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WO2025045768A1 - Récupération de silicium sous forme de tétrachlorure de silicium à partir de biocharbon - Google Patents

Récupération de silicium sous forme de tétrachlorure de silicium à partir de biocharbon Download PDF

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Publication number
WO2025045768A1
WO2025045768A1 PCT/EP2024/073697 EP2024073697W WO2025045768A1 WO 2025045768 A1 WO2025045768 A1 WO 2025045768A1 EP 2024073697 W EP2024073697 W EP 2024073697W WO 2025045768 A1 WO2025045768 A1 WO 2025045768A1
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WO
WIPO (PCT)
Prior art keywords
silicon
biochar
phosphorus
sewage sludge
content
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.)
Pending
Application number
PCT/EP2024/073697
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German (de)
English (en)
Inventor
Matthias Boll
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Lanxess Deutschland GmbH
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Lanxess Deutschland GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from EP23194301.0A external-priority patent/EP4516733A1/fr
Application filed by Lanxess Deutschland GmbH filed Critical Lanxess Deutschland GmbH
Publication of WO2025045768A1 publication Critical patent/WO2025045768A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • C01B33/10715—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material
    • C01B33/10721—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material with the preferential formation of tetrachloride

Definitions

  • the present invention relates to the recovery of silicon in the form of tetrachloride from biochar.
  • An alternative use of biomass using sewage sludge from wastewater treatment plants as an example, is that it is usually partially mechanically dewatered and/or thermally pre-dried and burned in incineration plants, possibly together with domestic or industrial waste.
  • the resulting ash is a mainly inorganic residue that contains various compounds of elements such as phosphorus (P), iron (Fe), aluminum (AI), calcium (Ca) and silicon (Si). Disposing of this ash by spreading it into the environment without further treatment can lead to serious environmental pollution, mainly due to the presence of heavy metals and other toxic substances.
  • the incineration of sewage sludge in preparation for the recovery of essential recyclable materials is a process step that does not, however, add any value. It simply serves to reduce the amount of waste.
  • the heat generated by the incineration is generally used in full to pre-dry new sewage sludge.
  • the concentration in sewage sludge is usually around 30% by weight of solids
  • silicon is usually around 1 to 12% by weight
  • phosphorus is around 1.5 to 15% by weight, each expressed in elemental form.
  • Silicon tetrachloride can and is currently preferably produced from the elements, but also from a mixture of sand and coal with chlorine.
  • diatomaceous earth with a high BET surface area is converted to silicon tetrachloride with chlorine, but only with the addition of special chlorides such as nickel chloride (see example 1) and in the presence of special types of coal with a high BET surface area, at temperatures as low as 500°C.
  • special chlorides such as nickel chloride (see example 1)
  • special types of coal with a high BET surface area at temperatures as low as 500°C.
  • normal beach sand with a smaller surface area does not react to silicon tetrachloride under these conditions below 1290°C (see comparative example 1).
  • SiC is also used as a starting material for the production of silicon tetrachloride.
  • temperatures of 1000°C to 1600°C are used, as described in US2843458.
  • EP3984966A1 describes a process for the extraction of phosphorus in the form of struvite from raw sludge produced in sewage treatment plants by a hydrolysis step.
  • EP2176177B1 also describes a precipitation process for recovering phosphate from biomass.
  • EP3061725B1 describes a process for recovering phosphorus from biomass by hydrothermal carbonization and then releasing the phosphorus as phosphate by lowering the pH value.
  • acid which inevitably leads to the formation of large quantities of neutral salts through the subsequent neutralization.
  • the processing process is usually laborious and the costs are correspondingly high. Because aqueous suspensions are processed, the energy costs for stirring or pumping are very high.
  • all of the processes only lead to a phosphate, which can be used in agriculture, but not to higher-value products such as phosphorus-chlorine compounds as raw materials for the chemical industry.
  • Biomass such as plant residues is usually recycled by drying and dry pyrolysis to produce so-called biochar. Such processes are described, for example, in EP3919586 and produce a product such as that described in WO2023/275271.
