Method for the treatment of organic waste

EP4594264A1Pending Publication Date: 2025-08-06SUEZ INTERNATIONAL
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Patent Information

Application Number
EP2023782535
Authority / Receiving Office
EP · EP
Patent Type
Applications
Current Assignee / Owner
Priority Date
2022-09-29
Filing Date
2023-09-28
Publication Date
2025-08-06

AI Technical Summary

Technical Problem

Hydrothermal treatments of biomass face challenges in controlling temperature and residence time, leading to unwanted reactions and significant thermal gradients due to low thermal conductivity and non-homogeneous biomass, resulting in the formation of unwanted compounds like oils and tars.

Method used

A process involving pressurization, controlled heating, mechanical shock injection, and vertical injection of supercritical water into a hydrotreatment reactor with a baffling system and filtration to separate residence times and enhance heat exchange, minimizing the formation of unwanted compounds.

Benefits of technology

This process allows for better heat exchange, reduced formation of unwanted compounds, and controlled process conditions, optimizing the treatment of biomass by ensuring uniform reaction kinetics and minimizing thermal consumption.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to a method for hydrotreating a mixture M1 comprising at least organic matter, the method comprising: a) pressurising the mixture M1 comprising at least organic matter in order to obtain a mixed stream M1p; b) a step of heating the mixture making it possible to obtain a mixed stream M2; c) introducing the stream M2 via an inlet E1 into a hydrotreatment reactor by injection facing an impact plate in order to create a mechanical impact; d) a step of vertically injecting water ES1 at a temperature of at least 374°C directly into the hydrotreatment reactor via an inlet E2; and e) recovering a stream M3 enriched with soluble materials and a stream M4 depleted of soluble materials, the stream M4 being recovered by an outlet S2 of the reactor, the outlet S2 and the inlet E2 each being located at an altitude lower than the inlet E1.
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Description

ORGANIC WASTE TREATMENT PROCESS TECHNICAL FIELD OF THE INVENTION

[0001] The invention relates to the field of biomass treatment, in particular sludge from sewage treatment plants, food and agri-food waste, manure digestates and agricultural residues. STATE OF THE ART

[0002] Hydrothermal treatments for biomass are becoming increasingly common. They require high temperatures. It is therefore essential to control temperatures in order to obtain the desired quality of hydrotreated biomass.

[0003] Thus, controlling the temperatures and residence times of the process is extremely important to achieve the desired result. Temperatures that are too high or too low, residence times that are too short or too long either do not allow the desired reactions to occur or lead to unwanted side reactions that result in an overall degradation of the desired performance or, worse, in the production of a residue whose treatment costs will be significant.

[0004] In particular, the heating stage of hydrothermal treatments is a major cause of these side reactions due to the long residence time at intermediate temperatures which can lead to the formation of unwanted compounds such as oils, tars or derivatives close to coal. This heating stage is all the longer as the temperatures to be reached are high, in particular when the temperatures to be reached are close to or higher than the temperature of supercritical water.

[0005] Furthermore, in the state of the art, heating is often carried out via a “tube in tube” type exchanger to recover the output heat in order to reduce the quantity of heat required for the process. However, in this type of exchanger, the low thermal conduction of the product to be heated leads to a very significant temperature variation inside the product and therefore different process conditions between the different parts of the product leading to unwanted parasitic reactions.

[0006] Finally, since biomass is not homogeneous, chemical reactions do not occur with identical kinetics throughout the biomass, particularly when it contains massive particles, part of the mass of which is not in direct contact with water.

[0007] There is therefore a need to provide a process for hydrotreating a mixture, such as biomass, allowing better heat exchanges and less formation of unwanted compounds such as oils, tars or derivatives close to coal.

[0008] The invention relates to a process for hydrotreating a mixture M1 comprising at least organic matter, said process comprising:

[0009] a) pressurizing the mixture M1 comprising at least organic matter to a pressure ranging from 20 to 350 bars, in order to obtain a flow of mixture M1p,

[0010] b) a step of heating the mixture M1p to a temperature ranging from 170 to 430°C, making it possible to obtain a flow of mixture M2,

[0011] c) an introduction of the flow M2 through an inlet E1 into a hydrotreatment reactor by an injection facing an impact plate in order to create a mechanical shock,

[0012] d) a vertical injection step of water ES1 at a temperature of at least 374°C directly into the hydrotreatment reactor via an inlet E2,

[0013] e) recovery of a flow M3 enriched in soluble materials and a flow M4 depleted in soluble materials, the recovery of the flow M4 being implemented by an outlet S2 of the reactor,

[0014] exit S2 and entrance E2 each being located at a lower altitude than entrance E1.

