphalt

Definitions

  • the invention relates to a method and a device for separating bitumen from asphalt according to the preamble of claim 1 and an apparatus for performing this method.
  • DE-A-32 01 719 describes a process in which, for example, oil shale or tar sands are treated with supercritical water at 360-600 ° C and 130-700 bar. In this case, after condensation of the water, an organic phase is formed which is free of the finest particles. The latter is the biggest problem in oil recovery from oil shale or tar sands with conventional methods (smoldering of oil shale, hot water extraction of tar sands). Other problems with conventional methods: high energy consumption, incomplete separation of the high molecular weight bitumen fraction.
  • the extraction is accelerated by adding salts (NaCl, K 2 CO 3, etc.) when dissolved in water vapor in the range of 0.05-0.2% by weight, the solubility of the salts being determined by temperature and pressure. With salts dissolved in the water, the extraction is faster and the deposition better (less org. Remainder in the water).
  • the condensed water can be used again after the oil separation without further workup.
  • cyclohexane was used in the boiling state under elevated temperatures and pressures.
  • the sample is treated in the pressure room without circulation of the extractant.
  • the production process according to DE-A-42 23 246 serves for the separation of tar and solids.
  • low molecular weight hydrocarbons alcohols, acetone
  • hydrogen hydrogen
  • water hydrogen
  • / or carbon dioxide are used supercritically at P> 70 bar and T> 100 ° C.
  • the goal is to crack the tar molecules.
  • Tar was formerly used in road construction, while today (in Germany) only bitumen is used.
  • it is proposed to set a grain size below 6 mm.
  • Tar sand should be treated by the method of US-A-4,005,005 with water between 301 and 468 ° C and a density of at least 0.1 g / cm 3 , wherein the supercritical region is used.
  • the deposition of the organic fraction is carried out by means of Pressure or temperature reduction. There is no question of an analysis.
  • oil shale is treated with water vapor in the supercritical region, an oil fraction recovered and the water recirculated.
  • the oil shale is also comminuted here to particle sizes below 1/4 inch to allow continuous promotion of the suspension or the sludge with water.
  • Road asphalt for example, is composed of a mixture of minerals and bitumen. Depending on the requirements, different mixes are produced. It is varied u.a. the type of minerals, their particle size distribution and the type of composite bitumen. The analysis of an asphalt sample provides information on whether the composition of the asphalt meets the requirements.
  • the asphalt sample is dissolved in trichloroethene, whereby a bitumen-free mineral fraction is obtained.
  • the bitumen dissolved in the trichloroethene is distilled off recovered of the solvent and can be subjected to a quality analysis (hardness, softening point, etc.).
  • a disadvantage of the conventional method is the use of halogen-containing and thus ozone-destroying compound trichloroethene.
  • the solvent must be completely distilled off to allow the analysis of the bitumen.
  • the invention is therefore based on the object to improve the aforementioned method and apparatus such that it is possible to dispense with the use of organic solvents, without a deterioration of the separation result must be taken into account.
  • bitumen-free mineral fraction in bitumen-free mineral fraction
  • bitumen fraction with the aid of hot water advantageously at temperatures between 320 and 350 ° C and a pressure corresponding to at least the associated vapor pressure, separated, so that the minerals remain bitumen-free.
  • the resulting fractions contain virtually no water, so that it may be possible to immediately subject them to further analysis.
  • Bitumen and minerals are also used in processing separated from tar sands.
  • water is used at temperatures of about 75 to 92 ° C under atmospheric pressure to replace the bitumen of the mineral particles.
  • this is only possible with particles that have a layer of water between bitumen and Mineralstoft. From road asphalt no bitumen can be separated under such conditions.
  • Another way to separate bitumen from minerals is to heat the mixture so high that the bitumen is volatile and thereby separates from the minerals. However, under such high temperatures, the bitumen is no longer stable.
  • the separation of the bitumen content of an asphalt sample is carried out in a pressure vessel according to the principle of Soxhlet extraction.
  • a sample vessel 2 is located in a pressure vessel 1, which comprises, for example, an internal volume of 1.5 liters.
  • the size of the container depends on the amount of sample to be analyzed. The specified size is sufficient for a sample amount of up to 500g.
  • the asphalt sample is located inside the pressure vessel in a sample vessel. The asphalt sample is shown hatched in Fig. 1. Below the sample vessel is presented as a release agent water 4 and is in the boiling state.
  • the pressure vessel 1 is heated with an electric heater 3 and is insulated to minimize heat loss to the environment.
  • the capacitor 5 is designed as a cone or pyramid.
  • the pressure P, the temperature of the water above the asphalt sample T1 and that of the water supply T2 can be determined.
  • Fig. 2 shows the processes in the sample vessel.
  • the dripping water on the sample material rises to a certain level and then flows off.
  • the sample material is located in an insert 7, which is connected to the overflow vessel 8, that at the bottom of a gap of about 1 - 2 mm results, so that the sample is continuously flowed through by condensate water.
  • the system cooled and the sample vessel 2 removed, the floating bitumen layer can be removed and sent for further analysis.
  • the mineral fraction can be removed bitumen-free via a line with outlet valve V.
  • Fig. 3 shows a sample vessel, in which no bitumen residues remain in the sample insert, but run off with the water.
  • the drops are collected in a funnel 9 whose shaft ends 1 - 2 mm above the bottom of the insert. In this way, the sample is flowed through from below.
  • the sample vessel is conically shaped to avoid dead spaces in the material flowed through. For any entrained fine grain another catch basin 10 is provided.
  • FIG. 1 Water from the reservoir 2 flows through the asphalt mixture in the extraction tank 1.
  • the water with the dissolved bitumen is passed into a separator 3, in which separate water and bitumen at a lower temperature.
  • the bitumen is removed at the end of extraction from the separator by means of a removable insert, the water is returned to the reservoir.
  • Fig. 4 Schematic representation of the apparatus for the separation of bitumen and minerals by means of hot water
  • a precisely weighed amount of asphalt (about 20g) is filled. If the vessel is located in the pressure vessel (1), it is closed. In the sealed container, a vacuum is created by evacuating the container via the valve (V) at the bottom to a vacuum pump or water jet pump. The required amount of water, e.g. 200 ml, sucked in via the bottom valve and started the heating process.
  • Achieving the desired test temperature T2 can be defined as the beginning of the experiment.
  • the pressure and temperatures T1 and T2 should be constant throughout the duration of the experiment. After the temperatures have been held constant for a while and the removal of the bitumen has taken place, the heating is turned off.
  • the sample vessel is removed after cooling, which removes above the sample on a water layer floating bitumen fraction and then removed the bitumen-free minerals. After a brief drying in a drying cabinet, the minerals are weighed and determined from the difference to the weighted sample amount of the separated bitumen content.
  • test time can be shortened considerably. For example, at 340 ° C, a one hour test for complete removal of the bitumen was sufficient.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Civil Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Extraction Or Liquid Replacement (AREA)
EP19950116320 1995-10-17 1995-10-17 Procédé et appareil de séparation de bitume d'asphalte Expired - Lifetime EP0768362B1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE59505852T DE59505852D1 (de) 1995-10-17 1995-10-17 Verfahren und Vorrichtung zum Abtrennen von Bitumen aus Asphalt
EP19950116320 EP0768362B1 (fr) 1995-10-17 1995-10-17 Procédé et appareil de séparation de bitume d'asphalte

