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US2670277A - Method and apparatus for the continuous production of carbon disulphide - Google Patents

Method and apparatus for the continuous production of carbon disulphide Download PDF

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US2670277A
US2670277A US98346A US9834649A US2670277A US 2670277 A US2670277 A US 2670277A US 98346 A US98346 A US 98346A US 9834649 A US9834649 A US 9834649A US 2670277 A US2670277 A US 2670277A
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retort
heat
sulphur
gases
reaction
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US98346A
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Charles Ernest
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PROD CHIM DE CLAMECY SOC D
PRODUITS CHIMIQUES DE CLAMECY Ste
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/70—Compounds containing carbon and sulfur, e.g. thiophosgene
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Definitions

  • anobject ortheinvention to-organize the formation of the carbon disul'fideinsuch manner as. to reduce to a minimum the amount of heat energy to betintroduced-from the outside into the zone of reaction.
  • Thenew method is characterizedessentially by the introduction into the reaction zone, of thecoalfreed-from volatile gases and the sulfur after bothhave been preheated to the reaction temperature.
  • the losses of heat in this zone are prevented by heat insulating or slightly heating the, reaction vessel; the-heat produced in the reaction being utilized underthe-best possible conditionsfor preheating thesulphur and the coal and obtaining-theinexpensive purification of the carbondisulphide.
  • coal in any form, natural or agglomerated, with or without sulphuration catalysts or substances adapted to change the melting temperature of the ashes
  • coal is fed into the hopper i. It is then dischargedinto the heat-insulated coal preheating retort l0 through the medium of a gas-tight distributor 2.
  • the coal is heated by passing in front ofthe blast-pipe 9 fed with air' under pressure from a suitable source (not shown) through a conduit 8 and with gases fed from the distillation of the charcoal through a conduit 1.
  • the red-hot charcoal descends into the upper portionof the'retort [3 which is kept under constant pressure by means of the automatic reguIatorSB having its pressure-intake at $4.
  • the solid sulphur introduced into the hopper 26 is fed by the screw conveyor 21 into the melting tunnel 24% provided wi'tl'r an agitator 23; This tunnel is heated by means of a cluster of tubularelements.
  • phi-1r is vaporized in; heater 2i. It is therefore apparent that the hot-gases and the-sulphur vapor. travel in a counter-current. The burnt gases and sulphur; also. travel.v in; counter-current The burnt gases escaping through the flue 25 and a stack (not shown).
  • the superheated sulfur vapor and the preheated coal react inside the reaction retort I3.
  • the vapor of crude carbon disulphide (containing sulphur and non-condensable gases) passes through the shutters M to a heat exchange coil 31 in a column 36 where the crude carbon disulfide and intermixed gases are reduced in temperature after which such gases pass to the sulphur separating column 49.
  • Liquid sulphur is sprinkled into the top portion of the column 40 from a source presently to be explained in order to bring about a separation of the sulphur contained in the crude disulfide gas fed into column 49 from coil 31.
  • the carbon disulfide leaving the top of column 49 is free of sulphur and passes from such column into the top of a condenser 30.
  • the carbon disulfide is caused to condense in the condenser 30 and is drawn therefrom into a cylinder 35 which receives both liquid carbon disulfide and non-condensible gases.
  • This carbon disulfide is free of sulphur but is saturated with dissolved sulphurated gases which are removed in the column 36 by evaporization of such gases by means of the heat transferred to the column by coil 31,