[0015] Preferably, the recovery of the M3 stream enriched in soluble materials during step e) is carried out through at least one filter, said filter comprising at least one filtration layer preferably having a mesh size of less than 100 µm, preferably less than 50 µm, more preferably less than 40 µm, said filter preferably being in the hydrotreatment reactor.

[0016] Preferably, step b) comprises at least one step of injecting water ES at a temperature of at least 374°C into the flow of mixture M1p in order to obtain the flow M2, the injected water preferably being at a pressure of at least 225 bars.

[0017] According to one embodiment, the recovery of the M3 stream during step e) is controlled by determining the pressure difference between the pressure in the hydrotreatment reactor and the pressure in the M3 stream at the outlet of the reactor downstream of the filter.

[0018] According to one embodiment, the hydrotreatment reactor is maintained at a temperature ranging from 150°C to a temperature below 374°C.

[0019] Preferably, the method further comprises, downstream of the filter and downstream of the reactor, a step f) of injecting water at a temperature of at least 374°C into the flow M3, counter-current to said flow, where appropriate said water preferably being at the same temperature and at the same pressure as the water injected during step b).

[0020] Preferably, when the countercurrent water injection of step f) is implemented, then the outlet S2 of the reactor is opened in order to extract a stream M4.

[0021] According to one embodiment, the hydrotreatment reactor further comprises a baffle system making it possible to guide the upward flow created by the vertical injection of water ES1 before extraction of the flow M3 during step e) through an upper part of the reactor, preferably through a filter.

[0022] According to one embodiment, the method further comprises; at least one heat exchange step X1 making it possible to recover heat from the flow M3 to at least partially heat the water intended to be injected for the heating step b), a cooled flow M5' then being obtained, and optionally comprising at least one additional water heating step, downstream of the heat exchange X1 making it possible to heat the water to the temperature of at least 374°C before its injection in step d) and / or where appropriate before its injection in step b) and / or where appropriate before its injection in step f), and optionally at least one heat exchange step X2 making it possible to recover heat from the flow M5' to heat the mixture M1p upstream of the water injection of step b), a flow M5'' then being obtained.

[0023] Preferably, the method further comprises:at least one step of cooling at least a fraction of the stream M5' or, where appropriate, the stream M5'' making it possible to obtain steam and a stream M6 comprising hydrotreated organic matter, anda step of injecting at least a portion of said steam to preheat the mixture M1 upstream of step a) of pressurizing, said mixture M1 preferably being preheated to a temperature ranging from 50 to 170°C, preferably from 50 to 90°C,optionally a step of cooling at least a fraction of the stream M6 to obtain a cooled stream M6' and optionally a step of digesting the stream M6'.

[0024] According to one embodiment, the impact plate has an extra thickness which resists erosion.

[0025] The invention also relates to an installation for implementing the hydrotreatment process according to the invention, said installation comprising: a mixture supply line M1, a pressurizing pump 2 supplied by the mixture supply line M1 and comprising a mixture outlet line M1p, a heating device 11 supplied with at least a fraction of the mixture M1p downstream of the pump 2 and having an outlet for the mixture flow M2, downstream of the heating device, a hydrotreatment reactor 1 comprising an inlet E1 for injecting the flow M2, an inlet E2 for injecting water ES1, an outlet S1 for extracting a flow M3 and an outlet S2 for extracting a flow M4, said reactor further comprising at least one impact plate located opposite the inlet E1 in order to create a mechanical shock during the injection of the flow M2 into the reactor,a water injection device ES1 directly into the reactor allowing vertical injection from bottom to top via inlet E2 of reactor 1,

[0026] exit S2 and entrance E2 each being located at a lower altitude than entrance E1.

[0027] Preferably, the hydrotreatment reactor 1 further comprises: at least one first filter F1, said first filter being arranged in such a way that the flow M3 enriched in soluble matter passes through the filter before leaving the reactor via the outlet S1, and optionally at least one second filter F1', said second filter F1' being arranged in such a way that the flow M3' enriched in soluble matter passes through said second filter F1' before leaving the reactor 1 via an outlet S1',

[0028] preferably, the outlets S1 and S1' are located in the upper part of the hydrotreatment reactor 1 and preferably allow vertical extraction, from the bottom to the top of the flows M3 and M3' respectively.

[0029] Preferably, the hydrotreatment reactor 1 further comprises a baffle system making it possible to guide the upward flow created by the vertical injection of water via the inlet E2 before its extraction via the outlet S1, the outlet S1 preferably being in the upper part of the reactor, allowing a vertical outlet from the bottom to the top.

