CA2817124C - Method for recycling organic waste material - Google Patents

Method for recycling organic waste material Download PDF

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Publication number
CA2817124C
CA2817124C CA2817124A CA2817124A CA2817124C CA 2817124 C CA2817124 C CA 2817124C CA 2817124 A CA2817124 A CA 2817124A CA 2817124 A CA2817124 A CA 2817124A CA 2817124 C CA2817124 C CA 2817124C
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phosphorus
drawn
oxides
chlorides
combustion chamber
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CA2817124A1 (fr
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Alfred Edlinger
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Italmatch Chemicals SpA
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ICL Europe Cooperatief UA
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/08Other phosphides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/01Treating phosphate ores or other raw phosphate materials to obtain phosphorus or phosphorus compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/02Preparation of phosphorus
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/18Treatment of sludge; Devices therefor by thermal conditioning
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/004Sludge detoxification
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/06Treatment of sludge; Devices therefor by oxidation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/40Valorisation of by-products of wastewater, sewage or sludge processing

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Thermal Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Processing Of Solid Wastes (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The invention relates to a method for recycling organic waste material containing phosphorus oxides and metal oxides, in particular for recycling sewage sludge.

According to the invention, the waste materials are mixed with chlorine carriers and then heat treated at an air ratio of 0.85 <=.lambda.<= 1.6 and at least partially oxidized. The metal chlorides formed are drawn off and recovered and the fraction remaining after the metal chlorides have been drawn off is subjected to reduction in order to obtain elemental phosphorus.

