US460004A - foliedesjardins - Google Patents

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US460004A
US460004A US460004DA US460004A US 460004 A US460004 A US 460004A US 460004D A US460004D A US 460004DA US 460004 A US460004 A US 460004A
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alkaline
phosphorus
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foliedesjardins
acid
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/087—Heating or cooling the reactor

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  • Myinvention' relates to an improved apparatus for "the simultaneous manufacture of phosphorus, alkaline.phosphates, and alkaline silicates on a commercial scale, and has for its object to transform the manufacture of phosphorus from an unhealthy industry cross-sectionof the furnace or oven with the opening G.
  • Fig. is across-section oi. the gas-generator,,taken through the charging- Fig. I is a front elevation of the gas-generator.
  • Fig. 5 is a front elevation of the furnace or oven with its condensers,
  • Fig. 6 is a horizontal section of the gasgencrator on the line IV V VI ⁇ "II of Fig.1, and a horirctorts.
  • Zontal section of the rcgenerator on the line XII XIII XIV XV of Fig. Fig. '7 is a plan of the gas-generator and a horizontal section of the regenerate! on the line IX X XVI and XVII of Fig. 2.
  • the apparatus comprises a furnace or oven in whicharc arranged a suitable number of These retorts (j, which are of refractory earth, may, if it be thought desirable, be provided'with an internal lining of magnesi'te. They have a slight inclination to allow of the overflow either of the product resulting Fig. 2 is av from the mineralphosphatesor the bone-ash in the first operation or of the residual alkaline silicate from the second operation.
  • the retorts are furnished with a tap-hole a.
  • the plugs V for closing the retort and the tap-holed are furnished with an internal liningof refractory material surrounded by a sleeve of asbestos for insuring tightness of joint. They are closed by means of a pressurescrew r.
  • Each retortjs provided at its upper part at the side near the opening of the retort withv a pipe for allowing of the escape of gases and formedinone piece with it for a certain length.
  • Brass extensions 1 (in the manufacture of phosphorus) are fitted on the pipe a, and serve to conduct the gas into the condenser On the right-hand side of Fig.
  • the condenser .2 is in sectioinand' is shown as connected by the extensions y to the pipes 50, whereas on the left of said figure the 7s condenser is in elevation and the extensions y leading thereto have been broken away.
  • One or more gasometers are provided in the manufacture of phosphorusior the reception of combustible gases, which on passing from the last gasoineter are conveyed by h a pipe to the burners, where'they are to be utilized according to requirement.
  • A is the gasoincter; B, the regcnerator of the waste heat; I), the gallery or passage for working thegas-generators; E, the galleryor passage for working the regenerators; F, the door of the furnace oroven; U, the charging plug, and ll the ash-pit door. 5
  • r Fig. 7
  • Fig. 7 is a sight-hole, closed by a castiron plug, for enabling the conduit I, forearbonic oxide to be examined and to be cleaned from dust carried along in suspension
  • f Y I, Figs. 1 and U are openings provided with cast-iron plugs for the passage of cleaningbars during the cleaning.
  • J is a cast-iron port serving for the introduction of air and water into the gasgenerator.
  • T. is a line for carbonic oxide.
  • M are flucs for-smoke and products of conibustiou which pass through N underneath the roof of the regenerator, and after passing between the tubes of the regenerator enter the chimney.
  • 0', Fig. 7, are orifices for placing the last rows of tubes into communication with the air-chamber Q.
  • I, Fig. 6, are exit-orifices for carbonic oxide.
  • Q is an air-chamber placing the orifices O for hot air into communication with one another.
  • Figs. 1, 2, 6, and 7 is an inlet for cold air into the regenerator.
  • T Figs. 1, 6, and 7, is a chimney furnished with a register '11.
  • the treatment of the phosphates in the first operation by means of alkaline sulphates or carbonates may be effected by means of a reverberatory furnace having a slightly-inclined bottom or hearth.
  • retorts and furnaces or ovens may be employed similar to those just described, except that tube a: of the retorts C communicates in such a case with a central conduit and not with a condenser, and the carbonic-acidgases or sulphurous-acid gases are conducted to apparatus which are intended to store up or else directly utilize the same.
  • the first operation to be performed is the elimination of the phosphoric acid from the phosphate of alumina or phosphate of lime by means of an alkaline sulphate or carbonate,or by means of a mixture of carbonate of soda and carbonate of potash, or by means of a sulphate of these two bases. As already stated, this maybe effected either in a reverratory furnace 'or in retorts of refractory earth heated by means of carbonic oxide.
