US852510A - Apparatus for the treatment of sulfids and other ores. - Google Patents

Apparatus for the treatment of sulfids and other ores. Download PDF

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US852510A
US852510A US36533804A US1904365338A US852510A US 852510 A US852510 A US 852510A US 36533804 A US36533804 A US 36533804A US 1904365338 A US1904365338 A US 1904365338A US 852510 A US852510 A US 852510A
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acid
ore
chamber
ores
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George Edward Kingsley
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2/00Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms
    • C07C2/54Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition of unsaturated hydrocarbons to saturated hydrocarbons or to hydrocarbons containing a six-membered aromatic ring with no unsaturation outside the aromatic ring
    • C07C2/56Addition to acyclic hydrocarbons
    • C07C2/58Catalytic processes
    • C07C2/62Catalytic processes with acids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/008Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
    • B01J8/009Membranes, e.g. feeding or removing reactants or products to or from the catalyst bed through a membrane

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  • My invention relates to improvements in apparatus for the economical extraction of metals from sulfide and other ores in a form ready for market, and the production during the process, of valuable by-products. I fur ther aim to construct the apparatus so that the process is cyclic in its nature and therefore conducted with comparatively small loss of the original re-agents employed.
  • myinvention consists essentially of the arrangement of the parts hereinafter more specifically described and then definitely claimed.
  • Figure 1 is a front elevation of the plant, partly in section on the line indicated in Fig. 2.
  • Fig. 2 is an end elevation of the plant, partly in section;
  • Fig. 1, 1, 2, 3 and 4 are square chambers provided with false bottoms 12 and preferably lined with thin fire brick, porcelain, enamel, or other acid resisting material. These chambers are formed as shown by subdividing a long tank. These chambers have openings in their tops provided with doors 34, by means of which they may be tightly sealed. Above and behind these chambers are arranged a series of similar chambers 5, adapted to receive dilute acid. The bottom of each of these chambers is connected with the top of the adjacent chamber by means of a pipe 26.
  • each of the chambers 1, 2, 3 and 4 is connected with the top of the next chamber in the series by means of a bentpipe 8, the lower end of each pipe being provided with a perforated nozzle or distributer 15.
  • Each dilute acid. receptacle is provided with a spigot 14, arranged to discharge through the opening in the top of the corresponding ore receptacle in fi'ont of it.
  • Each of the ore receptacles 1, 2, 3 and 4 is also provided with a spigot 25, arranged to discharge into the series of vats 32.
  • the 6 is an acid reservoir, and 7 a water reservoir, connected by the pipe 13, provided with the stop cocks 16 and 17
  • This pipe 13 is connected by suitable branches with the chambers 1, 2, 3 and 4, and these branches are provided with the stop cocks 18.
  • the top of the chamber 4 is connected with the bottom of the acid chamber 5, above and behind it, by means of the inverted U-shaped tube 9.
  • Adjacent to the chamber 4 is a retort 20, provided with a furnace 21.
  • the pipe 19, leading from the retort passes through the chambers 1, 2, 3 and 4, near their bottoms. The pipe then leads upward and passes into the end chamber 5, above and behind the chamber 1.
  • the retort is shown provided with suitable means for feeding acid thereto, but such forms no part of my invention.
  • the operation of the apparatus is substantially as follows: The ore is first ground, or crushed, to pass through a 30 or 40 mesh sieve, and then placed in the ore chambers 1, 2, 3 and 4, through the air-tight fitting doors 34.
  • the acid is mixed to the proper strength in the receptacles 5.
  • Acid and water are then admitted from the chambers 6 and 7, through the pipe 13, into the ore chambers 1, 2, 3 and 4.
  • a suitable salt and acid are heated together in the retort, and the heat and vapors therefrom pass through the pipe 19 and raise the temperature of the contents of the ore chambers sufliciently to greatly stimulate the chemical action therein.
  • my apparatus is especially adapted to the treatment of sulfids, it may also be employed with almost any ores, except those containing a high percentage of iron, or those so intimately mixed with calcium compounds, as calcium carbonate, as not to permit of ready and inexpensive sorting.
  • the dilute nitric acid is allowed to flow from the reservoirs 5 into the chambers 14. Acid and water may be instead admitted directly to these chambers from the reservoirs 6 and 7.
  • the chambers 14 are thereupon made air tight.
  • the chambers 5, during the re-action, are partially filled with water, their original contents having been drawn off to supply the ore chambers. Of course, if the ore chambers are filled directly from the tanks 6 and 7, the chambers 5 will be filled with water in the first place.
