US2041957A - Method of working up low valued materials such as pitch, acid sludge, and the like - Google Patents

Method of working up low valued materials such as pitch, acid sludge, and the like Download PDF

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Publication number
US2041957A
US2041957A US656204A US65620433A US2041957A US 2041957 A US2041957 A US 2041957A US 656204 A US656204 A US 656204A US 65620433 A US65620433 A US 65620433A US 2041957 A US2041957 A US 2041957A
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US
United States
Prior art keywords
working
pitch
acid sludge
materials
retort
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Expired - Lifetime
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US656204A
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English (en)
Inventor
Reis Alfred
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pape & Co G M B H
Pape & Co GmbH
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Pape & Co GmbH
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Publication date
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G9/00—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
    • C10G9/42—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils by passing the material to be cracked in thin streams or as spray on or near continuously heated surfaces
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B55/00—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material
    • 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
    • C10C1/19—Working-up tar by thermal treatment not involving distillation
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G17/00—Refining of hydrocarbon oils in the absence of hydrogen, with acids, acid-forming compounds or acid-containing liquids, e.g. acid sludge
    • C10G17/10—Recovery of used refining agents

Definitions

  • This invention relates to processes for working-up pitch, tar, acid sludge and other combustible substances by heat treatment with the exclusion of air, for the purpose, in particular, of producing liquid fuels.
  • 'I'he process differs essentially on the one hand from coking processes which produce coke in coherent form, and on the other hand from cracking processes in which the avoidance of the formation of appreciable amounts of solid coke-like residues is important if the process 'is to be of technical or commercial value.
  • the process in accordance with the invention mayV be employed for example for working-up acidpitches or acid'sludges of .a1l.kinds which are accumulated in the refining of petroleum and like products and are not only worthless but extremely troublesome. It is possible by means of the invention to obtain from these materials light liquid hydrocarbons, that is to say a valuable product. y
  • the process is also suitable in particular for working-up inferior heavy oils and bituminous substances and similar products which remain over from the treatment of petroleum or coal.
  • hydrocarbons obtained by the process in accordance with the invention represent especially readily volatile, .gasoline-like fuels of high quality which exhibit no tendency to knock.
  • a process i'or working-up' acid sludges is known v'in which the 'organic sulphur compounds are y
  • the main object of this process is to work-up the gas mixture obtained. for the manufacture of sulphuric acid.
  • the organic material is mostly. converted into coke and only a moderate proportion can be obtained in the form of liquid hydrocarbons.
  • the quality of the hydrocarbonsv produced is necessarily inferior under these circumstances.
  • a process for working-up acidA sludges is also known accordingto which these are carefully and gradually heated in stages in l order to prevent scum or foaming.
  • the essential feature of theprocess according to the invention is that the Imaterial to be treated, for example the acid sludge, is introduced into a retort heated to red heat and is heated with the exclusion of air and gasied.
  • a temperature of about 700 to 800 C. has proved to be suitable.
  • the reference numeral 2 indicates a sheet metal container into which the acid sludge or other material to be treated is placed. This container is heated by suitable heating means such as by the burner I. Fromthis container 2 the material .flows to a mixer or mill 6 after which it flows to a container 8. The material is pumped from the container 8 by the pump Il) through the pipe I2 to the dust separator Il, which is illled withRaschig-rings I8.
  • the gases evolved in the retort I8 simultaneously enter the separator I4 from below through the opening 20. These gases pass upwardly through the separator Il as the liquid material iiows downwardly therethrough.
  • the liquid material together withv4 solid particles it has picked up from the gases pass from .the separator I4 to A the mill 6 and back to the container 8.
  • the material is also drained off by the pump,22 from this container and forced through the pipe 24 to the atomizer nozzle 26 at the' top of the retort il. y
  • the retort is provided with Scrapers 3l which extend from top to bottom. They are ro,
  • 'I'he gases and vapors which are formed pass through the opening 42 to a centrifugal separator 44 which separates the finer solid particles and collects them in a worm conveyor 46.
  • 'I'he gases nally pass through the pipe 48 to the dust separator i4 where they are cleaned again and from the dust separator they vpass through the to a cooling apparatus (not shown).
  • the vapors and gases may be passed to a cracking chamber 52 as will be hereinafter described.
  • the greater part is converted by the action of rapid heating, in particular by the radiation of heat from the wall of the retort,
  • the process is based, as has been emphasized pipe above, on the employment of an unusually rapid heating of the raw material in a gasifying chamber of which the walls are heated to a high temperature and act mainly by radiation on the raw material.
  • the gasifying chamber may be provided with builtin parts or insertions which must also be heated to a high temperature.
  • the amount of material present in the gasifying chamber is kept small and the duration. of the material in the chamber is short. It has been found that by suitably regulating the operating conditions any material can be gasified in a very short time in such a manner that only a dry solid residue remains over.
