US106851A - Campbell morfit - Google Patents

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US106851A
US106851A US106851DA US106851A US 106851 A US106851 A US 106851A US 106851D A US106851D A US 106851DA US 106851 A US106851 A US 106851A
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liquor
lime
vat
phosphate
campbell
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05BPHOSPHATIC FERTILISERS
    • C05B11/00Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
    • C05B11/04Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid
    • C05B11/06Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid using nitric acid (nitrophosphates)

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  • my invention consists in the use of crude ammonia, in the form of coal-gas liquor, or as gas distilled th'erefrom, for recovering back the hydrochloric acid which may be employed for making solutions of navaza (navassa) guano and other kinds of mineral phosphates, by neutralizing the acid into chloride of ammoniunna valuable salt, and simultaneously precipitating the contained phosphate of lime in the state of a very potential fertilizer.
  • navaza navassa
  • guano and other kinds of mineral phosphates by neutralizing the acid into chloride of ammoniunna valuable salt, and simultaneously precipitating the contained phosphate of lime in the state of a very potential fertilizer.
  • the navaza guano or mineral phosphate must be reduced first to coarseor fine powder, according to its greater or lesser solubility in acids. It is then placed in stone vats, each of which is fitted with a false-bottom, and drenched with commercial hydrochloric acid, after which the vat is to be covered. From this cover there-must be a tube connection with a low chamber containing lime, for the-condensation of the noxious gases which may be evolved during the action of the acid on the mineral. As this acid percolates downward through the powder, it takes up all the soluble matter, and passes through the false bottom into the chamber below as a strong solution.
  • the collected liquors in the Montejus are to be raised into a very capacious reservoir of oak wood; by means of compressed air or steam.
  • the pipe through which the liquor is forced from the Montejus up into the reservoir must be of iron, lined with gutta-perchaor vulcanized India rubber.
  • the quantity of acid required for exhausting the mineral must be determined in advance, by testing aweighed portionpf the powder, for it will vary with the composition of the phosphatic guano or mineral under treatment.
  • the liquor which has been raised into the vat contains all the matters of the mineral soluble in the hydrochloric acid and. water, and consisting of phosphates of lime and magnesia, chlorides of the calcium and magnesium which existed originally as carbonates, together with more or less of alumina and oxide of iron, and some little of phosphates of alumina and iron, if these latter were present.
  • insoluble residue in the-vat is composed of sand, earthy and metallic silicates, fluoride of calcium, much of the alumina and oxide of iron, and nearly :the whole of the phosphates of alumina and iron.
  • This insoluble residue is to be drawn out from the vat through a man-hole, and thrown aside as rejected matter.
  • the latter To return to the liquor in the rat, the latter must be fitted with a tight cover, from which atube leadsdown the outside of the vat, and along the ground, into the tire ot'the steam-boiler furnace, in order that the noxious gases which are about to be eliminated may be consumed, forthe protection of the comfort and health of the workmen.
  • the vat should be fitted with a wooden stirrer, put in Imotion by steam gear 7 ing, and it should not be filled with liquor to more than one-half of its height, as upper space must be left for the addition of the precipitant and the effervescence which will accompany the chemical action about to take place.
  • Crude gas liquor is now added slowly and by instalments, while the stirrer is in motion,throngh a tunnel in the top of the vat, until the liquor becomes slightly alkaline to test-papcr'..
  • the phosphate oflime is to be drawn from the vat, through wood-n gutters, into a kiln similar to that which is used for drying white lead. By a carefully-managed heat it soon becomes a dry powder, of a bluish-grey color, and consisting of gelatinous or precipitated phosphate of lime, with chloride of ammo-' nium.
  • the gelatinous phosphate of lime retains, even as dry powder, a certain amount of water, which may be considered quasi constitutional, and is in that state most suited to give a prompt and consistent fertilizations to soils. Indeed, it has just that condition to which soluble superphosphate of lime is immediately reduced by the natural chemistry of the soil, as soon as it has been applied, and previous to being taken upby the growing crop.
  • the ratio of ammoniacal salt should be raised to twenty or thirty per cent., and associated witlrabout ten per cent. of potassa salt, according to the kind of crop for which it may be intended. This is done practically by mixing the proper weights of those salts with the phosphate prepared in manner as abot e explained.
  • the amount of crude gas liquor which may be required 'to neutralize the hydrochloric-acid liquor of the vat may be deterlnined in advance by gauging the quantity of the latter, then taking out a measured portion of it,-and carefully adding item a measured portion of the gas liquor until neutralized. From the volume of the latter consumed for this preliminary test sample maybe calculated thetotal required by the contents of the vat This test is necessary at each operation, because the ammoniacal strength of the crude gas liquor isvery variable.
  • the inconvenience of sulphureted odors from large bulk of liquid, and of color in-the precipitated phosphate of lime may be obviated by mixing the crude gas liquor with lime, and, it may be, also, some oxide of iron, in a round wrought-iron boiler, with a dome top and a tube leading from it into the contents of the vat. Another tube, leading from the steam-boiler, must pass down to the iron still containing the mixture of gas liquorand lime, or lime and oxide of iron.
  • the cock being opened and steam let on, causes the gas liquor to boil and give off its ammonia as gas,
  • Hydrochloric acid being in the public domain of chemical knowledge as a solvent of phosphatic substances, I do not claim its use for that purpose but What I do claim is---