  • nitrogen tetroxid is also formed in the gaseous form, and this, by combination with the water of the dilute acid, is de-composed, and forms nitric and nitrous acid, causing the ore to be exposed to the action of the acid in a nascent state, thus greatly increasing the energy of the re-action.
  • a certain proportion of the nitrogen tetroxid passes on into the reservoirs filled with water, and is there converted into nitric and nitroirs acid, and absorbed.
  • the nitrous acid can be converted into nitric acid, but, it may be pointed out, that a certain amount-of nitrous acid in the nitric acid appears to materially assist the latter in its action.
  • Any iron nitrate in the solution may be precipitated as a hydroxid by the action of carbon di-oxid, and upon being dried, and, if desired, calcined, is a valuable pigment.
  • the lead nitrate may be precipitated by a mixture of sodium carbonate and hydroxid to give a mixture of lead hydroxid and sodium nitrate, any nitric acid remaining in the solution being also converted into sodium nitrate.
  • Sodium nitrate obtained as above, may be employed, and when treated with sulfuric acid (made from the sulfur obtained from decomposition of the galena) generates the heat desired during the process, and thus forms part of the cycle.
  • a tank consisting of a series of compart ments, means to connect the top of each compartment to the bottom of the next compartment, means to permit the connection of the tops of adjacent compartments, means for excluding or admitting air to the first compartment of the series, and means for drawing 01? fluids from the tank,
  • a tank consisting of a series of connected compartments, each of said compartments except those at each end of the tank having not more than four outer radiating surfaces, pipes connecting the tops of adjacent compartments, valves in said pipes, means to exclude or admit air to said compartments and means to remove gases therefrom.
  • adjacent tanks each divided into compartments, means to connect each compartment to the next including a pipe to connect the last compartment of one tank to the first compartment of the other tank, means to exclude or permit access of air to the first tank, additional controllable connecting means between the compartments of the first tank and means for removing gases from the said first tank to the second.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Description

N0. 852,510. PATENTED'MAY 7, 1907. G. E. KINGSLEY.
APPARATUS FOR THE TREATMENT OF SULFIDS AND OTHER ORES. ATPLIOATION FILED DEC. 8, 1904. RENEWED MAR. 29, 1907.
2 SHEETS-SHEETI.
' WITNESSES I 1 v LVVENTOR. p1 M B14 W ATTORNE Y3 THE NORRIS PETERS can, WASHINGTON, a. c.
No. 852,510. 3 PATENTED MAY 7, 1907. G. E. KINGSLEY.
APPARATUS FOR TREATMENT OF SULFIDS AND OTHER ORES. APPLICATION FILED DEC]. 8, 1904. nmmwzn MAR. 29, 1907.
2 SHEETS-SHEET 2.
A TTORNE Y5 UNITED RTATRS PATENT OFFICE,
GEORGE EDWARD KIN GSLEY, OF TORONTO, ONTARIO, CANADA.
Specification of Letters Patent.
Patented May 7, 1907.
Application filed December 8, 1904. Renewed March 29,1907. Serial No, 365,338-
To all whmn it may concern.-
Be it known that I, GEORGE EDWARD KINGsLEY, of the city of Toronto, county of York, Province of Ontario, Canada, have invented certain new and useful Improvements in Apparatus for the Treatment of Sulfids and other Ores, of which the following is a specification.
My invention relates to improvements in apparatus for the economical extraction of metals from sulfide and other ores in a form ready for market, and the production during the process, of valuable by-products. I fur ther aim to construct the apparatus so that the process is cyclic in its nature and therefore conducted with comparatively small loss of the original re-agents employed.
With this object in view, myinvention consists essentially of the arrangement of the parts hereinafter more specifically described and then definitely claimed.
Figure 1 is a front elevation of the plant, partly in section on the line indicated in Fig. 2. Fig. 2 is an end elevation of the plant, partly in section;
In the drawings like letters of reference indicate corresponding parts in the different figures.
Referring particularly to Fig. 1, 1, 2, 3 and 4 are square chambers provided with false bottoms 12 and preferably lined with thin fire brick, porcelain, enamel, or other acid resisting material. These chambers are formed as shown by subdividing a long tank. These chambers have openings in their tops provided with doors 34, by means of which they may be tightly sealed. Above and behind these chambers are arranged a series of similar chambers 5, adapted to receive dilute acid. The bottom of each of these chambers is connected with the top of the adjacent chamber by means of a pipe 26.