  • plant residues always contain considerable amounts of silicon. In the ash, this is around 16 to 26% calculated as SiO2, 8 to 13% by weight calculated as elemental Si (see, for example, “Austrian Federal Ministry of Agriculture, Forestry, Environment and Water Management, BIOMASS ASH FLOWS IN AUSTRIA, Birgit Walter, Peter Mostbauer, Brigitte Karigl, REPORT REP-0561 Vienna, 2016”, Table 21).
  • Pyrolysis of plant residues is usually carried out to bind the carbon contained in them and prevent the formation of carbon dioxide through rotting.
  • the products are usually spread on fields as so-called biochar.
  • phosphorus-chlorine compounds can be used to produce, for example, flame retardants or high-purity phosphoric acid
  • high-purity SiCL can be used to produce very clean SiO2 or “fumed silica” for the production of fiber optic cables or polycrystalline silicon for the semiconductor industry.
  • the object of the invention is therefore to produce silicon compounds and preferably phosphorus compounds in the form of their chlorine compounds starting from a biomass base. solution to the task
  • the invention now relates to a process for the recovery of silicon in the form of the tetrachloride, in which biochar with a silicon content, expressed in wt. % of elemental silicon, of at least 1 wt. %, in particular at least 5 wt. %, preferably from 5 to 40 wt. %, particularly preferably from 7 to 30 wt. %, is reacted with elemental chlorine at a temperature of 350 to 900°C, preferably from 400 to 850°C, particularly preferably from 500°C to 800°C, and the silicon tetrachloride formed is separated from the exhaust gas stream, preferably by condensation.
  • Biochar which in English is also referred to as “biochar”, for example from EP3285920A1, is understood to mean the pyrolysis product of a biomass, more precisely the preferably solid pyrolysis residue of a biomass, which in the case of the present invention is the pyrolysis residue of a silicon-containing biomass.
  • a preferably used biochar has a Si content, determined as elemental silicon, of at least 5 wt.%, preferably from 5 to 40 wt.%, particularly preferably from 7 to 30 wt.%.
  • Si content determined as elemental silicon, of at least 5 wt.%, preferably from 5 to 40 wt.%, particularly preferably from 7 to 30 wt.%.
  • Preferred further inorganic components, each described as elements, may be included:
  • Phosphorus from 2 to 19 wt.%, and in particular
  • Titanium from 0 to 2 wt.%.
  • a preferably used biochar contains, in addition to the described proportion of Si compounds calculated as Si element, also phosphorus from 2 to 19 wt.%, in particular from 5 to 16 wt.% and preferably also iron from 3 to 14 wt.% and aluminum from 0.4 to 13 wt.%, each described as elements.
  • the biochar used in the process according to the invention preferably contains a carbon content of more than 20% by weight. If it has a lower carbon content of 20% or less by weight, the content can be increased by adding another carbon source.
  • the biochar can be used as it is produced from pyrolysis or it can be shaped. This can be done, for example, by extrusion, tableting, pelletizing, granulation or briquetting. If necessary, a binder and possibly water can be added to the biochar beforehand for shaping.
  • shaping can also take place at the level of the previous biomass used for pyrolysis, which remains largely intact after pyrolysis.
  • the shaping of the biochar is optional.
  • Pre-drying the biomass used in pyrolysis to a certain water content is optional. However, pre-dried material can be shaped more easily. This step is optional.
  • biomass and optionally one or more carbon sources are mixed, optionally formed into shaped bodies with a binder and solvent such as water and dried. If the carbon content in the carbon source is less than 70% by weight, pyrolysis is preferably carried out before mixing with sewage sludge or sewage sludge coal. In a particular embodiment, drying and pyrolysis can also be combined, for example by using a biomass with a water content of preferably >15 wt.%, in particular >12 wt.% under otherwise identical conditions.
  • the pyrolysis is particularly preferably carried out under inert gas such as nitrogen.
  • the pyrolysis is preferably carried out at temperatures of 350 to 550°C.
  • the pyrolysis is carried out in particular until the gas formation of volatile components is less than 11 gas / 1 kg of biomass used per hour.
  • the biochar thus obtained preferably has a carbon content of 3 to 45 wt.%.
  • the biochar obtained can preferably be diluted by adding sewage sludge ash or other silicon-containing bioashes from biomasses with lower carbon content, thereby improving the efficiency of the process.
  • biomass means the combustion residue of a biomass or biochar, preferably with a carbon content of preferably less than 3% by weight, in particular less than 1% by weight, particularly preferably less than 0.1% by weight.
  • the biomass preferably used for pyrolysis has a water content of less than 15% by weight, in particular less than 12% by weight, particularly preferably less than 8% by weight, very particularly preferably less than 4% by weight, which is preferably obtained by thermally drying a biomass with a water content of 12% by weight or more, particularly 15% by weight or more.