  • the pure carbon disulfide flowing from the lower section of column 36 is then cooled in a cooler 39.
  • the non-condensible gases issuing from the cylinder 35 pass through a reflux cooler 31 and are then forced toward the plant exit by means of an extractor 32.
  • a part of the condensed carbon disulfide emanating from the column 39 and cylinder 35 is transferred by means of conduit 29 to the column 40 through a regulator valve 29 which is controlled by the temperature at a selected point 40' in the separating column 40.
  • the substantially pure sulphur obtained at the bottom of separating column 46 is returned to the heater 2! by means of a conduit 46.
  • the vapors removed from the carbon disulfide in column 36 are introduced by means of a conduit 45 into the upper end of column 30 along with the vapors received from column 49.
  • the coal ashes are extracted by means of a gas-tight cleaning device 42 provided at the bottom of the reaction retort i3.
  • reaction retort I3 For starting the plant the reaction retort I3 is filled with coal which is then ignited at some suitable points. Through the difierent nozzles 14 air is blown in order to heat the coal to reaction temperature.
  • the reaction retort or oven 13 may be simply insulated with a convenient heat-insulating material. In this case the losses of heat should be low so that the temperature of the mass is held at a level sufficient to obtain a satisfactory reaction between the sulphur with the coal.
  • Any losses of heat may be compensated by providing an external source of heat.
  • reaction retort [3 may be placed inside the superheating section H! where the pre-treatment of the sulphur component is effected.
  • the sulphur vapor might also be directed to the bottom from the top portion thereof.
  • a vertically extending heat-insulated reaction retort comprising in combination, a vertically extending heat-insulated reaction retort, a vertically extending heat-insulated preheating chamber positioned above said retort and having its lower portion in communication with thejupperportion of said retort, means for feeding carbonaceous material into the upper portion of said preheating chamber, a burner for injecting a combustible gas and air into an intermediate portion of said chamber for combustion therein for heating said carbonaceous material whereby heated carbonaceous material is delivered into said retort, a gas pump for withdrawing combustible gas from the upper portion of said preheating chamber and a conduit for returning a portion thereof to said burner, a sulfur vaporizing and superheating furnace, a conduit for supplying another portion of said combustible gas to said furnace, a burner for burning said other portion of said combustible gas in said furnace to produce heat for vaporizing sulfur and superheating the resulting vapor,
  • Apparatus for producing carbon disulfide comprising in combination, a vertically extending heat-insulated reaction retort, a vertically extending heat-insulated preheating chamber positioned above said retort and having its lower portion inconstantly open communication with the upper portion of said retort, feeding means for feeding carbonaceous material into the upper portion of said preheating chamber, said feeding means including a sealing device for restricting entrance of air into said preheating chamber through said feeding means, a burner positioned intermediate the upper and lower portions of said preheating chamber for introducing a mixture of air and combustible gas into said preheating chamber for combustion therein, whereby heated carbonaceous material is delivered into said retort, a gas pump for withdrawing gases due to said combustion from the upper portion of said preheating chamber to prevent entrance of said gases into said retort, sulfur vaporizing apparatus including a burner, a conduit for delivering a portion of the gases from said gas pump to said burner, a conduit for delivering