The bottom of each of the chambers 1, 2, 3 and 4 is connected with the top of the next chamber in the series by means of a bentpipe 8, the lower end of each pipe being provided with a perforated nozzle or distributer 15.
' These pipes it will be noted are all internally located and all troubles due to leakage are thus avoided, both because the pipes are not subjected to contraction and expansion due to changes and irregularities in the tern erature of the atmosphere and because any eakage which may occur is Within the tank and therefore of no moment. Furthermore the cooling of the gases in their passage from one chamber to another is avoided and indeed the construction of the tanks is such as to prevent dissipation of heat since they present a minimum outside surface for radiation. The tops of these chambers are connected by the bent pipes 36, each having a stop cook 35 therein. In the chamber 1, an opening is formed in the side, near the top, closed by a suitable plug 37.
Each dilute acid. receptacle is provided with a spigot 14, arranged to discharge through the opening in the top of the corresponding ore receptacle in fi'ont of it. Each of the ore receptacles 1, 2, 3 and 4 is also provided with a spigot 25, arranged to discharge into the series of vats 32.
Beneath the chambers 1, 2, 3 and 4, rails are laid and a car 30 provided to run thereon. Dumping doors 27 are provided in the bottoms of these chambers, through which their contents may be dumped into the car 30.
6 is an acid reservoir, and 7 a water reservoir, connected by the pipe 13, provided with the stop cocks 16 and 17 This pipe 13 is connected by suitable branches with the chambers 1, 2, 3 and 4, and these branches are provided with the stop cocks 18. The top of the chamber 4 is connected with the bottom of the acid chamber 5, above and behind it, by means of the inverted U-shaped tube 9. Adjacent to the chamber 4 is a retort 20, provided with a furnace 21. The pipe 19, leading from the retort, passes through the chambers 1, 2, 3 and 4, near their bottoms. The pipe then leads upward and passes into the end chamber 5, above and behind the chamber 1.
The retort is shown provided with suitable means for feeding acid thereto, but such forms no part of my invention.
The operation of the apparatus is substantially as follows: The ore is first ground, or crushed, to pass through a 30 or 40 mesh sieve, and then placed in the ore chambers 1, 2, 3 and 4, through the air-tight fitting doors 34. The acid is mixed to the proper strength in the receptacles 5. Acid and water are then admitted from the chambers 6 and 7, through the pipe 13, into the ore chambers 1, 2, 3 and 4. A suitable salt and acid are heated together in the retort, and the heat and vapors therefrom pass through the pipe 19 and raise the temperature of the contents of the ore chambers sufliciently to greatly stimulate the chemical action therein. The gases and vapors resulting from the action of the acid on the ore rise in the chambers 1, 2, 3 and 4, and are forced from each chamber in succession, through the pipes 36, into the bottom of the next chamber, thus keeping the ore constantly in agitation, and obviating the necessity for any artificial stirrer, and, finally, any excess from the chamber 4: is forced through the pipe 9 into the bottom of the first chamber 5 and thence, in succession, into the bottoms of the next chambers, through the pipes 26. Here any metallic values contained in such gases are condensed and saved, and any excess of gas is also condensed. As soon as the decomposition is complete the fluids in chambers 1, 2, 3 and i are drawn off into the vats, and the residue containing the insoluble matter, having been first washed with water admitted from the reservoir 7, is dumped into the car 30. At
' the same time the plug 37 is removed and the stop cocks 35 opened. The noxious gases and fumes in the upper part of the chambers 1, 2, 3 and 4 are then drawn off by means of a pump 38 conventionally illustrated in the drawings, and pass through the pipe 9, into the acid containing chambers 5, where they are condensed.
While my apparatus is especially adapted to the treatment of sulfids, it may also be employed with almost any ores, except those containing a high percentage of iron, or those so intimately mixed with calcium compounds, as calcium carbonate, as not to permit of ready and inexpensive sorting.