  • the biomass can be shaped by extrusion, tabletting, pelletizing, granulation or briquetting. If necessary, a binder and possibly also water can be added to the biomass beforehand.
  • the shaping of the biomass is optional.
  • the biochar used in the process according to the invention is preferably the pyrolysis residue of a biomass, preferably sewage sludge, animal manure, also in a mixture with bedding, microalgae, aquatic plants, wood chips, wood waste, agricultural waste, straw, plants, fruits and the like.
  • Biomasses usually have a Si content which leads to a pyrolysis residue, the biochar, with a Si content of at least 1 wt.%.
  • the liquid in which the sewage sludge particles are suspended is wastewater, which preferably means all liquids of an aqueous and/or organic nature or mixtures thereof, which preferably do not have drinking water quality within the meaning of drinking water standards.
  • the biomass preferably contains, based on its dry weight, a Si content of at least 0.1 wt.%, in particular from 0.2 to 20 wt.%, preferably from 0.2 to 10 wt.%.
  • the preferred biomass used for pyrolysis is sewage sludge, alone or with other biomasses.
  • the biomass from which the biochar used in the process according to the invention is obtained contains a carbon content, expressed in wt.% of elemental carbon, of at least 1 wt.%, preferably at least 15 wt.%, in particular 15-50 wt.% carbon, based on the dry weight.
  • the biomass is used as so-called primary sludge, raw sludge, surplus sludge, as treated and/or stabilized sewage sludge (aerobic/anaerobic) or dried sewage sludge, also formed into pellets, for example, as it preferably arises in municipal sewage treatment plants.
  • the biomass used in the pyrolysis is a sewage sludge with a water content of ⁇ 15 wt.%, in particular ⁇ 12 wt.%, which contains the following inorganic constituents described as elements, based on the dry matter:
  • the chlorine gas can be brought into contact in various ways with the biochar or its mixture with another carbon source, preferably with a carbon content of greater than 20 wt.%, such as another biochar or with a bioash, preferably below 1 wt.%, particularly preferably below 0.1 wt.%.
  • chlorine is passed over or through the biochar, which may be in the form of the mixture described above, which is preferably moved during the reaction for effective conversion. This can be done in a rotary kiln or in a paddle dryer in which the biochar, which may be in the form of the mixture described above, is moved.
  • the chlorine gas can also be passed through the biochar, which may be in the form of the mixture described above, which can be achieved, for example, in a fluidized bed or fixed bed. If the addition of a further carbon source is a gaseous compound, the chlorine gas use described above is preferably carried out together with or separately from the gaseous carbon source for the biochar, which may be in the form of the mixture described above.
  • the residence time in the reactor during the reaction is generally dependent on the temperature and the possibility of contact between the material and chlorine gas.
  • the residence time in the reactor can vary for example, from one minute to 5 hours.
  • the process according to the invention can be operated as a batch or continuously.
  • the exhaust gas stream contains the gaseous reaction products, volatile components of the biochar at the chlorination temperature and possibly excess chlorine gas, which can be discharged together from the reaction chamber.
  • Iron(III) chloride and also AICI3 if the sewage sludge ash contains aluminum, can be separated from the exhaust gas stream and preferably by resublimation on surfaces of different temperatures. If the iron chloride is present together with AICI3 in the exhaust gas stream, the respective chlorides can also be fractionally resublimated on different surfaces with different temperatures due to sufficiently different boiling points and can thus be separated very cleanly.
  • the gaseous products PCI3, POCh and SiCL are condensed and collected in condensers.
  • Preferred deposition temperatures for FeCh are less than or equal to 307°C, in particular 150°C to 300°C, and for AICI3 less than or equal to 150°C, in particular 110°C to 149°C.
  • the invention further relates to the production of SiCL, characterized in that bioash is reacted with elemental chlorine in the presence of a carbon source at a temperature of 350 to 900°C and the SiCL formed is separated from the exhaust gas stream.
  • bioash and “carbon source” have the meaning given above, including the preferred ranges.
  • biomass in the context of this invention also means the combustion residue of a biomass or biochar, preferably with a carbon content of preferably less than 3% by weight, in particular less than 1% by weight, particularly preferably less than 0.1% by weight.
