US1841071A - Manufacture of phosphorus and compounds thereof - Google Patents
Manufacture of phosphorus and compounds thereof Download PDFInfo
- Publication number
- US1841071A US1841071A US76689A US7668925A US1841071A US 1841071 A US1841071 A US 1841071A US 76689 A US76689 A US 76689A US 7668925 A US7668925 A US 7668925A US 1841071 A US1841071 A US 1841071A
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- US
- United States
- Prior art keywords
- phosphorus
- charge
- chamber
- retorts
- compounds
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title description 24
- 229910052698 phosphorus Inorganic materials 0.000 title description 24
- 239000011574 phosphorus Substances 0.000 title description 24
- 150000001875 compounds Chemical class 0.000 title description 5
- 238000004519 manufacturing process Methods 0.000 title description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 239000002802 bituminous coal Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000011541 reaction mixture Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000000571 coke Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 235000021317 phosphate Nutrition 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003034 coal gas Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 206010022000 influenza Diseases 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 241000206607 Porphyra umbilicalis Species 0.000 description 1
- 208000027697 autoimmune lymphoproliferative syndrome due to CTLA4 haploinsuffiency Diseases 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/003—Phosphorus
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/01—Treating phosphate ores or other raw phosphate materials to obtain phosphorus or phosphorus compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
Definitions
- Figure 1 is a diagrammatic view, Jartiallv in section, showing apparatus suitable for use in carrying outy the present invention.
- FIG 2 isa diagrammatic sectional view of condensing apparatus suitable for use in connection with the present invention, as hereinafter set forth.
- the numeral 5 indicates an oven or furnace of the by-product coke oven type, that portion on the left of the vertical line ill-.A being shown in section through the retort or muffe-e chamber of a bench, and that portion of the right of theL line A-i being a sectional vieiv through the heating flues interposed betvveenmuffles or retorts in the bench.
- rlie retort shown may be regarded as one in a bench of retorts, certain of which are employed in the manufacture ofy by-product coke in the usual manner, that illustr: ted Jeing employed in association therewith for the manufactureA of phosphorus or phosphorus compounds as hereinafter more fully set forth.
- the retort or non chamber 6 is charged with the nhosphatic reaction min ure by the method usual in charging colte ovens coke; thatl is, the reaction mixture is chai thereinto through the ports 7 from suitable hopper cars 8.
- the individual retorts or ovens of the bench, which are relatively narrow, are heated in the customary manner, by means of a suitable fuel gas supplied through 21, 1925. Serial No. 76,689.
- l-.e retorts 6 are provded vith discharge iipes 15, through which the phosphorus vapors given off by the charge pass out to be handled as he iuafter more fully described.
- i suitable ram 14 is provided for forcing the spent charge from the retort after completion of the reaction.
- the phosphatic charge is prepared for the retorts by admiring previously ground phosphate rock and bituminous coal, both being preferably ground so that 90% thereof will pass through a Ll0 mesh screen.
- the mixture is so made (Withthe addition of suitable quantities of sand, if required) that the resulting charge has approximately7 he following constitution.
- This mixture is then employed as the charge in the retorts 6.
- a small quantity of bituminous coal be charged thereinto toform a layer extending Vover the base or .bottom of the oven, the phosphatic charge being then filled in over this laver of bituminous coal.
- the ovens having been charged, they are brought to a temperature between 1100o and 11150o C., at vvhich temperature the reaction takes place and phosphorus is evolved.
- the charge of the proportions hereinbefore set forth is not reduced to a molten condition, nor does it do more than sinter at temperatures as high as 1450O C.
- the phosphorus is therefore evolved under these conditions Without fusion of the reaction mixture.
- the relatively narrow width of the retorts or ovens permits of a very even distribution of heat through the charge.
- bituminous coal is employed as the carbonaceous reheated air for combustion is supplied to'l constituents of the charge, and as a result of its use there isa shrinkage of the charge during reaction which substantially facilitates the removal of the spent charge from the furnaces.