Description

METHOD FOR RECYCLING ORGANIC WASTE MATERIAL
The invention relates to a method for recycling organic waste material containing oxides of phosphorus and metal oxides, in particular for recycling sewage sludge.
Recycling organic waste material, in particular sewage sludge, dry sludge, sewage sludge ash and animal meal, is an important aspect of environmental technology;
because of the complex composition of the waste material involved, recycling is particularly difficult if, in addition to largely harmless natural substances, the waste material also contains environmental toxine such as heavy metals, halogens, pesticides, herbicides, antibiotics, carcinogenic and mutagenic contaminants, chlorinated hydrocarbons, polychlorinated biphenyls, hormones and endocrines. Along with the heavy metals copper, zinc and cadmium, sewage sludge also contains various oxides of calcium, silicon and aluminium, and in particular the presence of iron oxides renders the extraction of pure phosphorus impossible since phosphorus binds with iron to form iron phosphide and thus cannot be obtained in its pure form when iron is present. The quantity of the various metals and heavy metals usually prevents sewage sludge from being used directly as a fertilizer, and so sewage sludge has to be dumped in large quantities. However, dumping sewage sludge means that the recyclable materials contained therein, in particular phosphorus, which is flot just of interest to the fertilizer industry, cannot be put to use.
Thus, the aim of the present invention is to extract phosphorus or its derivatives in as pure a form as possible as a recyclable material from organic waste material and in particular from sewage sludge, and to separate out the metals it contains.
-2 -According to one embodiment of the present invention, the waste material of the aforementioned type is mixed with chienne carriers and then heat treated at an air ratio cf 0.85 5 I 5 1.6 and partially oxidized, the metal chlorides formed are drawn off and recovered and the fraction remaining after the metal chlorides have been drawn off undergoes a reduction in order to obtain gaseous elemental phosphorus, salol elemental phosphorous is drawn off and recovered.
The fact that the waste material to be processed is mixed with chloride carriers means that .in the subsequent oxidation step, which is carried out at raised temperatures, the metals are transformed into metal chlorides which are volatile and thus can be drawn off with the gas phase. In accordance with the invention, the remaining fraction then undergoes a reduction, whereupon pure phosphorus is obtained from the oxides of phosphorus. Thus, using the method of the invention, the aforementioned metals and metal oxides and in particular the mon oxides are séparated out as metal chlorides before the phosphorus is extracted in its elemental form by reduction.
Preferably, the heat treatment is carried out 'at temperatures of 1300 C - 1600 C.
In a preferred implementation, the method of the invention is further refined by the tact that in addition, lime is added to the waste material. In the method of the present invention, lime forms liquid molten slag with the inorganic combustion products; the quantity of lime to be added should be adapted to the Si02 content of the combustion products; in particular, a ratio of 0.85 5 CaO/Si02 5 1.3 should be established.
The slag which is produced can be used to good effect in the cernent industry.
- 3 -In order to obtain high efficiency in the oxidation step, the waste material is advantageously introduced into the oxidation step in a finely divided state. In accordance with a preferred embodiment of the present invention, the method is advantageously further refined in that for the purposes of oxidation, the waste material mixed with the chloride carriers is forced into a combustion chamber with a carrier gas via a cyclone, whereby preferably, an oxygen-containing gas, in particular hot air, is used as the carrier gas. As an example, a method of this type can be carried out with the device of WO 03/070651 Al, which device has already been used successfully for melting dust. In that device, the cyclone is upstream of the actual combustion chamber and the material or the waste material is blown in tangentially with the carrier gas and set in a rotary motion so that the waste material is introduced into the downstream combustion chamber with a preferred spin.
Upon entering the combustion chamber, rotation of the flow can be maintained for as long as possible so that a relatively long contact time with the flame is ensured over a relatively short axial length in the combustion chamber, and thus the reaction time which is available for oxidation is relatively long.
A particularly advantageous synergistic effect exists with other branches of industry and areas of the waste industry if, in a preferred embodiment of the present invention, the method is further refined such that the chloride carriers are selected from the group consisting of chloride-containing polymers, alkali chlorides, alkaline-earth chlorides, cernent kiln dust and steel mill dust. Chloride-containing polymers are available, for example, in the form of PVC, and cernent kiln dust and steel mill dust are considered to be problematic waste material in the respective branches of the industry, and so these materials are readily and cheaply
- 4 -available for carrying out the method of the invention and can be put to good use.
In accordance with the present invention, after the oxidation step and drawing off the metal chlorides formed in the oxidation step, a step for reduction of the remaining fraction, which contains the phosphorus, is carried out; in this case, preferably, the fraction remaining after drawing off the metal oxides is reduced using an at least partially inductively heated column with lump coke and/or graphite and the elemental phosphorus which is liberated is drawn off. At the same time, the reduction gas formed (CO, H2) is drawn off.
Following phosphorus condensation, this gas can be used as a reduction or combustion gas, for example as an energy supply for the heat treatment of the waste material. Reduction on an at least partially inductively heated column is known, for example, from WO 2006/079132 Al; that document also discloses an appropriate device for carrying out a reduction step.
Using an at least partially inductively heated coke column means that exceedingly high temperatures can be obtained, whereupon a reducing atmosphere can be set up since the carbon of the column is flot in thermal equilibrium with combustion products and in particular flot with CO2. In contrast to the method described in WO
2006/079132 Al, when using an inductively heated column the recyclable material is flot contained in the melt, but is drawn off with the reaction gas and, in a preferred embodiment of the present invention, can be obtained as white phosphorus by quenching.
In a preferred embodiment of the present invention, in the reduction step, the redox potential of the column is adjusted by blowing in gases and the temperature of the column is adjusted by adjusting the electrical power and by blowing in gases. In this manner, the redox
- 5 -potential and the temperature can be adjusted such that only the desired phosphorus is reduced and other oxides remain in the residual fraction.
The method of the invention is employed to separate the metals or metal oxides from phosphorus prior to the reduction step, in order to prevent the uncontrolled formation of iron phosphide.
When, however, the phosphorus contained in the waste material has been produced in its pure form using the method of the invention, the production of pure iron phosphide may in fact be desired, since the oxidation of iron phosphide produces iron phosphate which is a valuable starting material for the manufacture of lithium iron phosphate. Lithium iron phosphate itself is rapidly gaining importance as a cathode in lithium ion batteries. The method of the invention is thus preferably further refined in that the residual fraction after drawing off the metal chloride is mixed with iron or iron oxide. The lithium required may be obtained from clinker kiln dust, for example.
In a further aspect of the invention, an alternative, simplified procedure is provided in which the cited waste material and lime are placed on an inductively heated coke and/or graphite bed.
The resulting exhaust gas then undergoes fractionating cooling:
at 400-600 C, the chloride-containing contaminants precipitate out and can be separated by means of a cyclone or hot gas separator. Further cooling, for example in a water quench, results in the condensation of phosphorus. The remaining gas can be used as a combustion and/or reaction gas after optional drying.