  • the preferred bioash is sewage sludge ash, i.e. the ash that comes from the combustion of sewage sludge. This can be obtained both from sewage sludge incineration and from sewage sludge gasification to produce a fuel gas.
  • sewage sludge ash preferably contains compounds of iron (Fe), aluminum (Al), calcium (Ca) and silicon (Si).
  • the sewage sludge ash used in the process according to the invention has a phosphorus content, expressed as percentage by weight of elemental phosphorus in the ash, of at least 3%, preferably from 3 to 29% by weight, in particular from 3 to 15% by weight.
  • the bioash used in the process according to the invention in particular sewage sludge ash, has a silicon content, expressed as weight percent of elemental silicon in the ash, of at least 1%, preferably from 3 to 30% by weight, in particular from 3 to 20% by weight.
  • the sewage sludge ash preferably contains a proportion of iron compounds of 5 to 21% by weight (calculated as elemental iron), and preferably a proportion of calcium compounds of 4 to 38% by weight (calculated as elemental calcium).
  • the preferred composition of a sewage sludge ash preferably also contains, calculated on the basis of the respective element:
  • Titanium from 0 to 2 wt.%.
  • the elements together, calculated as oxides, preferably make up more than 70 wt.% of the sewage sludge ash.
  • the exact structural composition of the sewage sludge ash cannot be determined using the usual analytical methods available to experts, such as X-ray diffraction (XRD), since the diffractogram only shows reflections for the SiO2 present.
  • XRD X-ray diffraction
  • the carbon content in the bioash, in particular in the sewage sludge ash is less than 3 wt.%, in particular less than 1 wt.%, particularly preferably less than 0.1 wt.%.
  • the sewage sludge contains a carbon content, expressed as % by weight of elemental carbon, of at least 5% by weight of carbon.
  • the liquid in which the particles of the sewage sludge are suspended is waste water as defined herein.
  • waste water is understood to mean all liquids of an aqueous and/or organic nature or mixtures thereof that do not have drinking water quality within the meaning of drinking water standards.
  • the sewage sludge is preferably present as primary sludge, raw sludge, excess sludge, as treated and/or stabilized sewage sludge (aerobic/anaerobic).
  • biowaste refers to all organic waste of animal or plant origin that is generated in a household or factory and can be broken down by microorganisms, soil-dwelling organisms or enzymes. Examples of such waste include straw, sawdust, waxes, fats and bird droppings.
  • the carbon source can be solid, liquid or gaseous. The use of a solid carbon source is preferred.
  • pyrolysis is preferably carried out before the reaction with chlorine gas. This is preferably carried out under inert gas such as nitrogen at temperatures of 250 to 800°C, preferably at 350 to 550°C until the gas formation of volatile components is less than 11/1 kg carbon source used / hour.
  • Sewage sludge is particularly preferred as a carbon source.
  • the chloride content in the carbon source is less than 1 wt.%.
  • the ratio of the weight proportions of the carbon of the carbon source to bioash, in particular to sewage sludge ash, is preferably greater than 0.01, preferably from 0.04 to 0.5.
  • the invention further relates to the use of biochar and/or bioash, in particular sewage sludge ash, for producing SiCU by chlorination in the presence of a carbon source.
  • biochar in particular sewage sludge ash
  • This may already contain the carbon source.
  • the chlorination is preferably carried out with elemental chlorine at a temperature of 350 to 900°C, the SiCU formed being separated from the exhaust gas stream, as preferably described above.
  • the stated weight percentages were determined by an ICP-OES measurement. To do this, a weighed amount of the solid is first dissolved in a known amount of an acid, the concentration of the stated elements is determined in an ICP against a calibration measurement and from this the solid is calculated as a proportion.
  • Carbon analyses were carried out using a special carbon analyzer type G4 ICARUS HF.
  • the analysis of phosphorus and silicon compounds, especially POCl3, PCh and SiCU in the liquid phase is preferably carried out using a GC method.
  • a WLD and an FID or a QMS are used as detectors.
  • An MPS from Gerstel is used as the injection system.
  • a GC-MS is also used and the mass spectra obtained are compared with those in databases.
  • the water content is determined using an infrared drying scale.
  • the biomass used is 8 kg of sewage sludge (obtained from the Wuppertal sewage treatment plant, in % by weight as respective elements):
  • Al 0.86, Ca: 0.98, Fe: 0.8, K: 0.09, Cu: 0.01, Mg: 0.14, Mn 0.01, P: 0.91, Si: 2.33, Zn: 0.03, S: 0.16 wt.% and other elements in trace amounts.
  • the sewage sludge with a water content of 77% is spread on stainless steel sheets and dried in a drying cabinet at up to 180°C for five days in a vacuum at 20 mbar. A crumbly sewage sludge with a water content of less than ⁇ 1% was obtained. b) Pyrolysis

