US1946721A - Process of obtaining valuable light oils from the distillation of coal - Google Patents

Process of obtaining valuable light oils from the distillation of coal Download PDF

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Publication number
US1946721A
US1946721A US559573A US55957331A US1946721A US 1946721 A US1946721 A US 1946721A US 559573 A US559573 A US 559573A US 55957331 A US55957331 A US 55957331A US 1946721 A US1946721 A US 1946721A
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Prior art keywords
distillation
coal
ducts
light oil
sulphuric acid
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US559573A
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English (en)
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Still Carl
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Individual
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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
    • C10C1/00—Working-up tar
    • C10C1/20—Refining by chemical means inorganic or organic compounds
    • 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
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
    • 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
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/02—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by 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
    • C10G17/02—Refining of hydrocarbon oils in the absence of hydrogen, with acids, acid-forming compounds or acid-containing liquids, e.g. acid sludge with acids or acid-containing liquids, e.g. acid sludge
    • C10G17/04—Liquid-liquid treatment forming two immiscible phases
    • C10G17/06—Liquid-liquid treatment forming two immiscible phases using acids derived from sulfur or acid sludge thereof
    • 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
    • C10G5/00—Recovery of liquid hydrocarbon mixtures from gases, e.g. natural gas
    • C10G5/04—Recovery of liquid hydrocarbon mixtures from gases, e.g. natural gas with liquid absorbents
    • 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
    • C10G7/00—Distillation of hydrocarbon oils