  • X is the tube serving for the escape of the carbonic acid, (00 This gas passes byacenare exit-orifices for hot tral conduit toward the place of storage or soda, (NaO,Al.,O ,SiO,.).
  • the second operation has for its object to eliminate from the alkaline phosphatethe 1 phosphoric acid (P0 and to reduce'the said acid.
  • the alkaline phosphate, silicic' acid, and carbon are mixed intimately together.-
  • the mixture is sub ected to the action of heat in the retortsOof a furnace or oven heated by means of carbonic oxide, as illustrated in Figs. 1 and 5 of the annexed drawings.
  • Theintimate mixture being raised to a bright red heat in the retorts, the silicic acid attacks the base, forming an alkaline silicate, and liberates the phosphoric acid.
  • the latter being free is reduced by the carbon,which unites 'with the oxygen of the acid to form carbonlc quirements of the case, conveyed to the burners of'furnaces, or preferably to furnaces for regenerating the waste heat.
  • the products of theoperation are therefore, first, phosphorus, which is to be purified by the usual means; second, a simple or complex alkaline silicate, such as in the example chosena silicate of soda.
  • the degree of acidity of the alkaline silicate may vary at the will of the operator, according to the use for which it is intended.
  • the residual silico-aluminate of soda contains sesquioxide of iron.
  • This residue may be treated by known means so as to yield a precipitate of alumina and sesquioxide of iron, gelatinous silica, and a caustic alkaline or an alkaline carbonate.
  • the separation of the sesquioxide of iron from the alumina may be eifected by means of trimethylamine, (O H NH which precipitatesthe sesquioxide of iron and the alumina and then redissolves the latter.
  • This residue must not, therefore, be considered a waste product, for it is possible to recover the greater part of the alkaline salt.
  • phosphate of alumina, phosphate of lime, and an alkaline carbonate are employed, for instance, the addition of silica may be dispensed With,- the carbonate of lime obtained remaining in suspension in the melted material, being insoluble in it.
  • the first operation will thus be represented by one of the following equations: first, boneash 2 3030 3000) 1S(NaO,CO 3(PO ,3 NaO)+1)NaO+9CaO,CO,+9CO second, fossil phosphate of lime:(3PO,,3CaO)i-CaFl+ 1S(NaO,CO,) 3(PO,,3NaO)+CaFl+9NaO-i 9CaO,CO,1-DCO,.

Description

- 4Sl1eet-Sheet 1.. L. M. 01 FOLIEDESJARDINS APPARATUS FOR THE MANUFACTURE OF PHOSPHORUS AND ALKALINE SILIOATES.
Patented Sept. 22, 1891.
Iolololololo I01 000 not lololooooooooooooo I Iqqjololo olo o Q10 00 T l lotol l l l l f lolo (No Model.) 4
L. M. O. POLIEDESJARDINS. APPARATUS FOR THE MANUFACTURE OF PHOSPHORUS AND ALKALINE SILIGATES.
No. 460,004. Patented Sept. 22, 1891.
SheetsSheet 2.
f O %,IZ .04 A
aw/@zA g 2M @w W 6M7 aim! L i wvwba (No Model.) 4 sheets-sheet 3'.
L. M. G. FOLIED ESJARDINS.
APPARATUS FOR THE MANUFACTURE. OF PHOSPHORUS AND ALKALINE SILIGATES.
No. 460,004. Patented Sept. 22, 1891 (No Model.) 7 A. 4 Sheets-Sheet 4. L. M. U. FOLIEDESJARDINS.
APPARATUS FOR THE MANUFACTURE OF PHOSPHORUS AND ALKALINE SILIGATES. Y No. 460,004. Patented Sept. 2 1891.
tl-nrrnn Sink-res .Pn'rnnrr @rmcn.
touts-amen: cnARL'E's. FOLIEDESJARDINS, or 'rounousn, FRANCE.
APPARATUS FORTHE MANU FAGTURE OF PHOSPHORUS AND ALKALINE SILICATES.
SPECIFICATION taming part of Letters Patent No. 460,004, dated September 22, 1891. Applicationfiled Septeinber13;1890. Serial No. 364,874. (No model.) Patented in France Pebruary24, 1890, No. 203,942.