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  • Organic Chemistry (AREA)
  • Fertilizers (AREA)

Description

Hit-Iii ctjiflirr.
CAMPBELL MORFIT.
OFYNEW YORK, N. Y.
Letters Patent No. 106,851, dated August 30, 1870.
IMPROVEMENT IN THE TREATMENT OF GUANO AND A THE MANUFACTURE 01: PER- TILIZERS.
The Schedule referred to in these Letters Patent and making part of the same.
To all whom it may concern.
Be it known that I, CAMPBELL Monrrr, consulting chemist, of the city of New York, in the State of New York and United States of A merica, but now residing' temporarily at Sudbrook Park, Peter-sham, county of Surrey, England, have invented a new, improved, and economical Method of Treating Navaza Guano and other kinds of Mineral Phosphates, for their Conversion into Valuable Fertilizing Products; and I do hereby declare that the following is a full and exact -description thereof.
The nature of my invention consists in the use of crude ammonia, in the form of coal-gas liquor, or as gas distilled th'erefrom, for recovering back the hydrochloric acid which may be employed for making solutions of navaza (navassa) guano and other kinds of mineral phosphates, by neutralizing the acid into chloride of ammoniunna valuable salt, and simultaneously precipitating the contained phosphate of lime in the state of a very potential fertilizer.
To carry out the invention practically, the navaza guano or mineral phosphate must be reduced first to coarseor fine powder, according to its greater or lesser solubility in acids. It is then placed in stone vats, each of which is fitted with a false-bottom, and drenched with commercial hydrochloric acid, after which the vat is to be covered. From this cover there-must be a tube connection with a low chamber containing lime, for the-condensation of the noxious gases which may be evolved during the action of the acid on the mineral. As this acid percolates downward through the powder, it takes up all the soluble matter, and passes through the false bottom into the chamber below as a strong solution. Time would be saved by keeping the room at 80 to 100 Fahrenheit by means of steam- .pipes around the outside of the vats. The acid solution, as it collects in the lower chambers, must be drawn oil through a hole in the front, which is fitted with a plug for the purpose." A gutter running the length of the front of these vats must be arranged to conduct the solution into a stone reservoir constructed in the ground beneath, and as a Montejus. The first dose of acid having run through, a fresh addition'is next to be poured on, and allowed to pass through in the same way. Finally, and in like manner, two successive additions of boiling water are then to follow,
in order to rinse the powder, and the wash waters are madeto run and mix with the previous liquors. The residue in 'the vats is thus exhausted, and must be shoveled out as insoluble matter without value in this process. The vats are then ready to be charged again, with fresh materials for a new operation. The collected liquors in the Montejus are to be raised into a very capacious reservoir of oak wood; by means of compressed air or steam. The pipe through which the liquor is forced from the Montejus up into the reservoir must be of iron, lined with gutta-perchaor vulcanized India rubber.
The quantity of acid required for exhausting the mineral must be determined in advance, by testing aweighed portionpf the powder, for it will vary with the composition of the phosphatic guano or mineral under treatment. The liquor which has been raised into the vat contains all the matters of the mineral soluble in the hydrochloric acid and. water, and consisting of phosphates of lime and magnesia, chlorides of the calcium and magnesium which existed originally as carbonates, together with more or less of alumina and oxide of iron, and some little of phosphates of alumina and iron, if these latter were present. The
insoluble residue in the-vat is composed of sand, earthy and metallic silicates, fluoride of calcium, much of the alumina and oxide of iron, and nearly :the whole of the phosphates of alumina and iron. This insoluble residue is to be drawn out from the vat through a man-hole, and thrown aside as rejected matter. To return to the liquor in the rat, the latter must be fitted with a tight cover, from which atube leadsdown the outside of the vat, and along the ground, into the tire ot'the steam-boiler furnace, in order that the noxious gases which are about to be eliminated may be consumed, forthe protection of the comfort and health of the workmen. The vat should be fitted with a wooden stirrer, put in Imotion by steam gear 7 ing, and it should not be filled with liquor to more than one-half of its