- a suitable non-oxidizing gas such as nitrogen, carbon monoxide or colle-oven gas may be caused to passV through the retorts, thus aiding in sweeping out the phosphorus vapors.
- resulting gases includingphosphorus pentoxid and phosphoric acid. pass into a collecting chamber 20, being suitably forced thereinto by a pump 21. Loss of phosphorus pentthe phosphates.
- the latter has lected phosphorus may be readily Withdrawn therefrom.
- the method of producing phosphorus from a phosphatic material which comprises preliminarily applying to an interior Wall of an externally heated chamber a layer of bituminous coal, subsequently charging the chamber With a phosphatic material admixed lvvith silica and a carbonaceous material, and
- the Vmethod of producing phosphorus which comprises heating in an externally fired chamber to a temperature between 1100o and 1450o a mixture of natural phosphate, silicious material and bituminous coal, the proportion of bituminous coal being in excess of 18% andl that of silica not being above 20%.
- the method of producing phosphorus from a phosphatic material which comprises preliminarily applying to an interior Wall of an externally heated chamber a layer of bituininous coal, subsequently charging the chamber with a phosphaticmaterial admixed With silica and a carbonaceous material, and applying sufficient heat to remove the phosphorus from the charge Without fusing said charge, adherence of the charge to the Wall of the chamber being thereby prevented.
- the method of producing phosphorus which comprises heating a phosphatic reaction mixture comprising a natural phosphate, silica and carbonaceous material in a chamber. separatelyand simultaneously heating a Coking coal to a colring temperature, thereby evolving coalgas therefronnand Vdrawing said coal gas through .the heated phosphatic reaction mixture.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Working-Up Tar And Pitch (AREA)
Description
Jan. 12, 1932. w. H. WAGGAMAN ET AL MANUFACTURE OF PHOSPHORUS AND COMPOUNDS THEREOF Filed Dec. 2l, 1925 NN. Q
Patented Jan. 12, 1932 WILLAM E.. VAGGAMAN AND HENBY- W. EASTER-VJOGD, OF CHICAGO HEIGHTS,
ILLNOIS, ASSIGNORS '13() VICTOR CHEMICL vitfls, .A CORPORATIQN OF LLIN 01S IL'ANUFACTURE OF PHOSPHORUS .A1-TB COMPOUNDS THEREOF Application filed December The present invention relates to improvements inthe manufacture of phosphorus or `of compounds thereof, and will be fully understood from the following description, illustrated'by the accompanying drawings, in which:
Figure 1 is a diagrammatic view, Jartiallv in section, showing apparatus suitable for use in carrying outy the present invention; and
2 isa diagrammatic sectional view of condensing apparatus suitable for use in connection with the present invention, as hereinafter set forth.
naccordance With the present invention, the production of phosphorus and compounds thereof fromphosphatic materials is facilitated and the eifective recovery thereof substantially increased.. In the preferred method of carrying out the invention, conditions maybe so maintained that an effective recovery of phosphorus is secured Without the disadvantage of bringing the reaction materials to the fusion point of the mixture.
Tieferring more particularly to the drawings, the numeral 5 indicates an oven or furnace of the by-product coke oven type, that portion on the left of the vertical line ill-.A being shown in section through the retort or muffe-e chamber of a bench, and that portion of the right of theL line A-i being a sectional vieiv through the heating flues interposed betvveenmuffles or retorts in the bench. rlie retort shown may be regarded as one in a bench of retorts, certain of which are employed in the manufacture ofy by-product coke in the usual manner, that illustr: ted Jeing employed in association therewith for the manufactureA of phosphorus or phosphorus compounds as hereinafter more fully set forth.
' The retort or inutile chamber 6 is charged with the nhosphatic reaction min ure by the method usual in charging colte ovens coke; thatl is, the reaction mixture is chai thereinto through the ports 7 from suitable hopper cars 8. The individual retorts or ovens of the bench, which are relatively narrow, are heated in the customary manner, by means of a suitable fuel gas supplied through 21, 1925. Serial No. 76,689.