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Description

1954 E. CHARLES 2,670,277
METHOD AND APPARATUS FOR THE CONTINUOUS PRODUCTION OF CARBON DISULPHIDE Filed June 10, 1949 fiver/far:
Ere/ven- CHARLES Patented Feb. 23, 1954 METHOD. AND APPARATUS FOR THE CON- TINUOUS PRODUCTION OF CARBON DI- SULPHIDEK Ernest Charles, Clamecy, France, assignorto Soci'ete des Produits Chimiques de Clamecy Clamecy, France, a corporation of France- Application June .10, 1949,, Serial-No. 98,346 Glaimspriority, application France June 12, 1948- 2Glaimsi I This; invention relates to a method and to meansforreacting coaland suliur-for the formation of carbon disulfi'de.
anobject" ortheinvention to-organize the formation of the carbon disul'fideinsuch manner as. to reduce to a minimum the amount of heat energy to betintroduced-from the outside into the zone of reaction.
' Thenew methodis characterizedessentially by the introduction into the reaction zone, of thecoalfreed-from volatile gases and the sulfur after bothhave been preheated to the reaction temperature. The losses of heat in this zone are prevented by heat insulating or slightly heating the, reaction vessel; the-heat produced in the reaction being utilized underthe-best possible conditionsfor preheating thesulphur and the coal and obtaining-theinexpensive purification of the carbondisulphide. f
It is known that the reaction between" sulfur and coal (which is endothermic at-"ordinary temperature) is exothermic at the reaction temperature, ranging fromabout 900 and 1,000 C. Thus the productionof carbon disulphide the heat energy tobe provided from the outside is consumed in the preheating of the sulfur and the coal.
VWhenoperating batchwise with heat energy supplied from, the outside unsatisfactory results, are obtained because" the: transmission of heatthrough the charcoal layer'ispoor. Electric heat energyfori raising the-temperature, of the sulphur andthe coalis expensive. The main objection tow the introduction oflcharcoal at a low temperature into-the oven is that this product has a high gas content, so that. a large. amountof sulphur will be lost i'rrthe non-condensable gases.
Therefore according to the presentinvention the gases are removed from; the charcoal when heating; itand then exhausted from the; reaction oven.
'Eheequipment whereby the: new process may be carriedtinto efiect comprises-essentiallyz-r averticalreaction retort having: little or no loss of heat, a vertical coal preheating retort, placed on top of the, reaction retort and. heated by means otiniected-air and gas, a superheater adapted; to heat the sulphur vapor to the reaction temperameans for melting; and. vaporizing the sulphur treated and for rectifying the carbon disulphide.
In. the drawing affixed to this specification and forming part thereof the invention is illustrated diagrammatically by way of example.
Referring to the drawing coal (in any form, natural or agglomerated, with or without sulphuration catalysts or substances adapted to change the melting temperature of the ashes) is fed into the hopper i. It is then dischargedinto the heat-insulated coal preheating retort l0 through the medium of a gas-tight distributor 2. During itsdownwardtravel the coal is heated by passing in front ofthe blast-pipe 9 fed with air' under pressure from a suitable source (not shown) through a conduit 8 and with gases fed from the distillation of the charcoal through a conduit 1. The red-hot charcoal descends into the upper portionof the'retort [3 which is kept under constant pressure by means of the automatic reguIatorSB having its pressure-intake at $4. The coal distillation gases aretaken up at 3 by the fan 4 and forced through the blast-pipe 9 into a hearth of the sulfur superheater" It. In order to prevent the vapor from penetratingi'ntothe coal pre-heatingretort Ill a'very low pressure is maintainedin the bottom portion of this retort, and this very low pressure is transmitted-through the pressure intake I l to the automatic regulator 5. Due to the considerable loss of charge 0c curring between the two ends of the pre-heating oven I0 the amount of inert gas penetrating into the reaction retort I3 is insignificant. V
The solid sulphur introduced into the hopper 26 is fed by the screw conveyor 21 into the melting tunnel 24% provided wi'tl'r an agitator 23; This tunnel is heated by means of a cluster of tubularelements.
The molten sulphur passes through the filter 28 anoiis then fed to thebottom portion of thevaporizer 2i. The sulphur vapor is then superheated in the superheater l9 positioned in the compartment 2!? oi the'apparatus and is introduced at I 2 into the top-portionof the reactionv retortl3 Thefore-hearthl 8-is partially fed at- I 5 with thegases from the distillation of the coal in the pre-heating retort l0, the complementary heat units beingfed' through a conduit 6 from any suitable source on the outside-. In addition airis' injected: at Hi,
The. combustion. gases during. their travel meet thesulphur: zit-Miami melt it: and the molten sul:-.
phi-1r: is vaporized in; heater 2i. It is therefore apparent that the hot-gases and the-sulphur vapor. travel in a counter-current. The burnt gases and sulphur; also. travel.v in; counter-current The burnt gases escaping through the flue 25 and a stack (not shown).