height, as upper space must be left for the addition of the precipitant and the effervescence which will accompany the chemical action about to take place. Crude gas liquoris now added slowly and by instalments, while the stirrer is in motion,throngh a tunnel in the top of the vat, until the liquor becomes slightly alkaline to test-papcr'.. This testindicates that all the hydrochloric acid of the liquor has been neutralized by the ammonia of thegas liquor, which change causes it to drop at the same time the phosphate of lime, together with any alu minaand oxide of iron and their phosphates which the liquor may have contained. .When this has settled to the bottom, the liquor above will be an impure solution of chloride of ammonium, and is to be drawn oh and evaporated to a dense solution, in'order that it may form into crystals. These crystals of crude chlo-' ride of ammonium may be purified by recrystallization,
or'else .baked on a carefully-heated drying-kiln, so as to destroy its empyzeumatic, sulphureted,-and foreign remaining phosphate of lime retains a considerable 'portion'of-the impure chloride of ammonium liquor,
and is colored more or less lig'ht greenish blue by the small quantities of metallic sulphurets which have been formed by the impurities of the two liquors. There is present, also, some pitchy or empyzeumatic matters. The phosphate oflime is to be drawn from the vat, through wood-n gutters, into a kiln similar to that which is used for drying white lead. By a carefully-managed heat it soon becomes a dry powder, of a bluish-grey color, and consisting of gelatinous or precipitated phosphate of lime, with chloride of ammo-' nium. The gelatinous phosphate of lime retains, even as dry powder, a certain amount of water, which may be considered quasi constitutional, and is in that state most suited to give a prompt and consistent fertilizations to soils. Indeed, it has just that condition to which soluble superphosphate of lime is immediately reduced by the natural chemistry of the soil, as soon as it has been applied, and previous to being taken upby the growing crop. To perfect its efiiciency as a fertilizer, the ratio of ammoniacal salt should be raised to twenty or thirty per cent., and associated witlrabout ten per cent. of potassa salt, according to the kind of crop for which it may be intended. This is done practically by mixing the proper weights of those salts with the phosphate prepared in manner as abot e explained.
The amount of crude gas liquor which may be required 'to neutralize the hydrochloric-acid liquor of the vat may be deterlnined in advance by gauging the quantity of the latter, then taking out a measured portion of it,-and carefully adding item a measured portion of the gas liquor until neutralized. From the volume of the latter consumed for this preliminary test sample maybe calculated thetotal required by the contents of the vat This test is necessary at each operation, because the ammoniacal strength of the crude gas liquor isvery variable.
The inconvenience of sulphureted odors from large bulk of liquid, and of color in-the precipitated phosphate of lime, may be obviated by mixing the crude gas liquor with lime, and, it may be, also, some oxide of iron, in a round wrought-iron boiler, with a dome top and a tube leading from it into the contents of the vat. Another tube, leading from the steam-boiler, must pass down to the iron still containing the mixture of gas liquorand lime, or lime and oxide of iron.
The cock being opened and steam let on, causes the gas liquor to boil and give off its ammonia as gas,
which distils over, with. moreor less condensed steam,
when a piece of red litmus-paper dipped into it becomes immediately and permanently blue.
0 lat m.
Hydrochloric acid being in the public domain of chemical knowledge as a solvent of phosphatic substances, I do not claim its use for that purpose but What I do claim is-- The method of recovering back the hydrochloric acid employed in making hydrochloric solutions of navaza (navassa) guano and other kinds of mineral phosphate of lime, by the use of crude ammonia either in the form of coal-gas liquor or as gas distilled therefrom, for neutralizing the acid, so as to-produce simultaneously the salt chloride of ammonium and a semigelatinous precipitate of great agricultural value, to be known .as Colombian phosphate of lime or fertilizer, by the suitable means and after the economical manner herein described and substantially set forth.
In witness whereof, I, the said CAMPBELL MORFIT, have hereunto set my hand and seal, this 18th day of February, inthe year of our Lord 1870.
CAMPBELL MORFIT.
Witnesses:
'1. W. FRaJoN, 1*. W. ATKINSON.
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