UDS
ic flues from the regenerators 12, the op- 'ati'on of which is not here described, as it that conventional in coke oven practice.
l-.e retorts 6 are provded vith discharge iipes 15, through which the phosphorus vapors given off by the charge pass out to be handled as he iuafter more fully described. i suitable ram 14 is provided for forcing the spent charge from the retort after completion of the reaction.
In carrying out the invention, the phosphatic charge is prepared for the retorts by admiring previously ground phosphate rock and bituminous coal, both being preferably ground so that 90% thereof will pass through a Ll0 mesh screen. The mixture is so made (Withthe addition of suitable quantities of sand, if required) that the resulting charge has approximately7 he following constitution.
Silica (Si02) 18 to 20%.
(CaO) 34 to 37%.
phosphoric acid (P205) 22 to 25%.
Bituminous coal 18 to 25%.
This mixture is then employed as the charge in the retorts 6. Before charging thismiizture` into the retorts, it is preferred that a small quantity of bituminous coal be charged thereinto toform a layer extending Vover the base or .bottom of the oven, the phosphatic charge being then filled in over this laver of bituminous coal.
The ovens having been charged, they are brought to a temperature between 1100o and 11150o C., at vvhich temperature the reaction takes place and phosphorus is evolved. The charge of the proportions hereinbefore set forth is not reduced to a molten condition, nor does it do more than sinter at temperatures as high as 1450O C. The phosphorus is therefore evolved under these conditions Without fusion of the reaction mixture. The relatively narrow width of the retorts or ovens permits of a very even distribution of heat through the charge.
In accordance with this invention, bituminous coal is employed as the carbonaceous reheated air for combustion is supplied to'l constituents of the charge, and as a result of its use there isa shrinkage of the charge during reaction which substantially facilitates the removal of the spent charge from the furnaces. v The employment of abottom layer of bituminous coal in the retorts, as above i, described, aids substantially in preventing fue 'fill treatment.
adhesion of the charge thereto. Although it is preferred touse this bottom layer of bituminous coal, it may be omittedif desired, the proportion ofbiturninous coal in the charge and the resulting shrinkage reducing substantially the adherence of the charge to the Walls of the oven. During reaction, a suitable non-oxidizing gas, such as nitrogen, carbon monoxide or colle-oven gas may be caused to passV through the retorts, thus aiding in sweeping out the phosphorus vapors. rlhus, in the apparatus herein described,l coke-oven gas derived from other ovens of the bench -maybe supplied through the main 25 and the pipe 26 to the interior of thev retorts 6 in Which the phosphatic charge undergoes A current of the non-oxidizing gas thus supplied is preferably passed through the reaction mixture during Vthe entire period of evolution of phosphorus therefrom. f
' The phosphorus vapors, together With the non-oxidizing gas When the latter is employed, pass out through the pipes 15 into the discharge main 16. If phosphorus is desired as the iinal'product, the vapors are caused to pass from the main 16 through the vvalve controlled line 17 to the condensing apparatus illustrateddiagrammatically in Fig. 2.V If'itis desired to oxidize the vphosphorus vapors to form yphosphorus pentoxid and V'plied to effect the desired oxidization. The
resulting gases. includingphosphorus pentoxid and phosphoric acid. pass into a collecting chamber 20, being suitably forced thereinto by a pump 21. Loss of phosphorus pentthe phosphates.
Although the present invention has been described in connection With particular details of apparatus and of a method for carrying itinto effect, it is not intended that these details shall be regarded as limitations upon the scope of the invention, except insofar as included in the accompanying claims.
