EP0000698A1 - Appareil pour la préparation du pentoxyde de phosphore hexagonal - Google Patents
Appareil pour la préparation du pentoxyde de phosphore hexagonal Download PDFInfo
- Publication number
- EP0000698A1 EP0000698A1 EP7878100295A EP78100295A EP0000698A1 EP 0000698 A1 EP0000698 A1 EP 0000698A1 EP 7878100295 A EP7878100295 A EP 7878100295A EP 78100295 A EP78100295 A EP 78100295A EP 0000698 A1 EP0000698 A1 EP 0000698A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- cooling
- combustion chamber
- chamber
- condensation chamber
- phosphorus pentoxide
- 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.)
- Granted
Links
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000002485 combustion reaction Methods 0.000 claims abstract description 32
- 238000009833 condensation Methods 0.000 claims abstract description 28
- 230000005494 condensation Effects 0.000 claims abstract description 28
- 238000001816 cooling Methods 0.000 claims abstract description 28
- 238000007654 immersion Methods 0.000 claims abstract description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims description 11
- 239000011574 phosphorus Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 22
- 239000000047 product Substances 0.000 description 6
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229920000137 polyphosphoric acid Polymers 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 3
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005406 washing 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
- C01B25/12—Oxides of phosphorus
Definitions
- the present invention relates to a device for producing hexagonal phosphorus pentoxide, consisting of a water-cooled combustion chamber for phosphorus, which is followed by a cooled condensation chamber for the hexagonal phosphorus pentoxide (P 4 0 10 ).
- Phosphorus pentoxide occurs in several solid modifications.
- the hexagonal shape is used almost exclusively for technical purposes.
- the polymeric glass-like modifications are inert and therefore entirely undesirable.
- phosphorus pentoxide is obtained by burning elemental yellow phosphorus.
- the resulting phosphorus pentoxide vapor is condensed on cooled surfaces.
- this method has been carried out using devices which consist of a combustion chamber equipped with a phosphorus combustion nozzle and which is cooled from the outside by sprinkling with water.
- This combustion chamber is connected to a condensation chamber which carries an exhaust pipe and a discharge device for P 2 O 5 (US Pat. No. 1,700,708).
- this device has the disadvantage that it is not possible to produce hexagonal P205 in a targeted manner since part of the F 2 O 5 formed is already condensed in the combustion chamber. Since this condensation takes place within a very wide temperature range, products are obtained which consist of a mixture of the various modifications of P 2 O 5 .
- DT-PS 1 300 527 It is also known from DT-PS 1 300 527 to use a device for the simultaneous production of hexagonal phosphorus pentoxide and polyphosphoric acid, which consists of a cooled combustion chamber, which at the same time represents the condensation chamber for the P 2 O 5 , which is connected via an exhaust pipe with a reaction tower Connection is established in which the exhaust gases of the combined combustion / condensation chamber are absorbed by circulating phosphoric acid to form polyphosphoric acid.
- the devices used to carry out the known methods also have the disadvantage in common that direct heat transfer by radiation from the very hot phosphor flame to material already deposited cannot be prevented. In a short time, this leads to an at least partial conversion of the crystalline P 2 O 5 into glassy products.
- a device for the production of hexagonal phosphorus pentoxide which consists of a coolable combustion chamber 1 which is equipped with a two-component combustion nozzle 2 for elementary phosphorus and one via a shut-off device 7 with a Collection container 8 for phosphorus pentoxide connected condensation chamber 4 is connected downstream, which carries an exhaust pipe 9.
- This preferably horizontally arranged combustion chamber 1 is provided on its inner wall with cooling tubes 10 and connected to the condensation chamber 4 via a gas cooler 3, the gas cooler 3 consisting of a cooling tube system 5 , which ends in the manner of an open dip tube above the bottom of the condensation chamber 4, the walls of which are provided with a cooling device 6.