To all whomit may concern:
Be it known that 1, Louis MARIE CHARLES FOLIEDESJARDINS, chemist, a citizen of the Republic of France, residing at Toulouse,
lIau'te-Garon'ne, France, have invented a new and useful'Apparatus for the Simultaneous Manufacture of Phosphorus, Alkaline Phosphates, and Alkaline Silicates, (for which I have obtai'neda patent in France, No. 203,942, dated February 24, 1890;) and I do hereby declare that the following isa full, clear, and
line VIII IX X XI of Fig. 2.
ator on the line I II of Fig. I
exact descriptionof the same.
Myinvention'relates to an improved apparatus for "the simultaneous manufacture of phosphorus, alkaline.phosphates, and alkaline silicates on a commercial scale, and has for its object to transform the manufacture of phosphorus from an unhealthy industry cross-sectionof the furnace or oven with the opening G.
regenerator. Fig. is across-section oi. the gas-generator,,taken through the charging- Fig. I is a front elevation of the gas-generator. Fig. 5 is a front elevation of the furnace or oven with its condensers, Fig. 6 is a horizontal section of the gasgencrator on the line IV V VI \"II of Fig.1, and a horirctorts.
Zontal section of the rcgenerator on the line XII XIII XIV XV of Fig. Fig. '7 is a plan of the gas-generator and a horizontal section of the regenerate! on the line IX X XVI and XVII of Fig. 2. r l
The apparatus comprises a furnace or oven in whicharc arranged a suitable number of These retorts (j, which are of refractory earth, may, if it be thought desirable, be provided'with an internal lining of magnesi'te. They have a slight inclination to allow of the overflow either of the product resulting Fig. 2 is av from the mineralphosphatesor the bone-ash in the first operation or of the residual alkaline silicate from the second operation.
The retorts are furnished with a tap-hole a. The plugs V for closing the retort and the tap-holed are furnished with an internal liningof refractory material surrounded by a sleeve of asbestos for insuring tightness of joint. They are closed by means of a pressurescrew r. Each retortjs provided at its upper part at the side near the opening of the retort withv a pipe for allowing of the escape of gases and formedinone piece with it for a certain length. Brass extensions 1 (in the manufacture of phosphorus) are fitted on the pipe a, and serve to conduct the gas into the condenser On the right-hand side of Fig. 5 the condenser .2 is in sectioinand' is shown as connected by the extensions y to the pipes 50, whereas on the left of said figure the 7s condenser is in elevation and the extensions y leading thereto have been broken away. A condenser .2, provided with a draft fine or chimney'f, communicates with a central conduit, which conveys the carbonic oxide and other uncondensed gases into a gasoineter or gas-holder. (Not shown.)
One or more gasometers are provided in the manufacture of phosphorusior the reception of combustible gases, which on passing from the last gasoineter are conveyed by h a pipe to the burners, where'they are to be utilized according to requirement.
A is the gasoincter; B, the regcnerator of the waste heat; I), the gallery or passage for working thegas-generators; E, the galleryor passage for working the regenerators; F, the door of the furnace oroven; U, the charging plug, and ll the ash-pit door. 5
r], Fig. 7, is a sight-hole, closed by a castiron plug, for enabling the conduit I, forearbonic oxide to be examined and to be cleaned from dust carried along in suspension," f Y I, Figs. 1 and U, are openings provided with cast-iron plugs for the passage of cleaningbars during the cleaning.
J is a cast-iron port serving for the introduction of air and water into the gasgenerator. v
II, Figs. 1 and I, is the rose of a sprinkler, I00
serving for the rapid extinction of the ashesresulting from the cleaning.
T. is a line for carbonic oxide.
M are flucs for-smoke and products of conibustiou which pass through N underneath the roof of the regenerator, and after passing between the tubes of the regenerator enter the chimney.
0, Figs. Sand (3, air.
0', Fig. 7, are orifices for placing the last rows of tubes into communication with the air-chamber Q.
I, Fig. 6, are exit-orifices for carbonic oxide.
Q, Fig. 7,is an air-chamber placing the orifices O for hot air into communication with one another.
11, Figs. 1, 2, 6, and 7, is an inlet for cold air into the regenerator.
' S, Fig. 2, are internal baflies compelling the cold air to pass into all tle rows of tubes, as indicated by the arrows.
T, Figs. 1, 6, and 7, is a chimney furnished with a register '11.