[0030] Preferably, the heating device 11 comprises at least one water injection device ES in the mixing line M1p, said installation further preferably comprising: a heat exchanger 6 downstream of the hydrotreatment reactor 1, said heat exchanger making it possible to recover the heat in the flow line M3, possibly combined with the flow line M3', to obtain a flow M5' and to transfer this heat to the water upstream of the water injection device ES1 and / or upstream of the water injection device ES, and optionally a water heating device 7, downstream of the heat exchanger 6 and upstream of the water injection device ES and upstream of the water injection device ES1, said heating device 7 advantageously comprising at least two outlet lines, one line connected to the water injection device ES1 and one line connected to the water injection device ES,

[0031] said installation preferably further comprising: optionally a heat exchanger 8 making it possible to recover heat from the mixture M5' to obtain a mixture M5'' and to transfer this heat to the mixture M1p upstream of the water injection device ES, A cooling device 4 supplied by at least a fraction of the flow M5' or where appropriate M5'' making it possible to produce steam and a cooled flow M6, An injection device 3 of said steam produced into the mixture flow M1 upstream of the pressurization pump 2, optionally a cooling device 9 downstream of the cooling device 4 supplied by at least a fraction of the flow M6 making it possible to cool at least a fraction of the flow M6 to obtain a flow M6', and optionally a digester 5 supplied by the flow M6'.

[0032] The invention makes it possible, as a priority, to separate the residence times between the massive particles constituting the biomass and for which the chemical reaction times (in particular solubilization) must be longer and the solubilized molecules which must be removed more quickly from the reactor to avoid secondary reactions, for example repolymerization.

[0033] The invention also allows the biomass to be heated very quickly by direct heating, which subsequently allows the desired process conditions to be controlled.

[0034] The invention makes it possible to maintain the thermal recovery of the process by heating the water in supercritical conditions in order to minimize the overall thermal consumption of the process.

[0035] Biomass has a certain viscosity. However, viscosity makes heat exchange difficult. Since water has a lower viscosity than any other biomass, heating the water will result in a smaller recovery exchanger and therefore a lower cost.

[0036] The invention proposes injecting supercritical water directly into the flow of organic matter M1. Thus, the thermal shock between the organic matter (M1), part of which is cellular content, and the very hot supercritical water will cause local cavitations due to the difference in local density and therefore local pressure. These cavitations allow immediate release of the cellular content into the aqueous matrix and therefore, subsequently, in the hydrotreatment reactor, immediate reactions of the proteins and sugars contained in the bacteria.

[0037] The invention also makes it possible to initiate, by means of an impact plate at the reactor inlet, a maximum separation of the particle size by making it possible to pulverize, i.e. to transform into small particles, an element made up of larger particles. BRIEF DESCRIPTION OF THE FIGURES

[0038] represents an installation according to an embodiment of the method according to the invention.

[0039] represents an installation according to an embodiment of the method according to the invention.

[0040] represents an installation according to an embodiment of the method according to the invention.

[0041] represents an installation according to an embodiment of the method according to the invention.

[0042] represents an installation according to an embodiment of the method according to the invention.

[0043] represents an installation according to an embodiment of the method according to the invention. DETAILED DESCRIPTION OF THE INVENTION

[0044] The invention relates to the hydrothermal treatment of a mixture M1 comprising organic matter.

[0045] Mixture M1 is typically a biomass. Biomass can be pasty or liquid, and can include sewage sludge, food and agri-food waste, and especially manure digestate and agricultural residues.

[0046] The invention relates to a process for hydrotreating a mixture M1 comprising at least organic matter, said process comprising:

[0047] a) pressurizing the mixture M1 comprising at least organic matter to a pressure ranging from 20 to 350 bars in order to obtain a flow of mixture M1p preferably having a pressure of at least 40 bars,

[0048] b) a step of heating the mixture M1p to a temperature ranging from 170 to 430°C, preferably from 250 to 350°C, making it possible to obtain a flow of mixture M2,

[0049] c) an introduction of the M2 flow into a hydrotreatment reactor by an injection facing an impact plate in order to create a mechanical shock,

[0050] d) a vertical injection step of ES1 water at a temperature of at least 374°C directly into the hydrotreatment reactor in the lower part of said reactor,

[0051] e) recovery of an M3 stream enriched in soluble materials and an M4 stream depleted in soluble materials, the recovery of the M4 stream being carried out in the lower part of said reactor.

[0052] For the purposes of the present invention, the expression "at least a fraction of a mixture or stream" has the same meaning as the expression "all or part of said mixture or stream". When referring to a part of said mixture or stream, this expression refers to a certain proportion of said mixture or stream. For example, for the purposes of this expression "each fraction of the mixture" or "each fraction of the stream" will have the same composition.

[0053] For the purposes of the present invention, the expression "where appropriate of step X" introduces a characteristic present when step X is present.