- the cooling tubes 10 in the combustion chamber 1 and the cooling tube system 5 of the gas cooler 3 advantageously consist of spiral-wound tube bundles, which are expediently made of stainless steel.
- condensation chamber 4 and gas cooler 3 are dimensioned such that the diameter of the condensation chamber 4 is a multiple of the diameter of the cascooler 3.
- FIG. 1 A preferred embodiment of the device according to the invention is shown schematically in FIG. 1 below.
- FIG. 2 shows an enlarged section which shows the deposition of the polymeric phosphorus pentoxide in the gussets formed by the tubes 5.
- the combustion chamber 1 in which yellow phosphorus is burned in a two-substance nozzle 2 with a gas containing O 2 , consists of several sections of water-cooled stainless steel tubes 10 with an outer protective jacket.
- the use of a combustion chamber 1 consisting of tube bundles 10 has the advantage that intensive cooling is ensured in all sections of this chamber by the forced guidance of the cooling water.
- x is deposited as a result of cooling glassy polymeric phosphoric p entoxid (P 2 0 5) in the interstices, forming the tubes together. This is desirable here because the cooling tubes underneath are protected by this layer.
- the outside wall temperature of the cooled pipes can thus be kept below 100 ° C; on the other hand, the surface temperature of the protective layer made of (P205) x is approximately 650 ° C.
- the temperatures in front of the phosphor nozzle reach up to 2000 ° C. These high temperatures ensure complete oxidation of the P 4 to P 4 0 10 and do not need to be reduced by using a large excess of air or oxygen.
- the O 2 content in the exhaust gas can rather be reduced to near the stoichiometric value, preferably down to ⁇ 2% 0 2 . This is important for the later Ab separation of the P 4 0 10 from the gas flow because the separation is better, the less exhaust gas has to leave the condensation chamber 4 again.
- the amount of exhaust gas can be further reduced and the degree of separation improved accordingly if the dry air usually used for combustion is enriched with pure oxygen to about 40 volume% O 2 .
- the gaseous P 4 0 10 leaves the combustion chamber at a temperature of 800 to 900 ° C.
- this hot gas flows through the spirally turned and water-cooled tube bundle 5 made of stainless steel, which is arranged vertically as an “immersion tube”.
- Additional polymeric phosphorus pentoxide is deposited on the cooled pipe surface.
- the 800 to 900 ° C hot gas from the combustion chamber 1 heats this layer up to approx. 650 ° C.
- the (P 2 O 5 ) x starts to evaporate again.
- the layer here on the wall of the first cooling section is in evaporation equilibrium with the hot gas flowing past from the combustion chamber, ie the layer only reaches a certain thickness. Following the course of the temperature, it is only weakly formed in the upper part of the cooling device 3 at the connection to the combustion chamber 1, only weakly with a falling temperature.
- the gas containing P 4 0 10 is cooled from the combustion chamber 1 to a temperature of 650 to 400 ° C. It has then been cooled down to such an extent that it can be suddenly cooled to ⁇ 300 ° C. when it enters the condensation chamber 4.
- this pre-cooling in which one separates the polymeric phosphorus pentoxides for the formation of the above-described equilibrium state, it is achieved that there are no transition states with condensation of other phosphorus pentoxide modifications in the subsequent condensation chamber 4, but that the P 4 O 10 is only reflected in the desired hexagonal modification.
- the hexagonal product is then deposited on these cooled surfaces of the condensation chamber 4, which have a wall temperature of 100 ° C. It collects in the lower part of the condensation chamber 4 and is discharged into a collecting container 8 via a lock 7. Based on the phosphorus used, the yield of hexagonal F4010 is more than 90%.
- the degree of separation can be increased to more than 94% by using a combustion gas which is enriched with oxygen up to approx. 40 volume% 0 2 .
- the exhaust gas that emerges from the condensation chamber 4 through the nozzle 9 has a temperature of 100 to 120 ° C.