(Z e f, Figs. 5 and 6, are sight-holes lined with cast-iron. v
The treatment of the phosphates in the first operation by means of alkaline sulphates or carbonates may be effected by means of a reverberatory furnace having a slightly-inclined bottom or hearth. However, ifit is desired to utilize thecarbonic acid or the sulphurous acid, retorts and furnaces or ovens may be employed similar to those just described, except that tube a: of the retorts C communicates in such a case with a central conduit and not with a condenser, and the carbonic-acidgases or sulphurous-acid gases are conducted to apparatus which are intended to store up or else directly utilize the same.
The first operation to be performed is the elimination of the phosphoric acid from the phosphate of alumina or phosphate of lime by means of an alkaline sulphate or carbonate,or by means of a mixture of carbonate of soda and carbonate of potash, or by means of a sulphate of these two bases. As already stated, this maybe effected either in a reverratory furnace 'or in retorts of refractory earth heated by means of carbonic oxide.
X is the tube serving for the escape of the carbonic acid, (00 This gas passes byacenare exit-orifices for hot tral conduit toward the place of storage or soda, (NaO,Al.,O ,SiO,.).
' The second operation has for its object to eliminate from the alkaline phosphatethe 1 phosphoric acid (P0 and to reduce'the said acid.
For this purpose the alkaline phosphate, silicic' acid, and carbon are mixed intimately together.- The mixture is sub ected to the action of heat in the retortsOof a furnace or oven heated by means of carbonic oxide, as illustrated in Figs. 1 and 5 of the annexed drawings.
The reaction to be produced is illustrated by the following equation in the example I have taken.
Theintimate mixture being raised to a bright red heat in the retorts, the silicic acid attacks the base, forming an alkaline silicate, and liberates the phosphoric acid. The latter being free is reduced by the carbon,which unites 'with the oxygen of the acid to form carbonlc quirements of the case, conveyed to the burners of'furnaces, or preferably to furnaces for regenerating the waste heat. The products of theoperation are therefore, first, phosphorus, which is to be purified by the usual means; second, a simple or complex alkaline silicate, such as in the example chosena silicate of soda. The degree of acidity of the alkaline silicate may vary at the will of the operator, according to the use for which it is intended.
The residual silico-aluminate of soda contains sesquioxide of iron. This residue may be treated by known means so as to yield a precipitate of alumina and sesquioxide of iron, gelatinous silica, and a caustic alkaline or an alkaline carbonate.
The separation of the sesquioxide of iron from the alumina may be eifected by means of trimethylamine, (O H NH which precipitatesthe sesquioxide of iron and the alumina and then redissolves the latter. This residue must not, therefore, be considered a waste product, for it is possible to recover the greater part of the alkaline salt. If in place of phosphate of alumina, phosphate of lime, and an alkaline carbonate are employed, for instance, the addition of silica may be dispensed With,- the carbonate of lime obtained remaining in suspension in the melted material, being insoluble in it.
The first operation will thus be represented by one of the following equations: first, boneash 2 3030 3000) 1S(NaO,CO 3(PO ,3 NaO)+1)NaO+9CaO,CO,+9CO second, fossil phosphate of lime:(3PO,,3CaO)i-CaFl+ 1S(NaO,CO,) 3(PO,,3NaO)+CaFl+9NaO-i 9CaO,CO,1-DCO,. The product of the reactions when subjected to a slight lixiviation and allowed to rest deposits the carbonate of TOC lime (or, as the case may be,oarbonaioof lime and fluoride of calcium) and thererernsins a bon, which is submitted tothe action of heat,
as hereinbefore stated. I The reactions obtained are represented by the following equation:
v a(Po ,e1-rao +9mo+9sio so=seein ,0,2sio +15o0. If desired5xthe acidity of the' silieate may be modified by-increasing the proportion of silica, as before mentioned. The result is, first, im-
pure phosphorus; second, an alkaline silicate;
third, carbonic oxide.
- As vit is possible-t0 modify the degree M I acidity or'ol' alkalinity, so is it also possible by mixing the :ilkslies to obtain complex sili-. cates of potash and soda. -'I claim- T In an apparatus for the manufacture of phosphorus, slimline phosphates, and slim-- line silicates, the combination of a furnace orovcn, the retorts C, having pipes m, provided with extensions y, the condenser shaving a chimney t, the gasonieter A, and theregenerator B, substantially as shown and described. 7 In witness whereof I have hereunto s1 gned my name in the presence of two subscribing witnesses. I I
LOUIS MAR-IE CHARLES FOLIEDESJARDINS.
Witnesses:
D. H. BRAND N, A. LE AM.
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