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP19950116320 EP0768362B1 (fr) 1995-10-17 1995-10-17 Procédé et appareil de séparation de bitume d'asphalte

Publications (2)

Publication Number Publication Date
EP0768362A1 true EP0768362A1 (fr) 1997-04-16
EP0768362B1 EP0768362B1 (fr) 1999-05-06

Family

ID=8219724

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19950116320 Expired - Lifetime EP0768362B1 (fr) 1995-10-17 1995-10-17 Procédé et appareil de séparation de bitume d'asphalte

Country Status (2)

Country Link
EP (1) EP0768362B1 (fr)
DE (1) DE59505852D1 (fr)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3051644A (en) * 1959-07-01 1962-08-28 Texaco Inc Method for recovering oil from oil shale
US3509037A (en) * 1967-08-11 1970-04-28 Sun Oil Co Tar sand separation process using solvent,hot water and correlated conditions
US3738929A (en) * 1971-03-26 1973-06-12 Allied Chem Hydrocarbon extraction
US4005005A (en) * 1974-05-31 1977-01-25 Standard Oil Company (Indiana) Process for recovering and upgrading hydrocarbons from tar sands
US4376693A (en) * 1981-07-13 1983-03-15 Phillips Petroleum Company Solid liquid extraction
DE3201719A1 (de) * 1982-01-21 1983-07-28 Siegfried Prof.Dr. 8521 Uttenreuth Peter Verfahren zur extraktion von organischen stoffen aus mineralien
US5053118A (en) * 1990-07-02 1991-10-01 Thomas Houser Bitumen extraction from asphalt pavements
WO1992010612A1 (fr) * 1990-12-04 1992-06-25 Hollandsche Beton Groep N.V. Procede de transformation de beton bitumineux use en beton bitumineux reutilisable
DE4223246A1 (de) * 1992-07-15 1994-01-20 Tps Ges Fuer Tech Physikalisch Verfahren zur Trennung von Gemischen aus Teer und Feststoffen

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3051644A (en) * 1959-07-01 1962-08-28 Texaco Inc Method for recovering oil from oil shale
US3509037A (en) * 1967-08-11 1970-04-28 Sun Oil Co Tar sand separation process using solvent,hot water and correlated conditions
US3738929A (en) * 1971-03-26 1973-06-12 Allied Chem Hydrocarbon extraction
US4005005A (en) * 1974-05-31 1977-01-25 Standard Oil Company (Indiana) Process for recovering and upgrading hydrocarbons from tar sands
US4376693A (en) * 1981-07-13 1983-03-15 Phillips Petroleum Company Solid liquid extraction
DE3201719A1 (de) * 1982-01-21 1983-07-28 Siegfried Prof.Dr. 8521 Uttenreuth Peter Verfahren zur extraktion von organischen stoffen aus mineralien
US5053118A (en) * 1990-07-02 1991-10-01 Thomas Houser Bitumen extraction from asphalt pavements
WO1992010612A1 (fr) * 1990-12-04 1992-06-25 Hollandsche Beton Groep N.V. Procede de transformation de beton bitumineux use en beton bitumineux reutilisable
DE4223246A1 (de) * 1992-07-15 1994-01-20 Tps Ges Fuer Tech Physikalisch Verfahren zur Trennung von Gemischen aus Teer und Feststoffen

Also Published As

Publication number Publication date
DE59505852D1 (de) 1999-06-10
EP0768362B1 (fr) 1999-05-06

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