- 5a -According to one aspect of the present invention, there is provided a method for recycling organic waste material containing oxides of phosphorus and metal oxides comprising iron oxides in which the waste material is mixed with chlorine 5 carriers and then heat treated at an air ratio of 0.85 X --1.6 and at least partially oxidized, and the metal chlorides formed are drawn off and recovered and the fraction remaining after the metal chlorides have been drawn off undergoes a reduction in order to obtain elemental phosphorus.
According to another aspect of the present invention, there is provided a method for recycling organic waste material containing oxides of phosphorus and metal oxides comprising iron oxides in which the waste material is mixed with chlorine carriers and then heat treated at an air ratio of 0.85 X _<
1.6 and at least partially oxidized, and the metal chlorides formed are drawn off and recovered and the fraction remaining after the metal chlorides have been drawn off is supplemented with iron or iron oxide in order to produce iron phosphide.
The invention will now be described in more detail with the aid of an exemplary embodiment illustrated in a diagrammatic manner in the drawings. In the drawings,
- 6 -Figure 1 shows a device for carrying out the method of an embodiment of the invention. Figure 2 shows a block diagram of a simplified procedure. Figure 3 shows a reduction.
device for carrying out the simplified method.
In Figure 1, the reference numeral 1 indicates a device for carrying out the method of an embodiment of the invention.
The waste material is supplemented with chloride carriers and/or lime and sent to the infeed station 2. The reference numeral 3 indicates a dosing device, for example in the form of a conveying screw; it is used to convey the materials into the interior of a combustion chamber 4.
A ring une 5 which opens into the combustion chamber 4 at appropriate locations can be used to set an appropriate air ratio of air, 02 and, if appropriate, gaseous chloride carriers. Downstream of the combustion chamber is a cyclone or droplet separator 6 in which the melt with the partially oxidized phosphorus is separated from the product gas. The product gas or reduction gas, which contains CO2, CO, H20 and H2 in addition to the metal chlorides, is drawn off via the discharge une 7.
The melt, if appropriate supplemented with 02 and carbon carriers, is sent to a coke and/or graphite bed 8. The coke and/or graphite bed 8 is inductively heated by means of the cou l 9. Reduction to elemental phosphorus occurs in the bed 8; the phosphorus is drawn off via the opening 10 and can then be condensed and obtained as white phosphorus. The residual molten slag collects in a tundish 11; after tapping, it can, if appropriate, = be further processed into iron phosphide and iron phosphate.
In Figure 2, it can be seen that in a simplified procedure, the waste material along with lime carriers and coal dust from respective hoppers 12, 13 and 14 are placed in a mixer 15. From the mixer, the mixture is placed sent to an infeed device of a reduction reactor
-7-16. In the reduction reactor 16, the metal oxides are reduced and pig iron and cernent slag can be tapped off at the tundish 17. The hot gases are drawn off at temperatures of approximately 1600 C and cooled to about 400 C in a heat exchanger 18. Heavy metals, alkalis and halogens can now be separated in an appropriate separator 19 and the remaining gas, which also contains phosphorus in addition to CO and H2, is subjected to a water quench 20, where the phosphorus condenses out and can be collected in an appropriate receptacle 21 as white phosphorus. The residual combustion gas or product gas is withdrawn via the flue 22.
Figure 3 shows parts of the reduction device in more detail. The reference numeral 23 indicates an infeed device via which the starting materials are supplied to a coke and/or graphite bed 24 in as even a manner as possible. The bed 24 rests on a lining 25 formed from refractory material and is heated inductively by means of the cou l 26. In addition to the discharge for the molten iron and the cernent slag, the tundish 17 has a flue 27 for the product gases which then undergo fractionating condensation.

