US1051876A - Process of obtaining by-products from the gaseous distillation of fuels. - Google Patents

Process of obtaining by-products from the gaseous distillation of fuels. Download PDF

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US1051876A
US1051876A US67764512A US1912677645A US1051876A US 1051876 A US1051876 A US 1051876A US 67764512 A US67764512 A US 67764512A US 1912677645 A US1912677645 A US 1912677645A US 1051876 A US1051876 A US 1051876A
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tar
bath
acid
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/24Sulfates of ammonium
    • C01C1/242Preparation from ammonia and sulfuric acid or sulfur trioxide

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  • This invention relates to'processes of obtaining by-pi'oducts from the gaseous distillation of fuels, and more particularly to im proved methodsof manufacture of ammonium sulfate from distillation gases, and especially gases from coke ovens, gas IGtOItS and the like.
  • my I invention comprises withdrawing distillation gases evolved during the first part of the coking period and containing the greater part of tar yield separately and distinct from the latter quantities of gas containing little or no tar, cooling tie first quantities to condense tar and gas Water, and simultaneously but separately conducting both quantities of gases into the same they are drawn by pipe acid saturation bath and separately withdrawing both quantities of gas from the bath for use in heating the retorts or ovens and for market purposes.
  • 1 represents a battery of coke ovens or gas furnaces, shown in a longitudinal, irregular section, B being the forward end of one oven and A the rear end of another oven.
  • Each oven is periodically filled and discharged as usual.
  • the gases of distillation being of a higher calorific value and containing all'or the greater part of the tar yield from the oven charge, are drawn of from ovens lettered A (for instance) through standpipes '2 (provided for each oven')- into the gas main 3 which connects all of the similar standpipes of the ovens.
  • the gas main the gas is conducted through pipe i-into the tar drag 5, in which most of the tar is removed in the well known manner. From the drags the gases are con ducted by pipe 6 into coolers 7, from whence 8 into blower 9 which in turn forces such gases through tar extractor 10 where the last traces of tar are removed. After these gases are thuscooled and freed of their tar (and incidentally of a small part of their ammonia), they are without reheating conducted directly into the saturation vessel 12, through ipe 11, the saturation vessel containing sul f uric acid or an acid salt solution.
  • the gases from pipe 11 enter the annular subchamber 13. In passing through the absorption'lye the gases give up their ammonia to the acid and collect in the top part of the vessel 12 above the bath,
  • pipe 14 from whence they are led away by pipe 14 to be used for illuminating purposes or consumed in gas engines, or the like.
  • the tar free and hot gases leave the suction devices through pipe 19 to be forced directly into the saturation vessel 12 before referred to.
  • the temperature of these gases when conducted into the saturation vessel is preferably kept'slightly above the condensation point of the gases, whichis about 7 0 C. for retort gases and 80 C. for coke oven gases, the stated difference being due to coal used in gas works being practically free from moisture, while on the other hand the coal used in coke ovens is' frequently dampened to produce a better quality coke.
  • Any cooling means maybe employed in this lean gas system to maintain such gases at the proper temperature if too hot f orthe purpose they leave the ovens In view and when, for instance, it maybe desirabletocool them below the dew point.
  • the hot gases pass through the bath in the manner indicated bythe'arrows and collect in the inner annular'chamber 20, are con ducted through pipe 21into cooler 22 from whence theyiare, returned by'pipe 23 to the coke ovens'to serve forheating'purposes, if desired. If rthesef-igasesgj after passage through the-abidbatharveused for heating the ovens or retorts, the final pooling of sue gases may, ofcourse, be omitted. Ainmm nium sulfate formedlmay be removed from the saturation vessel 12in any desired manner.
  • ammonium sulfate which comprises collecting coal gases rich in tar. cleaning the same of tar and water, cooling the same and passing through sulfuric acid to form sulfate; and simultaneously but separately collecting gases less rich in tar, and passing through the sulfuric acid to'heat the same and form sulfate, collectingthe gases from said acid separately; and collecting the ammonium sulfate formed.
  • ammonium sulfate the process which comprises simultaneously. withdrawing from different sources, ammonia containing gases of different compositions, passing one such gas through an acid to heat the same and form sulfate, sii'miltaneously cleaning and cooling the other gas and passing it separately through the same acid to form sulfate, and separately collecting said gases after passage through said acid.