The superheated sulfur vapor and the preheated coal react inside the reaction retort I3. The vapor of crude carbon disulphide (containing sulphur and non-condensable gases) passes through the shutters M to a heat exchange coil 31 in a column 36 where the crude carbon disulfide and intermixed gases are reduced in temperature after which such gases pass to the sulphur separating column 49. Liquid sulphur is sprinkled into the top portion of the column 40 from a source presently to be explained in order to bring about a separation of the sulphur contained in the crude disulfide gas fed into column 49 from coil 31. The carbon disulfide leaving the top of column 49 is free of sulphur and passes from such column into the top of a condenser 30. The carbon disulfide is caused to condense in the condenser 30 and is drawn therefrom into a cylinder 35 which receives both liquid carbon disulfide and non-condensible gases. This carbon disulfide is free of sulphur but is saturated with dissolved sulphurated gases which are removed in the column 36 by evaporization of such gases by means of the heat transferred to the column by coil 31, The pure carbon disulfide flowing from the lower section of column 36 is then cooled in a cooler 39. The non-condensible gases issuing from the cylinder 35 pass through a reflux cooler 31 and are then forced toward the plant exit by means of an extractor 32.
In order to supply the separating column 40 with the necessary liquid sulphur to effect the separation a part of the condensed carbon disulfide emanating from the column 39 and cylinder 35 is transferred by means of conduit 29 to the column 40 through a regulator valve 29 which is controlled by the temperature at a selected point 40' in the separating column 40. The substantially pure sulphur obtained at the bottom of separating column 46 is returned to the heater 2! by means of a conduit 46.
The vapors removed from the carbon disulfide in column 36 are introduced by means of a conduit 45 into the upper end of column 30 along with the vapors received from column 49.
The coal ashes are extracted by means of a gas-tight cleaning device 42 provided at the bottom of the reaction retort i3.
For starting the plant the reaction retort I3 is filled with coal which is then ignited at some suitable points. Through the difierent nozzles 14 air is blown in order to heat the coal to reaction temperature.
The reaction retort or oven 13 may be simply insulated with a convenient heat-insulating material. In this case the losses of heat should be low so that the temperature of the mass is held at a level sufficient to obtain a satisfactory reaction between the sulphur with the coal.
Any losses of heat may be compensated by providing an external source of heat.
On the other hand, the reaction retort [3 may be placed inside the superheating section H! where the pre-treatment of the sulphur component is effected.
The sulphur vapor might also be directed to the bottom from the top portion thereof.
Various changes may be made in the process as well as in the means as described by way of example in the above specification without departing from the spirit of the invention or sacrificing the advantages thereof.
I claim:
1. Apparatus for producing carbon disulflde,
comprising in combination, a vertically extending heat-insulated reaction retort, a vertically extending heat-insulated preheating chamber positioned above said retort and having its lower portion in communication with thejupperportion of said retort, means for feeding carbonaceous material into the upper portion of said preheating chamber, a burner for injecting a combustible gas and air into an intermediate portion of said chamber for combustion therein for heating said carbonaceous material whereby heated carbonaceous material is delivered into said retort, a gas pump for withdrawing combustible gas from the upper portion of said preheating chamber and a conduit for returning a portion thereof to said burner, a sulfur vaporizing and superheating furnace, a conduit for supplying another portion of said combustible gas to said furnace, a burner for burning said other portion of said combustible gas in said furnace to produce heat for vaporizing sulfur and superheating the resulting vapor, a conduit for supplying the resulting superheated sulfur vapor to the upper portion of said retort, and a conduit for withdrawing crude carbon disulfide vapors from the lower portion of said retort.
2. Apparatus for producing carbon disulfide, comprising in combination, a vertically extending heat-insulated reaction retort, a vertically extending heat-insulated preheating chamber positioned above said retort and having its lower portion inconstantly open communication with the upper portion of said retort, feeding means for feeding carbonaceous material into the upper portion of said preheating chamber, said feeding means including a sealing device for restricting entrance of air into said preheating chamber through said feeding means, a burner positioned intermediate the upper and lower portions of said preheating chamber for introducing a mixture of air and combustible gas into said preheating chamber for combustion therein, whereby heated carbonaceous material is delivered into said retort, a gas pump for withdrawing gases due to said combustion from the upper portion of said preheating chamber to prevent entrance of said gases into said retort, sulfur vaporizing apparatus including a burner, a conduit for delivering a portion of the gases from said gas pump to said burner, a conduit for delivering sulfur gases from said vaporizing apparatus into the upper portion of said retort, and a conduit for withdrawing crude carbon disulfide vapors from the lower portion of said retort.
ERNEST CHARLES.
References Cited in the file of this patent UNITED STATES PATENTS Number Name Date 1,615,659 Siedler Jan. 25, 1927 1,918,033 Griswold July 11, 1933 2,046,818 Harkness July 7, 1936 2,052,297 Iddings Aug. 25, 1936 2,079,017 Iddings et a1 May 4, 1937 2,107,264 Baxter Feb. 1, 1938 2,141,758 Merriam Dec. 27, 1938 2,392,629 Avery Jan. 8, 1946 2,443,854 Ferguson June 22, 1948 2,480,639 Ferguson Aug. 30, 1949