- the relatively small amounts of exhaust gas which only have a minimal content of P 4 0 10 , can then be cleaned without great effort, if necessary, by washing with water, phosphoric acid or the like before they are passed into the atmosphere.
- the advantage of the device according to the invention is essentially that it prevents the direct heat radiation of the phosphorus flame onto deposited P 2 O 5 and also enables a targeted cooling of the reaction product, with a relatively large temperature difference in and in a relatively small space in the first cooling phase the second phase in a relatively large space a relatively small temperature difference is achieved.
- the gas containing F 4 O 10 expands into the cooled condensation chamber 4, which surrounds the cooling device 3 over a wide area, which results in a further sudden cooling of the gas.
- Hexagonal loose P 4 0 10 settles on the cooled walls of the condensation chamber 4 .
- Pneumatic tapping devices knock the product off the walls. It collects in the lower part. the condensation chamber 4. 355 kg of phosphorus pentoxide are discharged here every hour.
- the product is free of suboxides, reacts spontaneously with water and is free of glass-like impurities in the polymeric form of P 2 O 5 .
- the yield based on the elemental phosphorus used, is 91%.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treating Waste Gases (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE2736765 | 1977-08-16 | ||
| DE19772736765 DE2736765A1 (de) | 1977-08-16 | 1977-08-16 | Vorrichtung zur herstellung von hexagonalem phosphorpentoxid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0000698A1 true EP0000698A1 (fr) | 1979-02-21 |
| EP0000698B1 EP0000698B1 (fr) | 1981-08-05 |
Family
ID=6016444
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP78100295A Expired EP0000698B1 (fr) | 1977-08-16 | 1978-07-03 | Appareil pour la préparation du pentoxyde de phosphore hexagonal |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US4219533A (fr) |
| EP (1) | EP0000698B1 (fr) |
| JP (1) | JPS5443195A (fr) |
| AT (1) | AT377957B (fr) |
| CA (1) | CA1097034A (fr) |
| DE (2) | DE2736765A1 (fr) |
| IT (1) | IT1106883B (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0242678A3 (en) * | 1986-04-25 | 1989-02-01 | Hoechst Aktiengesellschaft | Process for the preparation of phosphorus pentoxide with reduced reactivity |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3033109A1 (de) * | 1980-09-03 | 1982-04-22 | Hoechst Ag, 6000 Frankfurt | Verfahren zur herstellung von phosphorpentoxid unter ausnutzung der reaktionswaerme |
| DE3315630A1 (de) * | 1983-04-29 | 1984-10-31 | Hoechst Ag, 6230 Frankfurt | Verfahren und vorrichtung zur herstellung von phosphorpentoxid unter ausnutzung der reaktionswaerme |
| US4713228A (en) * | 1983-05-23 | 1987-12-15 | Fmc Corporation | Heat recovery in the manufacture of phosphorus acids |
| DE3926105A1 (de) * | 1989-08-08 | 1991-02-14 | Metallgesellschaft Ag | Vorrichtung zum katalytischen umsetzen eines h(pfeil abwaerts)2(pfeil abwaerts)s und so(pfeil abwaerts)2(pfeil abwaerts) enthaltenden gasgemisches nach dem clausverfahren |
| US8551437B2 (en) * | 2008-11-12 | 2013-10-08 | Straitmark Holding Ag | Process for the manufacture of P4O6 with improved yield |
| KR20130041183A (ko) * | 2010-07-08 | 2013-04-24 | 솔베이(소시에떼아노님) | LiPO2F2의 제조법 및 결정형 LiPO2F2 |
| EP2605646B1 (fr) | 2010-08-18 | 2016-07-20 | Monsanto Technology LLC | Application précoce des acetamides encapsulés pour eviter des dégâts à des plantes cultivées |