Claims (10)

CLAIMS:
1. A method for recycling organic waste material containing oxides of phosphorus and metal oxides comprising iron oxides in which the waste material is mixed with chlorine carriers and lime, and then at least partially oxidized in a combustion chamber at an air ratio of 0.85<=.lambda.<=1.6, and the metal chlorides formed are drawn off and recovered and the phosphorus-containing melt fraction remaining after the metal chlorides have been drawn off undergoes a reduction in order to obtain gaseous elemental phosphorus, said elemental phosphorous is drawn off and recovered.
2. The method as claimed in claim 1, wherein the oxidation in the combustion chamber is carried at temperatures of 1300°C-1600°C.
3. The method as claimed in claim 1 or 2, wherein for the purposes of oxidation, the waste material mixed with the chlorine carriers is forced into the combustion chamber with a carrier gas via a cyclone.
4. The method as claimed in claim 3, wherein an oxygen-containing gas is used as the carrier gas.
5. The method as claimed in claim 4, wherein the oxygen-containing gas is hot air.
6. The method as claimed in any one of claims 1 to 5, wherein the chlorine carriers are chloride-containing polymers, or alkali chlorides, or alkaline-earth chlorides, or cement kiln dust, or steel mill dust.
7. The method as claimed in any one of claims 1 to 6, wherein the fraction remaining after drawing off the metal chlorides is reduced using an at least partially inductively heated column with at least one of lump coke and graphite, and the elemental phosphorus which is liberated is drawn off.
8. The method as claimed in any one of claims 1 to 7, wherein the phosphorus which is drawn off is obtained as white phosphorus by quenching.
9. The method as claimed in claim 7, wherein the redox potential of the column is adjusted by blowing in gases and the temperature of the column is adjusted by adjusting the electrical power and by blowing in gases.
10. The method as claimed in any one of claims 1 to 9, wherein the organic waste material is sewage sludge.
CA2817124A 2010-11-15 2011-10-18 Method for recycling organic waste material Active CA2817124C (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT0187510A AT509593B1 (de) 2010-11-15 2010-11-15 Verfahren zum aufarbeiten von organischen abfallstoffen
AT1875/2010 2010-11-15
PCT/EP2011/068157 WO2012065798A2 (fr) 2010-11-15 2011-10-18 Procédé de traitement de déchets organiques

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CA2817124A1 CA2817124A1 (fr) 2012-05-24
CA2817124C true CA2817124C (fr) 2018-08-14

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US (1) US9751762B2 (fr)
EP (1) EP2640531B1 (fr)
JP (1) JP5843877B2 (fr)
AT (1) AT509593B1 (fr)
CA (1) CA2817124C (fr)
DK (1) DK2640531T3 (fr)
ES (1) ES2639400T3 (fr)
HU (1) HUE036221T2 (fr)
PL (1) PL2640531T3 (fr)
PT (1) PT2640531T (fr)
WO (1) WO2012065798A2 (fr)