[0054] For the purposes of the present invention, the expression “where applicable of the flow X” introduces a characteristic present when the flow X is present. Pressurization step a)

[0055] The method according to the invention comprises a step of pressurizing the mixture M1 preferably to a pressure ranging from 20 to 350 bars, preferably from 50 to 300 bars, preferably from 150 to 270 bars, preferably from 170 to 220 bars, said mixture M1 possibly already being under pressure before step a).

[0056] In particular, pressurization allows mixture M1 to be brought to a pressure sufficient for the mixture to be in a predominantly liquid phase. More specifically, the pressure in mixture M3 will typically be greater than the saturated vapor pressure of said mixture M3 to maintain the water in the liquid phase.

[0057] For the pressurization step, a pump can be provided on the M1 mixing line.

[0058] Downstream of the pressurization, a flow of M1p mixture is obtained. Heating step b)

[0059] The method of the invention comprises a step of heating the mixture M1p to a temperature ranging from 170 to 430°C, preferably from 250 to 350°C, making it possible to obtain a flow of mixture M2.

[0060] This heating can be implemented in one or more stages. A sub-stage can be heating by an external heat flow (electric heating, heat exchanger by a hot fluid (gas / liquid), microwave, etc.) or water injection.

[0061] Thus, according to a preferred embodiment, the heating step b) comprises at least one step during which water ES at a temperature of at least 374°C is injected into the mixture stream M1p in order to obtain a mixture stream M2 comprising water and organic matter. The mixture M2 will typically also comprise inorganic matter.

[0062] Water injection can, for example, be implemented at an angle ranging from 15° to 90°, preferably from 45 to 90°, or even from 45 to 75°, relative to the flow arrival line M1p.

[0063] According to one embodiment, the mixture M1p during the water injection of step b) is at a temperature ranging from 90°C to 300°C. In this case, the heating step b) may optionally comprise a sub-step of heating by an external heat flow (electric heating, heat exchanger by a hot fluid (gas / liquid), microwave, etc.).

[0064] Upstream of the water injection implemented in step b), the injected water will typically be at a pressure higher than the pressure of the mixture M1p.

[0065] According to a preferred embodiment of the invention, the water injected in step b) is at a pressure of at least 225 bars. According to this embodiment, the injected water will then be called “supercritical water”.

[0066] According to one embodiment, the heating step b) of the method comprises two sub-steps: a first sub-step of heat exchange between the flow M1p and flow M3, said flow M3 having optionally been subjected to one or more heat exchanges between the outlet of the reactor and this heat exchange with M1p, a second sub-step of injection of ES water at a temperature of at least 374°C and preferably at a pressure of at least 225 bars, in the flow line M1p downstream of the first sub-step.

[0067] According to one embodiment, the method of the invention comprises at least one step of heating the water making it possible to obtain water at a temperature of at least 374°C upstream of its injection in step b).

[0068] According to one embodiment, the method according to the invention comprises a step of pressurizing the water to a pressure of at least 225 bars followed by at least one step of heating the water to obtain water at a temperature of at least 374°C upstream of its injection in step b).

[0069] Preferably, at least one water heating step is implemented by heat exchange with the heat of at least a fraction of the M3 stream enriched in soluble matter leaving the hydrotreatment reactor, the stream thus cooled will be called M3' stream at the end of this heat exchange (it could be the heat exchange step X1 described below).

[0070] At the outlet of the injection between water and mud M1p, a static turbulator (e.g. chosen from propeller, blades, pipe bends, or combinations thereof) can also be introduced to increase turbulence and rapid heat exchange between mud and water and prevent mud and water from remaining in separate flows (to avoid laminar hydraulic lines).

[0071] Thus, according to one embodiment of the invention, upstream of step c), the mixture M2 is introduced into a static turbulator, said static turbulator then being located upstream or at the inlet of the hydrotreatment reactor.

[0072] According to one embodiment, a static turbulator is present upstream or at the inlet of the hydrotreatment reactor in order to increase the turbulence in the mixture M2.

[0073] According to a particular embodiment, the flow line M2, downstream of the water injection when it is present, comprises one or more pipe bends upstream of the hydrotreatment reactor. M2 flow introduction step c)

[0074] The method according to the invention comprises a step of introducing the flow M2 into a hydrotreatment reactor. The hydrotreatment reactor typically comprises an inlet E1 for introducing the flow M2, and the reactor comprises at least one impact plate facing said inlet E1. This impact plate thus makes it possible, when introducing the flow M2 via the inlet E1, to create a mechanical shock within the flow M2.

[0075] According to one embodiment, the impact plate is a siphon partition, meaning that the flow can then pass over and under the plate.