AWe claim: Y
1. The method of producing phosphorus from a phosphatic material Which comprises preliminarily applying to an interior Wall of an externally heated chamber a layer of bituminous coal, subsequently charging the chamber With a phosphatic material admixed lvvith silica and a carbonaceous material, and
applying heat to remove the phosphorus from the charge, adherence of the charge to the Wall of the chamber being thereby prevented.
2. The Vmethod of producing phosphorus which comprises heating in an externally fired chamber to a temperature between 1100o and 1450o a mixture of natural phosphate, silicious material and bituminous coal, the proportion of bituminous coal being in excess of 18% andl that of silica not being above 20%.
3. The method of producing phosphorus from a phosphatic material Which comprises preliminarily applying to an interior Wall of an externally heated chamber a layer of bituininous coal, subsequently charging the chamber with a phosphaticmaterial admixed With silica and a carbonaceous material, and applying sufficient heat to remove the phosphorus from the charge Without fusing said charge, adherence of the charge to the Wall of the chamber being thereby prevented.
4.-. The method of producing phosphorus yfrom a phosphatic material which comprises preliminarily applying to an interior Wall of an externally heated chamber a layer of bituminous coal, subsequently charging the chamber With a phosphatic material admixed Withl silica and bituminous coal, and applying sufficient heat to remove the phosphorus from the charge Without fusing said charge,
Yadherence of the charge to the Wall 'of the chamber being thereby prevented.
QThe method of producing phosphorus Which comprises heating a phosphatic reaction mixture comprising a natural phosphate, silica and carbonaceous material in a chamber. separatelyand simultaneously heating a Coking coal to a colring temperature, thereby evolving coalgas therefronnand Vdrawing said coal gas through .the heated phosphatic reaction mixture.
llLLlAM H. WAGGAMAN. HENRY W. EASTEBW OOD.
a properly drained bottom, so that the col-
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US76689A US1841071A (en) | 1925-12-21 | 1925-12-21 | Manufacture of phosphorus and compounds thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US76689A US1841071A (en) | 1925-12-21 | 1925-12-21 | Manufacture of phosphorus and compounds thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US1841071A true US1841071A (en) | 1932-01-12 |
Family
ID=22133622
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US76689A Expired - Lifetime US1841071A (en) | 1925-12-21 | 1925-12-21 | Manufacture of phosphorus and compounds thereof |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US1841071A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2897057A (en) * | 1955-08-25 | 1959-07-28 | Sam Tour | Process of winning elemental phosphorus |
| US2974016A (en) * | 1957-06-27 | 1961-03-07 | Virginia Carolina Chem Corp | Process for the production of phosphorus |
| US3052523A (en) * | 1960-02-01 | 1962-09-04 | Kellogg M W Co | Phosphorus production |
| US3056659A (en) * | 1960-02-26 | 1962-10-02 | Kellogg M W Co | Phosphorus production |
| US3433601A (en) * | 1965-10-07 | 1969-03-18 | Monsanto Co | Condensed phosphorus transfer by recycled turbulent phosphorous stream |
| US4578088A (en) * | 1984-12-17 | 1986-03-25 | Fmc Corporation | Electrical insulating and sealing apparatus and process for using same |
-
1925
- 1925-12-21 US US76689A patent/US1841071A/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2897057A (en) * | 1955-08-25 | 1959-07-28 | Sam Tour | Process of winning elemental phosphorus |
| US2974016A (en) * | 1957-06-27 | 1961-03-07 | Virginia Carolina Chem Corp | Process for the production of phosphorus |
| US3052523A (en) * | 1960-02-01 | 1962-09-04 | Kellogg M W Co | Phosphorus production |
| US3056659A (en) * | 1960-02-26 | 1962-10-02 | Kellogg M W Co | Phosphorus production |
| US3433601A (en) * | 1965-10-07 | 1969-03-18 | Monsanto Co | Condensed phosphorus transfer by recycled turbulent phosphorous stream |
| US4578088A (en) * | 1984-12-17 | 1986-03-25 | Fmc Corporation | Electrical insulating and sealing apparatus and process for using same |
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