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JP5941344B2 (ja) * 2012-06-12 2016-06-29 株式会社クボタ 配合剤、藻場構造物、植生構造物、及び配合剤の製造方法
CA2910015A1 (fr) * 2013-05-03 2014-11-06 Outotec (Finland) Oy Procede et installation de separation de metaux lourds a partir d'une matiere premiere phosphorique
AT518979B1 (de) * 2016-11-15 2018-03-15 Radmat Ag Verfahren und Vorrichtung zur Aufarbeitung einer Eisenoxid und Phosphoroxide enthaltenden Schmelze
AT519251B1 (de) * 2016-12-30 2018-05-15 Radmat Ag Verfahren zur Aufarbeitung von Eisenoxid und Phosphoroxide enthaltenden Stäuben
EP3670468B1 (fr) 2018-12-21 2021-11-24 Scheuch GmbH Procédé d'obtention d'une matières première secondaire pour la production de ciment et cimenterie
NL2023083B1 (en) * 2019-05-07 2020-11-30 Axpip Bv A process for recovering elemental phosphorus
AT523447B1 (de) * 2020-02-02 2021-08-15 Alfred Edlinger Dipl Ing Verfahren zum Abtrennen von Phosphor und/oder Phosphorverbindungen aus eisen(oxid)haltigen Phosphor- und/oder Phosphatträgern
EP4097046A1 (fr) 2020-02-02 2022-12-07 Radmat AG Procédé de séparation de phosphore et/ou de composés à base de phosphore à partir de supports de phosphore et/ou de supports de phosphate contenant du fer (oxyde)
WO2021175406A1 (fr) * 2020-03-02 2021-09-10 Montanuniversität Leoben Appareil et processus de traitement thermique de matière première contenant des composés du lithium et des composés du phosphore, procédé de récupération du lithium et/ou du phosphore contenus dans le matériau résiduaire de batteries au lithium-ion
CN111484226A (zh) * 2020-04-24 2020-08-04 大庆市奥普斯石油科技有限公司 一种含油污泥脱水烘干设备
AT524558B1 (de) * 2021-06-02 2022-07-15 Radmat Ag Aufarbeiten von Eisenoxid-haltigen und Phosphat-haltigen Edukten
JP6962536B1 (ja) * 2021-06-25 2021-11-05 学校法人福岡工業大学 製鋼スラグの処理方法
CN114110608B (zh) * 2021-11-29 2022-06-24 崇左南方水泥有限公司 一种利用工业余热协同处置废弃物的系统及其方法
CN114380323A (zh) * 2022-02-11 2022-04-22 株洲科能新材料股份有限公司 一种磷化铟中铟的回收方法

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AT403294B (de) 1994-10-10 1997-12-29 Holderbank Financ Glarus Verfahren zum aufarbeiten von müll oder von metalloxidhaltigen müllverbrennungsrückständen sowie vorrichtung zur durchführung dieses verfahrens
AT405944B (de) * 1996-04-19 1999-12-27 Holderbank Financ Glarus Verfahren zum reduzieren von oxidischen schlacken
JP3774994B2 (ja) * 1997-06-06 2006-05-17 月島機械株式会社 資源分離法および装置
US6022514A (en) * 1998-05-18 2000-02-08 Nkk Corporation Method for recovering phosphorus from organic sludge
JP3619699B2 (ja) * 1999-03-19 2005-02-09 Jfeエンジニアリング株式会社 燐回収設備及び燐回収方法
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AT411363B (de) 2002-02-21 2003-12-29 Tribovent Verfahrensentwicklg Einrichtung zum schmelzen von stäuben
JP2008528256A (ja) 2005-01-27 2008-07-31 パトコ エンジニアリング ゲゼルシャフト ミット ベシュレンクテル ハフツング 金属酸化物を含有するスラグ又はガラスを還元する方法及び/又は無機溶融物を脱ガスする方法及び該方法を実施する装置
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Publication number Publication date
DK2640531T3 (en) 2017-08-07
AT509593B1 (de) 2011-10-15
EP2640531A2 (fr) 2013-09-25
PL2640531T3 (pl) 2017-11-30
JP5843877B2 (ja) 2016-01-13
WO2012065798A3 (fr) 2013-06-13
HUE036221T2 (hu) 2018-06-28
PT2640531T (pt) 2017-09-04
AT509593A4 (de) 2011-10-15
US20130272944A1 (en) 2013-10-17
JP2013544184A (ja) 2013-12-12
EP2640531B1 (fr) 2017-06-07
WO2012065798A2 (fr) 2012-05-24
US9751762B2 (en) 2017-09-05
ES2639400T3 (es) 2017-10-26
CA2817124A1 (fr) 2012-05-24

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