  • ammoniacontaining. gases of different compositions one such gas containing a relatively large percentage of tar as compared to the other gas, cleaning and cooling the gas containing the larger percentage of tar and passing the same through an acid bath to form sulfate, passing the other gas direct to the acid bath to heat the same and form sulfate, and separately collecting said gases from the acid bath, after formation of the salt.
  • ammonium sulfate In the manufacture of ammonium sulfate, the process which comprises cleaning and passing ammonia containing gases from one source through an acid bath to heat the same and form sulfate, simultaneously but separately cleaning, cooling and passing gases from another source through said acid bath to form ammonium sulfate, collecting andsenarating the products cleaned from both gases, distilling a portion of them to recover ammonia, and conducting such ammonia into said acid bath to form sulfate.

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Industrial Gases (AREA)

Description

W. FEICKS. PROCESS OF OBTAINING BY'PRODUGTS FROM THE GASEOUS DISTILLATION 0F FUELS.
APPLICATION FILED I'EB.14, 1012. 7
1,051,876. Patented Feb. 4, 1913.
I/VVE/VTOF? MIA/E5555: fg/
WILLIAM FEICKS, OF BLOOMFIELD, NEW JERSEY.
PROCESS OF OBTAIN G BY-IPRODUCTS FROM THE GASEOUS DISTILIJATION OF FUELS.
Specification of Letters Patent.
Patented Feb. 4,1913.
Application filed February 14, 1912. Serial No. 677,645..
I 0 all whom it may concern Be it known that I, YVILLIAM FEICKS, a subject of the German Emperor, residing at Bloomfield, in the county State of New Jersey, have invented new and useful Improvements in Processes of Ohtaining By-Products from the Gaseous Distillation of Fuels, of which the following is a specification. v
This invention relates to'processes of obtaining by-pi'oducts from the gaseous distillation of fuels, and more particularly to im proved methodsof manufacture of ammonium sulfate from distillation gases, and especially gases from coke ovens, gas IGtOItS and the like.
:In processes for the manufacture of ammonium sulfate from distillation gases heretofore known, the gases from coke ovens, gas furnaces and the like are usually cleaned and cooled so as to condense tar and water, after which they are either directly or in a superheated state conducted into a sulfuric acid bath for the formation of ammonium sulfate. Or, according to other known methods, the first quantities of gases from the retorts or coke ovens containing I the greater part of tar yield are divided from the latter quantities of the ases containing relatively little or no tar, and are freed rom tar, then combined with the latter quantities and passedto the acid bath.v
An objection to the first mentioned process is that the whole of the ammoniacal liquor from the gases is condensed in cooling such gases to eliminate tar and water and thus comparatively large apparatus is necessary for the cooling, and extracting step,
since, as stated, the whole of the gases evolved by the ovens are sent through the apparatus. Furthermore, the superheating of the gases after they have been cooled re quires special apparatus, and this is a serious objection from the manufacturing standpolnt and tends to increase the cost of manufacture. I process, no superheatin of the gas is effected, as it has been fbund that while in most cases the heat transmitted to the acid saturationbath, due to the chemical reaction between the ammonia and-acid, may suffice to keep the bath at a sulfate-forming 1 temperature, this recess cannot be carried out under all co itions, for there may not of Essex and In the second named above a] be suflicient self-generating heat in the bath and the gases ma be below the correct temperature for eflicient o eration of the process. Also, it frequently happens that the ases contain relatively large quantities of fixed ammonia, whose heat of reaction with sulfuricacid is relatively small, in which event additional 'heatin means should be employed. There are a so a few other factors governing the above, so that the su erheating of the gases before conducting t cm into the saturation bath cannot be altogether dispensed with.
According to the last named known pr0cess, there are no cooling or reheating steps, and there also bein no condensates to be treated in stills, di 'culties have been encountered in efli'ciently removing the tar from the oven gases at hi h temperature, even with a. tar injector. hand, accordin to the process now under discusion, the first and larger quantities of gases from theretorts or ovens are cooled and thus freed of their tar, upon the comf, onthe other bination of such tar-freed gases with the to provide a process of making ammonium SLIlfatQ,WlIiCh process may be performed with the aid of smaller and thus cheaper apparatus; and to generally more economicall y and effectually recover the by-products from the gases than has been hitherto accomplished. through any known'process.