[0076] The mechanical shock resulting from the introduction of the M2 flow will modify the direction of the flow of the M2 flow and thus the speed of the particles suspended without being dissolved in this fluid according to their densities which will allow the separation of the undissolved particles (solids), thus leading to a phenomenon of decantation towards the bottom of the reactor of the non-hydrotreated solid matter (flow depleted in soluble matters) while the low density hydrotreated matter (flow enriched in soluble matters) will move towards the top of the reactor.

[0077] The hydrotreatment reactor is advantageously maintained at a temperature ranging from 150°C to 430°C. For example, this temperature maintenance can be carried out via a peripheral heat exchange with a hot fluid, the implementation of the equipment inside a furnace maintained at temperature, the implementation of an electric heating collar.

[0078] According to one embodiment, the impact plate has an extra thickness to protect it over time from erosion created by the impact.

[0079] According to one embodiment, the inlet diameter into the reactor allows an introduction speed greater than 3 m / s, preferably greater than 6 m / s, preferably greater than 10 m / s.

[0080] In the context of the process of the invention, control of the flow rates of the injected water, preferably supercritical water, and of the M1p mixture is advantageously implemented and will typically allow the new mixture (mixture called M2) to have a residence time in the hydrotreatment reactor ranging from 1 minute to 30 minutes, preferably 10 minutes to 15 minutes. Vertical water injection stage d)

[0081] The method according to the invention comprises a step d) of vertical injection (with respect to gravity) of water at a temperature of at least 374°C directly into the hydrotreatment reactor, from bottom to top. Preferably, the water injected in step d) is at a pressure of at least 225 bars. According to this embodiment, the injected water will then be called “supercritical water”.

[0082] This water injection step will thus contribute to maintaining the temperature of the hydrotreatment reactor.

[0083] Preferably, the hydrotreatment reactor also comprises within it (in its volume) a baffle system making it possible to guide the upward flow created by the vertical injection of water during step d), before the recovery of the flow(s) enriched in soluble matter downstream of the reactor during step e).

[0084] This baffle system can consist of plates that guide the upward flow towards the top of the reactor and then towards the bottom of the reactor; the latter guide preferably stopping at an altitude lower than that of the filter. The soluble matter at the end of this baffle system can then be sucked up by the filter present in the reactor while the solid (non-soluble) matter will return to the bottom of the reactor.

[0085] Said plates can be of different lengths and are at different altitudes to allow the desired guidance inside the reactor.

[0086] This system of injecting water into the lower part of the reactor makes it possible to extend the residence time of insoluble or slightly soluble materials (solids), so as not to evacuate them immediately from the reactor.

[0087] When the water injection system is coupled with a baffle system, this allows the residence time to be extended further in order to improve solubilization in the hydrotreatment reactor. This baffle system also prevents poorly or insoluble matter from sticking to the filter and blocking it.

[0088] According to one embodiment, the method of the invention comprises at least one step of heating the water making it possible to obtain water at a temperature of at least 374°C upstream of its injection in step d).

[0089] According to one embodiment, the method according to the invention comprises a step of pressurizing the water to a pressure of at least 225 bars followed by at least one step of heating the water to obtain water at a temperature of at least 374°C upstream of its injection in step d).

[0090] Preferably, at least one water heating step is implemented by heat exchange with the heat of at least a fraction of the M3 stream enriched in soluble matter leaving the hydrotreatment reactor, the stream thus cooled will be called M3' stream at the end of this heat exchange (it could be the heat exchange step X1 described below).

[0091] Step of recovering an M3 flow and an M4 flow e)

[0092] Downstream of the hydrotreatment reactor, an M3 stream enriched in soluble matter and an M4 stream depleted in soluble matter are recovered.

[0093] The flow depleted in soluble matter M4 is extracted from the reactor in the lower part of said reactor.

[0094] The M3 stream may be recovered downstream of one or more filters, said filter(s) being able to be present in the reactor and / or downstream of the reactor on the M3 stream line.

[0095] According to an advantageous embodiment of the invention, the recovery of the M3 stream enriched in soluble materials during step e) is carried out through at least one filter, preferably said at least one filter is present in the hydrotreatment reactor.

[0096] When the filter is present in the hydrotreatment reactor, this makes it possible to increase the filtering surface area and to have filters with a larger specific surface area, particularly in comparison with a filter present in the piping.

[0097] Additionally, when the filter is outside the hydrotreating reactor, it can be either in the piping or in another reactor downstream of the hydrotreating reactor, but in both cases the filter will clog faster than when the filter is in the hydrotreating reactor.

[0098] The filter limits the size of solid particles in the flow of hydrotreated organic matter M3, also called flow enriched in soluble matter.