Claims (1)

1. APPARATUS FOR PRODUCING CARBON DISULFIDE, COMPRISING IN COMBINATION, A VERTICALLY EXTENDING HEAT-INSULATED REACTION RETORT, A VERTICALLY EXTENDING HEAT-INSULATED PREHEATING CHAMBER POSITIONED ABOVE SAID RETORT AND HAVING ITS LOWER PORTION IN COMMUNICATION WITH THE UPPER PORTION OF SAID RETORT, MEANS FOR FEEDING CARBONACEOUS MATERIAL INTO THE UPPER PORTION OF SAID PREHEATING CHAMBER, A BURNER FOR INJECTING A COMBUSTIBLE GAS AND AIR INTO AN INTERMEDIATE PORTION OF SAID CHAMBER FOR COMBUSTION THEREIN FOR HEATING SAID CARBONACEOUS MATERIAL WHEREBY HEATED CARBONACEOUS MATERIAL IS DELIVERED INTO SAID RETORT, A GAS PUMP FOR WITHDRAWING COMBUSTIBLE GAS FROM THE
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2859101A (en) * 1952-05-21 1958-11-04 Shikoku Kasei Kogyo Company Lt Reaction furnace for producing carbon disulphide
CN103803505A (en) * 2014-03-12 2014-05-21 四川宏达股份有限公司 Overheating sulfur steam production technology
CN104555938A (en) * 2015-01-20 2015-04-29 上海三夫工程技术有限公司 Preparation method of high-purity sulfur gas serving as reducing gas

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1615659A (en) * 1925-06-29 1927-01-25 Ig Farbenindustrie Ag Manufacture of carbon disulphide
US1918033A (en) * 1927-02-07 1933-07-11 Dow Chemical Co Apparatus for the production of carbon disulphide
US2046818A (en) * 1933-06-30 1936-07-07 Gen Chemical Corp Sulphur vaporizer
US2052297A (en) * 1933-10-18 1936-08-25 Gen Chemical Corp Carbon bisulphide process
US2079017A (en) * 1933-10-18 1937-05-04 Gen Chemical Corp Apparatus for heating materials
US2107264A (en) * 1936-01-03 1938-02-01 Ici Ltd Process for the production of carbon disulphide
US2141758A (en) * 1937-10-20 1938-12-27 Gen Chemical Corp Manufacture of carbon bisulphide
US2392629A (en) * 1942-01-21 1946-01-08 Little Inc A Method of making carbon bisulphide
US2443854A (en) * 1943-03-06 1948-06-22 Standard Oil Dev Co Fluidized-solid process for forming carbon disulfide
US2480639A (en) * 1947-07-03 1949-08-30 Standard Oil Dev Co Preparation of carbon disulfide

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1615659A (en) * 1925-06-29 1927-01-25 Ig Farbenindustrie Ag Manufacture of carbon disulphide
US1918033A (en) * 1927-02-07 1933-07-11 Dow Chemical Co Apparatus for the production of carbon disulphide
US2046818A (en) * 1933-06-30 1936-07-07 Gen Chemical Corp Sulphur vaporizer
US2052297A (en) * 1933-10-18 1936-08-25 Gen Chemical Corp Carbon bisulphide process
US2079017A (en) * 1933-10-18 1937-05-04 Gen Chemical Corp Apparatus for heating materials
US2107264A (en) * 1936-01-03 1938-02-01 Ici Ltd Process for the production of carbon disulphide
US2141758A (en) * 1937-10-20 1938-12-27 Gen Chemical Corp Manufacture of carbon bisulphide
US2392629A (en) * 1942-01-21 1946-01-08 Little Inc A Method of making carbon bisulphide
US2443854A (en) * 1943-03-06 1948-06-22 Standard Oil Dev Co Fluidized-solid process for forming carbon disulfide
US2480639A (en) * 1947-07-03 1949-08-30 Standard Oil Dev Co Preparation of carbon disulfide

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2859101A (en) * 1952-05-21 1958-11-04 Shikoku Kasei Kogyo Company Lt Reaction furnace for producing carbon disulphide
CN103803505A (en) * 2014-03-12 2014-05-21 四川宏达股份有限公司 Overheating sulfur steam production technology
CN104555938A (en) * 2015-01-20 2015-04-29 上海三夫工程技术有限公司 Preparation method of high-purity sulfur gas serving as reducing gas
CN104555938B (en) * 2015-01-20 2017-01-18 上海三夫工程技术有限公司 Preparation method of high-purity sulfur gas serving as reducing gas

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