For the purpose of further illustrating the process for Which my apparatus is adapted, I will select the lead ore galena. This is crushed, as already described, and freed as far as possible from gangue, silicious, calcareous, and other foreign matters. A charge is placed in the chambers 1, 2, 3 and 4. Dilute nitric acid is mixed in the reservoirs 5. In the rogress of decomposition this nitric acid will be found to contain a small proportion of nitrous acid. It should also be noted that it is designed to keep the temperature of the re-action as nearly 80 degrees centigrade as may be possible. In the retort is placed a mixture of some suitable salt, such as sodium nitrate, and an appropriate acid, such as sulfuric acid, and heat is applied. The dilute nitric acid is allowed to flow from the reservoirs 5 into the chambers 14. Acid and water may be instead admitted directly to these chambers from the reservoirs 6 and 7. The chambers 14 are thereupon made air tight. The chambers 5, during the re-action, are partially filled with water, their original contents having been drawn off to supply the ore chambers. Of course, if the ore chambers are filled directly from the tanks 6 and 7, the chambers 5 will be filled with water in the first place. The action of the Warm dilute acid on the lead sulfid re sults in the formation of lead nitrate. As the result of more or less complicated actions and re-actions, nitrogen tetroxid is also formed in the gaseous form, and this, by combination with the water of the dilute acid, is de-composed, and forms nitric and nitrous acid, causing the ore to be exposed to the action of the acid in a nascent state, thus greatly increasing the energy of the re-action. A certain proportion of the nitrogen tetroxid passes on into the reservoirs filled with water, and is there converted into nitric and nitroirs acid, and absorbed. By the aeration of the solution the nitrous acid can be converted into nitric acid, but, it may be pointed out, that a certain amount-of nitrous acid in the nitric acid appears to materially assist the latter in its action.
All parts of the galena insoluble in dilute nitric acid are left in the chambers when drawing off the solution of nitrate of lead and other metals, and with this residue is left the sulfur, which may be Washed out or converted into sulfuric acid.
Any iron nitrate in the solution may be precipitated as a hydroxid by the action of carbon di-oxid, and upon being dried, and, if desired, calcined, is a valuable pigment.
The lead nitrate may be precipitated by a mixture of sodium carbonate and hydroxid to give a mixture of lead hydroxid and sodium nitrate, any nitric acid remaining in the solution being also converted into sodium nitrate.
Sodium nitrate, obtained as above, may be employed, and when treated with sulfuric acid (made from the sulfur obtained from decomposition of the galena) generates the heat desired during the process, and thus forms part of the cycle.
If the plant is properly constructed and run there should be very little loss of nitric acid, but, as the proper treatment of the various products and by-products of my process will be readily understood by any skilled chemist, it will be unnecessary to further describe them. 4
If a copper ore be substituted for the lead ore, I mix in the reservoirs a saturated solution of sodium chlorid with dilute nitric acid, resulting in the formation of hydrochloric acid. When this is allowed to act on the ore in the chambers 1- 1, chlorin gas is generated, and the cycle of operations proceeds as in the case of lead ores. The acid formed is usually nitric and nitrous acid.
The treatment of the resulting salts pro duced by the action of the acid on the ore is within the scope of any chemist skilled in the art.
It will be seen that the process is cyclic in its nature, that is, all the gaseous products of each chemical reaction are sent through the successive ore chambers and the gases finally condensed for use with a new charge.
What I claim as my invention is:
1. In reduction apparatus the combination of a series of ore reduction chambers; pipes connecting seriatim the tops and bottoms of adjacent chambers; a feed door in the top of each chamber; a dumping door in the bottom of each chamber; a spigot for each chamber to draw ofl' liquid; a liquid chamher; a pipe adapted to lead gases from the last ore chamber into the said liquid cham ber; pipes connecting the ore chambers at their upper ends; and stop cocks in said pipes, a suitably closed air inlet being provided in the ore chamber remote from the connecting pipe with the liquid tank, substantially as described.
2. In apparatus of the character described, a tank consisting of a series of compart ments, means to connect the top of each compartment to the bottom of the next compartment, means to permit the connection of the tops of adjacent compartments, means for excluding or admitting air to the first compartment of the series, and means for drawing 01? fluids from the tank,
3. In apparatus of the character described, a tank consisting of a series of connected compartments, each of said compartments except those at each end of the tank having not more than four outer radiating surfaces, pipes connecting the tops of adjacent compartments, valves in said pipes, means to exclude or admit air to said compartments and means to remove gases therefrom.
4. In apparatus of the character described, adjacent tanks each divided into compartments, means to connect each compartment to the next including a pipe to connect the last compartment of one tank to the first compartment of the other tank, means to exclude or permit access of air to the first tank, additional controllable connecting means between the compartments of the first tank and means for removing gases from the said first tank to the second.
Toronto, November 30th, 1904.
GEORGE EDWARD KINGSLEY.
In the presence of JOHN G. RIDoUT, A. M. MoRAE.
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