[0099] The filter may comprise one or more filtration layers, which may optionally have different mesh sizes, preferably the external filtration layers have mesh sizes larger than the internal filtration layers.

[0100] According to one embodiment, the filter has a mesh size of less than 100 µm, preferably less than 50 µm, more preferably less than 40 µm. When the filter comprises several filtration layers, then the finest mesh will preferably have a size of less than 100 µm, preferably less than 50 µm, more preferably less than 40 µm.

[0101] According to a particular embodiment, a second filter is present in the hydrotreatment reactor or downstream of the hydrotreatment reactor on a flow outlet line M3' separate from the flow line M3. Thus, the second filter is configured such that material enriched in soluble materials is extracted from the reactor via this second filter. This second flow extracted via the second filter will be called M3'. The second filter will allow hydrotreated material (enriched in soluble materials) to be extracted when the first filter is saturated and while the first filter is being cleaned. Once the first filter is cleaned, it will resume its filtration role. This second outlet of material enriched in soluble materials will thus advantageously be open during the backflush period implemented on the first filter.

[0102] Advantageously according to this embodiment, the second filter will have a mesh size different from that of the first filter (filter allowing the extraction of the M3 flow), preferably a mesh size larger than that of the first filter.

[0103] Thus, according to this embodiment, the second filter will preferably have a mesh size of less than 200 µm, preferably less than 100 µm.

[0104] According to a particular embodiment, the first filter has a mesh size less than 40 µm and the second filter has a mesh size less than 100 µm.

[0105] This second filter may also comprise one or more filtration layers which may optionally have mesh sizes of different sizes, preferably the external filtration layers have mesh sizes larger than the internal filtration layers. When the second filter comprises several filtration layers, then preferably the finest mesh has a size of less than 200 µm, preferably less than 100 µm.

[0106] According to one embodiment, the recovery of the M3 stream during step e) is controlled by determining the pressure difference between the pressure in the hydrotreatment reactor and the pressure in the M3 stream at the outlet of the reactor downstream of the filter. According to one embodiment, the recovery of the M3 stream is carried out, typically by opening a valve V1 on the M3 stream line downstream of the filter, as long as the pressure difference is less than a predetermined threshold value, for example when the pressure difference is less than 10 bars.

[0107] This pressure difference check ensures that the filter is not excessively clogged.

[0108] According to one embodiment, the extraction of the M3 stream is carried out in the upper part of the hydrotreatment reactor, by a vertical outlet line (with respect to gravity). Thus, according to this embodiment, the stream enriched in soluble materials M3 is preferably extracted from the reactor by a stream circulating from the bottom to the top (with respect to gravity).

[0109] Preferably, the hydrotreatment reactor thus comprises at least one outlet in the upper part, at least a second outlet in the lower part, and possibly at least a third outlet located in the upper part.

[0110] For the purposes of the present invention, the expression "lower part" is opposed to the expression "upper part". Thus, an exit in the upper part will be located at a higher altitude than the exit in the lower part. Similarly, an exit in the upper part will be located at a higher altitude than an entrance in the lower part.

[0111] The method of the invention thus comprises an introduction of a flow M2, an extraction of a flow M3 and an extraction of a flow M4. Preferably, the inlet of mixture M2 is via an inlet E1 of the hydrotreatment reactor, the outlet of flow M3 is via an outlet S1 and the outlet of flow M4 is via an outlet S2.

[0112] Thus, according to an advantageous embodiment, the inlet E1 is located at a lower altitude than the outlet S1 and the inlet E1 is located at a higher altitude than the outlet S2 to extract the flow M4.

[0113] When a second filter is present, a flow M3' is extracted from the reactor via a third outlet S1', distinct from outlets S1 and S2. Thus, preferably, according to this embodiment, outlet S1' is located at an altitude higher than inlet E1, inlet E1 itself being at an altitude higher than outlet S2. Preferably, outlets S1 and S1' are at similar or even identical altitudes.

[0114] All of these configurations (E1, S1, S2 and where applicable S1') thus make it possible to optimize residence times and promote the solubilization of the material in the reactor. Other steps

[0115] According to one embodiment, the method further comprises a step f) during which water ES2 at a temperature of at least 374°C is injected into the flow line M3 leaving the hydrotreatment reactor downstream of the filter, preferably said water is at a pressure of at least 225 bars, more preferably said water injected ES2 into the flow line M3 is at the same temperature and at the same pressure as the water injected ES1 into the reactor in step d) and / or said water injected ES2 into the flow line M3 is, where appropriate (i.e. when step b) comprises an injection of water ES) at the same temperature and at the same pressure as the water injected into the flow M1p during step b).