With these and other objects in View, my I invention comprises withdrawing distillation gases evolved during the first part of the coking period and containing the greater part of tar yield separately and distinct from the latter quantities of gas containing little or no tar, cooling tie first quantities to condense tar and gas Water, and simultaneously but separately conducting both quantities of gases into the same they are drawn by pipe acid saturation bath and separately withdrawing both quantities of gas from the bath for use in heating the retorts or ovens and for market purposes. In this manner all disadvantages of the previous named processes are obviated, there being no super-- heating of the cooled gases necessary, since the latter quantities of gases which enter the bath at a comparatively high temperature serve to maintain such temperature of the bath that the salt is easily and effectually The accompanying drawings illustrate diagrammatically one form of a plant for carrying out my processes in connection with coke ovens.
In the drawings, 1 represents a battery of coke ovens or gas furnaces, shown in a longitudinal, irregular section, B being the forward end of one oven and A the rear end of another oven. Each oven is periodically filled and discharged as usual. During the first part of the coking period the gases of distillation, being of a higher calorific value and containing all'or the greater part of the tar yield from the oven charge, are drawn of from ovens lettered A (for instance) through standpipes '2 (provided for each oven')- into the gas main 3 which connects all of the similar standpipes of the ovens.-
lfro-m the gas main the gas is conducted through pipe i-into the tar drag 5, in which most of the tar is removed in the well known manner. From the drags the gases are con ducted by pipe 6 into coolers 7, from whence 8 into blower 9 which in turn forces such gases through tar extractor 10 where the last traces of tar are removed. After these gases are thuscooled and freed of their tar (and incidentally of a small part of their ammonia), they are without reheating conducted directly into the saturation vessel 12, through ipe 11, the saturation vessel containing sul f uric acid or an acid salt solution. The preferred tem perature of the gases flowing through pipe lllies between approximately 1O" and centigrade, but, of course, the invention is not to be limited to operationupon gases of these specific temperaturespa'lhe saturation vesselhere' shown is of novel construction, and is not claimedhere, but is to fornrthe subjectmattergof an applicationisoon befiled by me. The gases from pipe 11 enter the annular subchamber 13. In passing through the absorption'lye the gases give up their ammonia to the acid and collect in the top part of the vessel 12 above the bath,
from whence they are led away by pipe 14 to be used for illuminating purposes or consumed in gas engines, or the like.
Simultaneously with the above, the gases of distillation of other furnaces (for in stance B) comprising the battery of ovens and whose coal charges are in their last stages of carbonization and are giving of? a poor gas practically free of tar, are con ducted through the standpipes 15, one of which is provided for each oven, and into the main 16 which runs along the length of the battery. These gases are conducted by pipe 17 to the suction device 18, which, as illustrated, is a tar injector. The tar injector has for its object to remove any traces of tar which may be left in these gases; In cases where such gases contain very little or no tar so as to be unobjectionable, an ordinary blower may be used to thesame advantage. The tar free and hot gases leave the suction devices through pipe 19 to be forced directly into the saturation vessel 12 before referred to. The temperature of these gases when conducted into the saturation vessel is preferably kept'slightly above the condensation point of the gases, whichis about 7 0 C. for retort gases and 80 C. for coke oven gases, the stated difference being due to coal used in gas works being practically free from moisture, while on the other hand the coal used in coke ovens is' frequently dampened to produce a better quality coke. Any cooling means maybe employed in this lean gas system to maintain such gases at the proper temperature if too hot f orthe purpose they leave the ovens In view and when, for instance, it maybe desirabletocool them below the dew point.
The hot gases pass through the bath in the manner indicated bythe'arrows and collect in the inner annular'chamber 20, are con ducted through pipe 21into cooler 22 from whence theyiare, returned by'pipe 23 to the coke ovens'to serve forheating'purposes, if desired. If rthesef-igasesgj after passage through the-abidbatharveused for heating the ovens or retorts, the final pooling of sue gases may, ofcourse, be omitted. Ainmm nium sulfate formedlmay be removed from the saturation vessel 12in any desired manner..
.If the secondhand poorer quality of gases are obtained-in excessof that required to heat the ovens, in connection with other heating means, the pressure regulator 24%,
upon exceeding a certain pressure in the second system, automatically allows a larger or smaller quantity of gases to pass through pipe 25, through regulator 24 and pipe 26, back into the first described system handling the richer gases, thus making the whole operation perfectly selfgovcrning. The quantities of gases sent through either system during the duration of a coking period depends upon the rapidity with which the coking of the charge progresses, and further on the temperature to be maintained in the acid bath and some other factors, and may in different plants vary within wide limits.