Definitions

  • the subject of this invention is a process for obtaining valuable light oils from the distillatlon of fuel in chamber or retort ovens.
  • ovens for the distillation of coal provided with external heating, that is,
  • the products from which the valuable light oils are to be obtained are themselves obtained by forming channels or ducts in the mass of coal, for example by ramming, boring or embedding forming bodies such as rods or tubes, which may be entirely or partially withdrawn.
  • the distillation products evolved in the interior of the mass of coal are drawn on through these ducts, collected in a pipe common to all the ducts and then led in the usual manner into one or more gas and tar mains.
  • the distillation products are, preferably,
  • tubes drawn off from the said ducts by tubes connect- All ed gas-tight to the discharge ends of the ducts or by perforated tubes inserted in the ducts, the tubes being carried through the oven walls, for example in the case of vertically arranged ducts, through the oven roof or still within the oven, and open into a common collecting pipe leading from the oven chamber.
  • the suction apparatus should be provided with pressure regulating devices which enable the suction pressure in the ducts to be controlled as required, and, if required, to be modified during the course of and according to the phase of the distillation process.
  • the suction pressure used in the ducts is preferably maintained at least at mm. of the water gauge below atmospheric.
  • suction pressures For particular classes of coal, and also in the later stages of the distillation process, much higher suction pressures may be employed. For instance, in the distillation and coking of Westphalian coals, suction pressures up to 200 mm. W. G. below atmospheric and even more have been found advisable.
  • the pressure regulation is, preferably, effected by means of resistances, such as throttling devices or liquid seal resistances, inserted between the suction ducts and the gas and tar main.
  • the distillation products which are obtained in this manner are then treated at first in the usual manner.
  • the light oils, the recovery and treatment of which form the main object of this invention, are contained partly in the tar condensed by cooling the distillation gas and partly remain as vapours in the cooled gas itself and can be removed from it, for example, by an oil wash.
  • An oven for the distillation of coal for example a horizontal chamber oven, suitable for carry- 6 ing out the process, is shown at l.
  • Ducts 3 are formed in the loosely shaken or embedded mass of coal 2 by forming bodies rammed or bored in the coal, and from these ducts the distillation products evolved in the interior of the coal are drawn off by suction by means of inserted tubular members 4.
  • the tubular members 4 are inserted in discharge tubes 6 and are, preferably, provided with packing 5 to seal the members 4 against the interior of the discharge tubes 6.
  • the tubes 6, in the case of vertically arranged ducts are, preferably, led through the oven roof and are connected to a collecting pipe 7 disposed over or outside the brickwork of the roof.
  • the individual collecting pipes of the chambers lead into a gas and tar main 8, the connection of each individual pipe 7 to the gas and tar main 8 including, besides the usual closing valve, a controlling member 9 formed, for example, as a throttling cap.
  • the controlling members 9 enable the suction pressure in the ducts 3 to be regulated as required for the particular coal being employed or as called for by the particular phase of the distillation process.
  • the distillation products obtained pass through a pipe 10 into one or more gas coolers 11 and thence, by a pipe 12 into a tar extractor 13.
  • the apparatus 14 represents an ammonia washer of any suitable kind and 15 a benzol washer operating with washing oil, which in known manner are arranged and designed to be traversed in succession by the distillation products.
  • the gas is led away from the benzol washer 15 through a .105 pipe 16, while the saturated wash oil passes through a pipe 1'7 into an oil heater 18 from which it is led through a pipe 19 into a stripping still 20.
  • the stripping still allows the washing oil freed from light oil to be discharged at 410 the bottom, while the light oil passes from the top of the stripping still into a cooler 21 and after condensation therein into a pipe 22.
  • the further treatment of the light oil product is effected through a rectifying column 23 which separates out the remainder of the washing oil, while the crude light oil passes through a pipe 24 into a cooler 26 and from there into a pipe 27.
  • the pipe 27 leads the crude oil into an apparatus 28 in which the first, or acid wash treatment is carried out.
  • the first acid wash is succeeded according to the invention by a second wash, which is carried out with highly concentrated sulphuric acid.
  • the same apparatus 28 can serve for the second wash, but it is preferable to insert a second washer 29.
  • the crude light oil, after being passed through both washers 28 and 29 is subjected to an alkali and water wash in a washing apparatus 30 and then is passed into a further rectifying column 31. From this, the residues are collected at 32, while the light oil, which is now pure, is led again into a cooler 33 and is then stored.
  • Crude tar is separated out in the cooling of the distillation products by the gas cooler 11 and this tar also contains light oils.
  • the crude tar in the cooler 11 is led by a pipe 43 to an indirectly heated stripping still 34, where the crude light oil is separated from the tar.
  • the tar forming the residue is, pref rably, led away at 35, while the crude light oil passes into a cooler 36 and from there into a pipe 37.
  • the crude light oil may be led directly into the washer 28, but it is preferable to lead the crude light oil by a pipe 39 into the pipe 22 at the junction l0, so that the crude light oil obtained from the crude tar is also rectified in the column 23.
  • For the purpose of leading the light oil either through the pipe 38 or through the pipe 39 it is necessary to close or open the valve 41 or 42.
  • These light oils obtained in the described distillation process have a special composition and chemical properties. They do not consist exclusively of aromatic hydrocarbons, i. e. benzol and its higher homologues, as in the fomer proc esses for the distillation of coal conducted at higher temperature and without the use of the interior suction ducts. They consist essentially in a mixture of aromatic and aliphatic hydrocarbons with a greater or less proportion of the latter.
  • the applicant has found that all the requirements as regards the purity of the light oil and its resistance to light and air are complied with, if the purifying treatment is conducted in two stages; in the first stage the light oil being treated with a polymerizing mebent. HzSOrat ordinary temperature.
  • the tomdium of restricted activity such as, for example, moderately concentrated or dilute sulphuric acid or haloid salts or with adsorption media, such as silica gels, activated coal, infusorial earths, or with mixtures of such materials, while in the second stage a treatment is effected with concentrated acid or other similarly strongly active medium.
  • this treatment can be carried out, if, for example, sulphuric acid of at the most per cent.
  • H2804 is employed at ordinary or only slightly higher temperatures, and then sulphuric acid of at least 90 per cent.
  • H2SO4 at a higher temperature, preferably between the limits of about 30-35 C. This can be followed by the usual treatment with alkali lye and washing with water and distillation.
  • these constituents in the combined treatment in the first stage are polymerized to lower molecular oils, that is stabilized and brought into a l form in which they are resistant to the succeeding attack of the highly concentrated sulphuric acid and remain as valuable constituents of the light oil.
  • An essential advantage of the new process is 1 that a larger quantity of the distillation products, drawn by suction from the charge of coal, is obtained as improved light oils, and not again lost wholly or partly as Worthless waste materials in the later stages of the purifying processes.
  • the process according to the invention therefore, a very essential diminution of the losses due to purification is obtained and at the same time the yield in light oil is considerably increased.
  • moderately concentrated or dilute sulphuric acid can, as explained, be employed, or haloid salts, for example ferric chloride, zinc chloride, aluminium chloride, chloride, of lime; also materials such as ferric sulphate, sodium methylate, sodium ethylate, boric acid, phosphoric acid; also solid adsorption materials such as silica gels, activated coals, infusorial earths, fullers earth, or mixtures of several such materials.
  • the first described treatment can be varied in many ways, for example, by the first treatment with sulphuric acid being effected by means of a considerably lower content in H2504 than 80 per cent. and in order to obtain a similar polymerizing action, as with, for example, 80 per cent. acid, the temperature must be correspondingly raised. In the succeeding second treatment with sulphuric acid of higher concentration the said temperature must, however, be
  • the remaining light oil is treated with 50 grams sulphuric acid of 91 per cent. H2804.
  • the acid is imparted slowly and the temperature is maintained at 32 C. by watching or by special external cooling.
  • the washed light oil is subjected to the usual treatment with soda lye and water and, finally, is distilled so as to obtain a pure product.
  • sulphuric acid Type 1
  • the total loss of the purification including the distillation, amounting to grams, viz. 8 per cent. of the original quantity.
  • suction pressure used is of the order of 40 mm. of the water gauge below atmospheric.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Materials Engineering (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US559573A 1930-08-29 1931-08-26 Process of obtaining valuable light oils from the distillation of coal Expired - Lifetime US1946721A (en)

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Application Number Priority Date Filing Date Title
DE378217X 1930-08-29

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US (1) US1946721A (enrdf_load_stackoverflow)
FR (1) FR722139A (enrdf_load_stackoverflow)
GB (1) GB378217A (enrdf_load_stackoverflow)
NL (1) NL32264C (enrdf_load_stackoverflow)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4077868A (en) * 1975-02-10 1978-03-07 Deco Industries, Inc. Method for obtaining hydrocarbon products from coal and other carbonaceous materials

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4077868A (en) * 1975-02-10 1978-03-07 Deco Industries, Inc. Method for obtaining hydrocarbon products from coal and other carbonaceous materials

Also Published As

Publication number Publication date
FR722139A (fr) 1932-03-11
GB378217A (en) 1932-08-11
NL32264C (enrdf_load_stackoverflow)

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