[0116] Thus, this injection of water ES2, preferably supercritical water, is implemented counter-currently to the flow M3 leaving the hydrotreatment reactor. According to one embodiment, this water injected into the flow line M3 counter-currently is obtained by the same method as that described for the water injected in step d) and / or where appropriate in step b) (advantageously heat exchange X1 then additional heating).

[0117] Typically, during this countercurrent water injection into the M3 stream, the M3 stream is no longer extracted from the hydrotreatment reactor, typically by closing a valve V1 present downstream of the hydrotreatment reactor and downstream of the filter on the M3 stream outlet line. The ES2 water injection then typically takes place between the filter and the valve V1.

[0118] This injection of water into the M3 stream allows a backflush of the first filter to be carried out. This washing step can be activated at the same time as the recovery of the M4 stream via the lower outlet of the reactor, for example by opening a valve V2 on the M4 stream line. Thus, this countercurrent water injection can be triggered when the pressure difference between the pressure in the hydrotreatment reactor and the pressure in the M3 stream at the reactor outlet exceeds a certain predetermined threshold, for example from 10 bars.

[0119] According to one embodiment of the method of the invention, when a counter-current injection of water ES2, preferably supercritical water, is implemented in the flow M3, then preferably the outlet of the reactor in the lower part is opened (during said water injection), via the opening of a valve V2 downstream of the hydrotreatment reactor on the flow line M4, in order to extract a flow M4 depleted in soluble matter.

[0120] For the purposes of the present invention, the term “flow enriched in soluble materials” means a flow comprising a mass proportion of soluble materials greater than the mass proportion of soluble materials in the mixture M2.

[0121] For the purposes of the present invention, the term “flow depleted in soluble materials” means a flow comprising a mass proportion of soluble materials lower than the mass proportion of soluble materials in the mixture M2.

[0122] For the purposes of the present invention, a soluble material will be a material obtained after filtration in a 40 µm filter (material not retained by said 40 µm filter) then drying of an initial material.

[0123] Thus, according to one embodiment, the ratio between the concentration of soluble materials of the flow M3 and the concentration of soluble materials of the flow M4 is at least 2, preferably at least 4, more preferably at least 6, or even at least 10.

[0124] According to an embodiment implementing a second filter, during backwashing of the first filter, the flow outlet M3 is closed (for example by means of a valve V1) and it is possible for a flow M3' enriched in soluble matter to be extracted from the reactor via the second filter during said backwashing of the first filter.

[0125] Preferably, each of the flow outlets M3 and M3' is located in the upper part of the reactor, in order to allow a vertical outlet of the flow, from bottom to top.

[0126] Thus, according to this embodiment, a first valve V1 is present on the flow outlet M3 and a second valve V1' is present on the flow outlet M3'. Preferably according to this embodiment, when the first valve V1 is open, then either the second valve V1' is open or the valve V2 is open or both valves V1' and V2 are open.

[0127] According to the embodiment implementing two filters, said filters can be (i) in the hydrotreatment reactor or (ii) downstream of the hydrotreatment reactor or (iii) one of the two filters can be in the reactor and the other filter can be downstream of the reactor. According to this embodiment, two streams enriched in soluble matter M3 and M3' are then obtained downstream of the hydrotreatment reactor and downstream of said filters. Advantageously, the two stream lines M3 and M3' are combined, typically downstream of the valves V1 and V1'.

[0128] According to a particularly advantageous embodiment, the method of the invention further comprises at least one heat exchange step X1 making it possible to recover heat from the flow M3, possibly combined with the flow M3' to at least partially heat the water W1 intended to be injected in step d) and intended to be injected where appropriate for the heating step b). Downstream of the heat exchange X1, the flow M3 (possibly combined with the flow M3') which will have been cooled will be called flow M5' and the water W1 which will have been heated will be called water W2.

[0129] Typically, according to this embodiment, the method of the invention further comprises at least one step of heating the water W2, downstream of said heat exchange X1, making it possible to heat the water to a temperature of at least 374°C before its injection in step d), and where appropriate in step b).

[0130] When the method of the invention comprises a heat exchange step X1, said heat exchange step X1 is preferably carried out with water having a pressure of at least 225 bars, it will thus preferably be carried out after a step of pressurizing the water W1 to a pressure of at least 225 bars.

[0131] Preferably, according to the embodiment implementing two filters, the heat exchange X1 is implemented downstream of the recombination of the flow lines M3 and M3'.

[0132] According to one embodiment, the method of the invention further comprises a heat exchange step X2 making it possible to recover heat from the flow M5' to heat the mixture M1p (preferably upstream of the injection of water ES) during step b) of the method. This heat exchange then makes it possible to obtain a cooled flow M5''.