The tar and other condensates from the tar drag 5, coolers 7, tar extractor 10 and suction device 18, are conducted by a system of pipes into settlin tank 27, from which the tar flows into tanks 28, and the gas water into tank 29. From this latter tank the gas water is lifted by pump 30 and forced in still 31, where the ammonia may be drawn off in the usual manner with steam. The ammonia vapors mixed with the steam leave the still by pipe 32 and after being dried as usual in a condenser 33 are led by pipe 34 into pipe 19 ,and mixed with gas passing therethrough to the saturation vessel 12 or may be conducted direct to such vessel.
It is to be understood that a whole battery of ovens may be operated upon at the same time, the rich gases from some of such ovens being conducted through one process, while the poorer gases from the other ovens in a different stage of carbonization are being conducted through the other process.
lVhat I claim is 1. The process of manufacturing ammonium sulfate which comprises collecting coal gases rich in tar. cleaning the same of tar and water, cooling the same and passing through sulfuric acid to form sulfate; and simultaneously but separately collecting gases less rich in tar, and passing through the sulfuric acid to'heat the same and form sulfate, collectingthe gases from said acid separately; and collecting the ammonium sulfate formed.
2. In the manufacture of ammonium sulfate, the process which comprises simultaneously. withdrawing from different sources, ammonia containing gases of different compositions, passing one such gas through an acid to heat the same and form sulfate, sii'miltaneously cleaning and cooling the other gas and passing it separately through the same acid to form sulfate, and separately collecting said gases after passage through said acid.
3. In the manufacture of ammonium sulfate, the process which comprises simultaneously withdrawing from different sources ammonia containing gases of different compositions, cooling and treating one such gas to separate tar and ammonia water therefrom, partially cooling the other gas and treating it to remove tar, simultaneously passing both gases through the same sulfate forming bath and separately withdrawing said gases from said bath.
.4. In the manufacture of ammonium sulfate, the process which comprises simultaneously withdrawing from different sources,
ammoniacontaining. gases of different compositions, one such gas containing a relatively large percentage of tar as compared to the other gas, cleaning and cooling the gas containing the larger percentage of tar and passing the same through an acid bath to form sulfate, passing the other gas direct to the acid bath to heat the same and form sulfate, and separately collecting said gases from the acid bath, after formation of the salt.
5. In the manufacture of ammonium sulfate, the process which comprises simultaneously withdrawing from different sources ammonia containing gases of different compositions, cleaning one such gas of any tar and passing such gas without cooling to an acid bath to heat the same to form sulfate, and simultaneously cleaning and cooling the other gas and passing it separately from. the first mentioned gas into said acid bath to form an ammonium salt.
6. In the manufacture of ammonium salts from coke ovens or gas furnace gases, the process which comprises withdrawing am; monia containing gases of difierent compositions from different ovens, passing one such gas through an acid bath to heat the same and to form a salt and burning such gas under the furnaces, simultaneously cleaning and cooling the other gas and conducting it to the acid bath to form a salt and thence to a storage tank, and automatically passing gas of the first named composition into gas of the second named composition, when consumption of the gas burning under the furnaces diminishes.
7. In the manufacture of ammonium sulfate, the process which comprises cleaning and passing ammonia containing gases from one source through an acid bath to heat the same and form sulfate, simultaneously but separately cleaning, cooling and passing gases from another source through said acid bath to form ammonium sulfate, collecting andsenarating the products cleaned from both gases, distilling a portion of them to recover ammonia, and conducting such ammonia into said acid bath to form sulfate.
8. In the manufacture of ammonium sulfate, the process which comprises treating an ammoniacal gas fromjone source to remove tar, and passing 'such tar-free gas through an acid bath to heat the same and form a sulfate; simultaneously but separately treating another ammoniacal gas from a different source to form condensates'in' eluding tar and gas Water, passing such gas In testimony whereof I have hereunte set to said acid to form sulfate cellecting said my hand, in the presence of W tnesses.
condensates together with the tar removed from said first named gas, separating the WILLIAM E tax" from the gas Water, distilling the latter. Witnessesz' S. K. FEIOKS,
to form ammonia and passing said ammonia M. K. MERKLE to said acid bath to form sulfate.
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