  • a particularly suitable method of carrying the process according to the invention into effect is to introduce the material into the gasifying chamber in a finely divided form which may be effected in particular by atomizing or disintegrating the liquid or liquefied material through nozzles or by other known means for this purpose.
  • the size of the drops, the intensity of the radiation and the duration in the gasifying chamber must be relatively regulated or adapted to suit one another in such a manner that the residual grains leave the gasifylng chamber in a condition in which they have been sufliciently used up.
  • period of duration in the gasifying chamber and the passage of the drops through it can also be regulated by the introduction of gases which exert no harmful effect on the gasied material.
  • the drops in the middle of the retort that is to say those lying furthest away from the radiating surface, are subjected to a suiiiclently intense radiation.
  • the density of the drops therefore, must not be so great that the radiation is too strongly absorbed before it reaches the middle of the retort; on the other hand, the economy of the process requires that the permissible density of the drops and, therefore, the permissible output of the ga/ sifying chamber is sufficiently utilized. This taking into consideration of the absorption of the radiation in the gasifying chamber which is filled with drops is, therefore, a feature of the process.
  • Example 1 As the gaslfying retort there is employed a vertical iron ⁇ tube of 40 cm. internal Width and 3 metres-in height. Into the retort, which is heated to '150 C., molten petrol-pitch is blown-in from the top through an atomizing nozzle, the output being 60 kg. per hour. The size of the drops is of the order of 0.1 mm'., the period of duration in the gasifying chamber is of the order of 1 sccond. The pressure in the retort is the atmospheric pressure. For regulating the atomization and the movement of the material in the gasifying chamber the gases resulting from the decomposition are employed.
  • An important advantage of the process is that the vapors formed in the gasifying chamber may be conducted to a following heat treatment process (cracking) of any desired nature without previous condensation, and that for this cracking process the temperature, the duration of the process and the form of the cracking chamber 52 may be entirely independent of the gasifying condiformation of troublesome scum or foam.
  • the gasifying chamber and the cracking chamber can be fitted in two separate furnaces or in one furnace.
  • the process may be carried out at the ordinary pressure or at an increased pressure.
  • the materials obtained, insofar as they cannot otherwise be profitably used, can be returned to the process. This holds good, in contradistinction to the usual cracking process, in particular also for heavy oils and for tar-like or pitch-like ⁇ dstillates.
  • the admixture of distillates may also assist in facilitating the disintegration.
  • the acid sludge in accordance also with the invention is intimately mixed before the heat treatment with an excess of basic substances in the presence of water, and the mixture is treated at the temperature of boiling Water or at a somewhat lower temperature until the evolution of gas (sulphurous acid and carbonic acid) is ended.
  • Example 2 10 kg. of chalk are stirred with 20 litres of hot I water and 20 kg. of acid sludge (originating from excess water is poured on and the neutralized acid Dressing.
  • Example 3 Neutralized acid oil and heated. The proportions of the mixture are 120 kg. of oil to 100 kg. of the crude acid sludge contained in the neutralizedV product. 'I'here is formed an emulsion which 'is stable at 90 C. and flows easily.
  • the whole ofthe sulphur content of the acid sludge remains in the retort residue and is thus rendered harmless, with the single exception of a proportion of sulphuretted hydrogen inthe gas evolved, which can be absorbed in gas purifiers by known methods after condensation oi the liquid fuel.
  • a method oi working-up low valued materials such as pitch, acid sludge and the like to produce light liquid hydrocarbons therefrom which comprises gasiiying and evaporating a portion of said materials by rapidly passing the same in a tlnely divided state downwardly through a Zone heated by radiation to a temperature equivating to red heat and at least to about 700 C., and in which air has been excluded, and in' then cracking the vapor thus formed.
  • a method of working-up low valued materials such as pitch, acid sludge and the like to sludge is stirred with heavy through a zone heated by radiation to a ternperature over 700 C. and from which oxygen has been excluded, and cracking the vapor thus formed.
  • a method of Worg-up low valued umta-l1 g rials such as. pitch, acid sludge and the like to produce light liquid hydrocarbons therefrom which comprises gasifying and evaporating a portion of said materials by rapidly passing the same in a iinely divided state downwardly through a zone heated by radiation to a temperature equivalent to red heat and at least to about 700 C.,and in which air has been excluded, regulating the duration of the passage of the divided material through said zone by introducing into it said zone a gas which does not ailect the properties-of the material and which by its own velocity regulates the passage oi the material.
  • mate- ⁇ rials such as pitch, acid sludge and the like
  • a methodof working-up low valued mated5 'raus such as pitch, acid sludge and the like w produce light liquid hydrocarbons therefrom, which comprises mixing the material with water 'and a basic alkaline substance such as chalk to neutralize said material, removing the excess 50 water from said neutralized material, mixing the neutralized material with oil, rapidly passing said mixture in a iinely divided state downwardly through a zone heated by radiation to a teniperature equivalent to red heat to gasii'y and evaporate the same.
  • a method of working-up low valued materials such as pitch, acid sludge and the like tu produce light liquid hydrocarbons therefrom, which comprises mixing the material with water and a basic alkaline substance such as chalk to neutralize said material, removing the excess water from said neutralized material, mixing neutralized material with Oli, rapidly passing said mixture in a nely divided state downwardly t5 through a. zone heated by radiation to a wolfl perature equivalent to ,red heat to gasify and evaporate the saine, and cracking the vapor thus formed.
  • a basic alkaline substance such as chalk