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Processing Of Solid Wastes (AREA)
  • Treatment Of Sludge (AREA)

Abstract

L'invention concerne un procédé de récupération de silicium sous la forme de tétrachlorure de silicium, dans lequel du biocharbon ayant une teneur en silicium, exprimée en % en poids de silicium élémentaire, d'au moins 1% en poids est mis à réagir avec du chlore élémentaire à une température de 350 à 900°C et le tétrachlorure de silicium formé est séparé du flux de gaz d'échappement, de préférence par condensation.
PCT/EP2024/073697 2023-08-30 2024-08-23 Récupération de silicium sous forme de tétrachlorure de silicium à partir de biocharbon Pending WO2025045768A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
EP23194301.0 2023-08-30
EP23194301.0A EP4516733A1 (fr) 2023-08-30 2023-08-30 Récupération de phosphore sous forme de ses chlorures à partir de cendres de boues d'épuration
EP24194127.7A EP4516734A1 (fr) 2023-08-30 2024-08-12 Récupération de silicium sous forme de tétrachlorure de charbon biologique
EP24194127.7 2024-08-12

Publications (1)

Publication Number Publication Date
WO2025045768A1 true WO2025045768A1 (fr) 2025-03-06

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PCT/EP2024/073697 Pending WO2025045768A1 (fr) 2023-08-30 2024-08-23 Récupération de silicium sous forme de tétrachlorure de silicium à partir de biocharbon

Country Status (3)

Country Link
AR (1) AR133659A1 (fr)
TW (1) TW202515831A (fr)
WO (1) WO2025045768A1 (fr)

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2843458A (en) 1955-10-20 1958-07-15 Cabot Godfrey L Inc Process for producing silicon tetrachloride
EP0034897A1 (fr) 1980-02-13 1981-09-02 Ube Industries, Ltd. Procédé pour la production de chlorures d'éléments des groupes III, IV ou V du système périodique
US4288414A (en) * 1978-01-30 1981-09-08 Public Service Company Of New Mexico Process for chlorinating clays and bauxite
US4604272A (en) 1984-07-06 1986-08-05 Wacker-Chemie Gmbh Process for the preparation of silicon tetrachloride
US4695436A (en) * 1985-01-16 1987-09-22 Toth Aluminum Corporation Process for manufacturing high purity metal chlorides
EP2176177B1 (fr) 2007-07-05 2011-12-21 Seaborne EPM AG Procédé destiné à récupérer du phosphate à partir d'une biomasse
US20160130154A1 (en) * 2013-06-28 2016-05-12 Ecotec Risorse S.R.L. Process for the extraction, from bauxite, from red mud resulting from the processing of bauxite, and from chemically similar materials, of products of industrial interest, separated from each other
EP3285920A1 (fr) 2015-04-20 2018-02-28 Rainbow Bee Eater IP Pty Ltd. Appareil et procédé de pyrolyse
EP3061725B1 (fr) 2015-02-26 2018-06-20 TerraNova Energy GmbH Procédé de séparation du phosphore de la biomasse
EP3919586A1 (fr) 2020-06-04 2021-12-08 Schuster, Reimund Dispositif de fabrication de charbon végétal par pyrolyse de la biomasse
EP3984966A1 (fr) 2020-10-14 2022-04-20 Parforce Engineering & Consulting GmbH Procédé de traitement des boues brutes contenant du phosphore/phosphate et dispositif de traitement des boues brutes contenant du phosphore/phosphate
WO2023275271A1 (fr) 2021-06-30 2023-01-05 Schierbecker Handels GmbH & Co. KG Unité d'ensemencement comprenant du charbon végétal et un superabsorbant polymère