| EA202191330A1 (ru) * | 2018-11-19 | 2021-09-20 | Монсанто Текнолоджи ЛЛК | Способы производства оксида фосфора и фосфорной кислоты |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU179752A1 (ru) * | Научно исследовательский институт удобрени , инсектофунгици | Способ получения фосфорного ангидрида | ||
| GB197863A (en) * | 1922-07-06 | 1923-05-24 | Richard Threlfall | Improved manufacture of phosphorus pentoxide |
| US2132360A (en) * | 1936-05-19 | 1938-10-04 | American Agricultural Chem Co | Vaporizing and oxidizing phosphorus |
| US2532322A (en) * | 1946-06-01 | 1950-12-05 | Tennessee Valley Authority | Phosphorus combustion furnace |
| FR1292032A (fr) * | 1961-06-12 | 1962-04-27 | Stauffer Chemical Co | Procédé et appareillage pour le traitement de l'anhydride phosphorique |
| FR1305386A (fr) * | 1961-04-11 | 1962-10-05 | Stauffer Chemical Co | Procédé de préparation d'anhydride phosphorique |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1478750A (en) * | 1922-02-09 | 1923-12-25 | Gulf Refining Co | Process of and apparatus for condensation |
| US1700708A (en) * | 1925-10-22 | 1929-01-29 | Firm I G Farbenindustrie Ag | Production of phosphorus pentoxide and phosphoric acid |
| DE2109350A1 (de) * | 1971-02-27 | 1972-10-26 | Metallgesellschaft AG, 6000 Frankfurt; Deutsche Babcock & Wilcox-AG, 4200 Oberhausen | Verfahren zur Gewinnung von Phosphorpentoxid |
-
1977
- 1977-08-16 DE DE19772736765 patent/DE2736765A1/de not_active Withdrawn
-
1978
- 1978-07-03 EP EP78100295A patent/EP0000698B1/fr not_active Expired
- 1978-07-03 DE DE7878100295T patent/DE2860894D1/de not_active Expired
- 1978-08-09 CA CA308,985A patent/CA1097034A/fr not_active Expired
- 1978-08-11 US US05/932,804 patent/US4219533A/en not_active Expired - Lifetime
- 1978-08-11 IT IT50721/78A patent/IT1106883B/it active
- 1978-08-14 AT AT0590878A patent/AT377957B/de not_active IP Right Cessation
- 1978-08-16 JP JP9993778A patent/JPS5443195A/ja active Granted
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU179752A1 (ru) * | Научно исследовательский институт удобрени , инсектофунгици | Способ получения фосфорного ангидрида | ||
| GB197863A (en) * | 1922-07-06 | 1923-05-24 | Richard Threlfall | Improved manufacture of phosphorus pentoxide |
| US2132360A (en) * | 1936-05-19 | 1938-10-04 | American Agricultural Chem Co | Vaporizing and oxidizing phosphorus |
| US2532322A (en) * | 1946-06-01 | 1950-12-05 | Tennessee Valley Authority | Phosphorus combustion furnace |
| FR1305386A (fr) * | 1961-04-11 | 1962-10-05 | Stauffer Chemical Co | Procédé de préparation d'anhydride phosphorique |
| FR1292032A (fr) * | 1961-06-12 | 1962-04-27 | Stauffer Chemical Co | Procédé et appareillage pour le traitement de l'anhydride phosphorique |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0242678A3 (en) * | 1986-04-25 | 1989-02-01 | Hoechst Aktiengesellschaft | Process for the preparation of phosphorus pentoxide with reduced reactivity |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0000698B1 (fr) | 1981-08-05 |
| IT1106883B (it) | 1985-11-18 |
| CA1097034A (fr) | 1981-03-10 |
| US4219533A (en) | 1980-08-26 |
| ATA590878A (de) | 1984-10-15 |
| JPS5510527B2 (fr) | 1980-03-17 |
| DE2860894D1 (en) | 1981-11-05 |
| IT7850721A0 (it) | 1978-08-11 |
| JPS5443195A (en) | 1979-04-05 |
| AT377957B (de) | 1985-05-28 |
| DE2736765A1 (de) | 1979-03-01 |
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