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Treatment Of Sludge (AREA)
US656204A 1932-02-16 1933-02-10 Method of working up low valued materials such as pitch, acid sludge, and the like Expired - Lifetime US2041957A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE418204X 1932-02-16

Publications (1)

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US2041957A true US2041957A (en) 1936-05-26

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US (1) US2041957A (enrdf_load_html_response)
FR (1) FR750337A (enrdf_load_html_response)
GB (1) GB418204A (enrdf_load_html_response)
NL (1) NL40643C (enrdf_load_html_response)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2758061A (en) * 1949-10-31 1956-08-07 Ruetgerswerke Ag Vaporization and cracking of liquids or mixtures of liquids, more particularly of hydrocarbons
US4839021A (en) * 1986-06-19 1989-06-13 Recherche Carbovac Inc. Treatment of petroleum derived organic sludges and oil residues

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2758061A (en) * 1949-10-31 1956-08-07 Ruetgerswerke Ag Vaporization and cracking of liquids or mixtures of liquids, more particularly of hydrocarbons
US4839021A (en) * 1986-06-19 1989-06-13 Recherche Carbovac Inc. Treatment of petroleum derived organic sludges and oil residues

Also Published As

Publication number Publication date
FR750337A (fr) 1933-08-08
GB418204A (en) 1934-10-15
NL40643C (enrdf_load_html_response) 1937-05-15

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