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2843458A (en) 1955-10-20 1958-07-15 Cabot Godfrey L Inc Process for producing silicon tetrachloride
US4288414A (en) * 1978-01-30 1981-09-08 Public Service Company Of New Mexico Process for chlorinating clays and bauxite
EP0034897A1 (fr) 1980-02-13 1981-09-02 Ube Industries, Ltd. Procédé pour la production de chlorures d'éléments des groupes III, IV ou V du système périodique
US4604272A (en) 1984-07-06 1986-08-05 Wacker-Chemie Gmbh Process for the preparation of silicon tetrachloride
EP0167156B1 (fr) * 1984-07-06 1991-02-27 Wacker-Chemie Gmbh Procédé de préparation de tétrachlorure de silicium
US4695436A (en) * 1985-01-16 1987-09-22 Toth Aluminum Corporation Process for manufacturing high purity metal chlorides
EP2176177B1 (fr) 2007-07-05 2011-12-21 Seaborne EPM AG Procédé destiné à récupérer du phosphate à partir d'une biomasse
US20160130154A1 (en) * 2013-06-28 2016-05-12 Ecotec Risorse S.R.L. Process for the extraction, from bauxite, from red mud resulting from the processing of bauxite, and from chemically similar materials, of products of industrial interest, separated from each other
EP3061725B1 (fr) 2015-02-26 2018-06-20 TerraNova Energy GmbH Procédé de séparation du phosphore de la biomasse
EP3285920A1 (fr) 2015-04-20 2018-02-28 Rainbow Bee Eater IP Pty Ltd. Appareil et procédé de pyrolyse
EP3919586A1 (fr) 2020-06-04 2021-12-08 Schuster, Reimund Dispositif de fabrication de charbon végétal par pyrolyse de la biomasse
EP3984966A1 (fr) 2020-10-14 2022-04-20 Parforce Engineering & Consulting GmbH Procédé de traitement des boues brutes contenant du phosphore/phosphate et dispositif de traitement des boues brutes contenant du phosphore/phosphate
WO2023275271A1 (fr) 2021-06-30 2023-01-05 Schierbecker Handels GmbH & Co. KG Unité d'ensemencement comprenant du charbon végétal et un superabsorbant polymère

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Title
CHEN JEN-MIN ET AL: "KINETICS AND CATALYSIS The Chlorination Kinetics of Rice Husk", 1 January 1991 (1991-01-01), XP093219364, Retrieved from the Internet <URL:https://pubs.acs.org/doi/abs/10.1021/ie00058a001> *
MOCHIZUKI YUUKI ET AL: "Production of Silicone Tetrachloride from Rice Husk by Chlorination and Performance of Mercury Adsorption from Aqueous Solution of the Chlorinated Residue", ACS OMEGA, vol. 5, no. 45, 2 November 2020 (2020-11-02), US, pages 29110 - 29120, XP055913394, ISSN: 2470-1343, Retrieved from the Internet <URL:http://pubs.acs.org/doi/pdf/10.1021/acsomega.0c03789> DOI: 10.1021/acsomega.0c03789 *
SEO E.S.M ET AL: "Silicon tetrachloride production by chlorination method using rice husk as raw material", JOURNAL OF MATERIALS PROCESSING TECHNOLOGY, vol. 141, no. 3, 1 November 2003 (2003-11-01), NL, pages 351 - 356, XP093219286, ISSN: 0924-0136, Retrieved from the Internet <URL:https://pdf.sciencedirectassets.com/271356/1-s2.0-S0924013600X02026/1-s2.0-S0924013603002875/main.pdf?X-Amz-Security-Token=IQoJb3JpZ2luX2VjEOr//////////wEaCXVzLWVhc3QtMSJGMEQCIHpuQPGzHVnHEAh/AcSIAwgK5hjEu1mG2deGBT7uP15iAiAcyaoA5CcVh5o6hbIAhqGQOZdRx66HPYX7hZa4K4h3hSqyBQhjEAUaDDA1OTAwMzU0Njg2NSIMKctxl> DOI: 10.1016/S0924-0136(03)00287-5 *
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