[0133] The M1p flow downstream of the X2 heat exchange could typically have a temperature ranging from 90 to 170°C.

[0134] Said heat exchange step X2 may be combined with another external heating step to heat the mixture M1p to the desired temperature when implementing step b), this may in particular involve heating by injecting water to a temperature of at least 374°C.

[0135] The M5'' flux can typically have a temperature ranging from 100 to 200°C.

[0136] Preferably, according to this embodiment, the hydrotreatment process according to the invention further comprises: a step of cooling at least a fraction of the stream M5'' making it possible to obtain steam and a stream M6 enriched in soluble materials, and a step of injecting at least a portion of said steam to preheat the mixture M1 upstream of step a) of pressurizing.

[0137] The cooling step can be implemented using a cooling device chosen from a heat exchanger integrated or not in a rankine, flash, scrubber cycle, preferably using a flash.

[0138] The steam produced during cooling is, according to this embodiment, used to preheat the mixture M1 upstream of step a) of pressurizing.

[0139] Preferably, according to this embodiment, the mixture M1 is preheated upstream of the pressurization step a) to a temperature ranging from 50 to 170°C, preferably from 50 to 90°C, using the steam resulting from the cooling of at least a fraction of the flow M5''. It should be noted that the mixture M1 may possibly already be under pressure, before step a) defined in the invention.

[0140] The invention thus allows for better optimization of the viscosity of the biomass undergoing high-pressure treatments. Indeed, the difficulty of pumping at these high pressures requires a minimum viscosity of the biomass to be pumped in order to meet the specifications of very high-pressure pumps.

[0141] By injecting steam into the M1 mixture, all possibilities are used to reduce the viscosity of the biomass to an acceptable value for pumping technologies while minimizing the dilution of the biomass which can cause additional costs in the sizing of downstream equipment (residence time to be respected, etc.).

[0142] According to one embodiment, the cooling of at least a fraction of the flow M5' or where appropriate M5'' is carried out at a pressure regulated as a function of the preheating temperature of the mixture M1 upstream of the pressurization step a).

[0143] Indeed, pressure and temperature are linked for saturated steam. Maintaining a constant pressure makes it possible to control the temperature of the steam and therefore the maximum temperature that can be reached by the product heated by the steam (mixture M1 in the case of the invention).

[0144] For example, the pressure can be maintained between 2 and 10 bars.

[0145] According to one embodiment, the method according to the invention further comprises an additional step of cooling at least a fraction of the M6 ​​stream (enriched in soluble matter) to obtain a M6' stream followed by a step of introducing said M6' stream into a digester to enable the digestion of the organic matter contained in the M6' stream.

[0146] The additional cooling step makes it possible, for example, to cool the M6 ​​flow to a temperature less than or equal to 100°C, preferably less than or equal to 60°C, more preferably less than or equal to 40°C.

[0147] According to one embodiment, the cooled M6' stream is then introduced into a digester to undergo a digestion step.

[0148] Digestion can be carried out according to any digestion method known to those skilled in the art.

[0149] According to one embodiment, the treatment method according to the invention comprises at least one anaerobic digestion step implemented on the M6' stream.

[0150] Anaerobic digestion can be mesophilic or thermophilic.

[0151] When mesophilic digestion is implemented, then the temperature in the digester ranges from 33°C to 37°C and the residence time is 16 to 22 days.

[0152] When thermophilic digestion is implemented, then the temperature in the digester ranges from 55° to 60°C and the residence time is 10 to 12 days.

[0153] Residence time and temperature are two factors influencing the proper degradation of sludge and therefore the optimization of energy production.

[0154] When the flow to be digested is sufficiently liquid, digestion can be of the UASB type and residence times reduced.

[0155] At the end of the digestion stage, biogas is obtained.

[0156] This biogas typically comprises a mixture consisting essentially of methane, carbon dioxide and water. The biogas may optionally comprise other gases, such as hydrogen, oxygen, nitrogen, hydrogen sulfide, but these other gases collectively represent less than 10% by weight of the biogas, of the total weight of the biogas.

[0157] According to one embodiment, at least a fraction of the M3 flow enriched in soluble materials leaving the reactor is sent to one or more subsequent treatment stages.

[0158] In the embodiment implementing two filters, the two flow lines M3 and M3' are advantageously recombined upstream of the subsequent processing steps.

[0159] Among the subsequent treatments that can be implemented, mention may be made of an additional heating step, a hydrothermal gasification step. According to this embodiment, the heat exchange(s) (X1, X2) described in the present invention and the digestion described in the invention will be implemented where appropriate, downstream of said subsequent treatments.

[0160] According to a particular embodiment of the invention, the hydrotreatment process comprises: pressurizing the mixture M1 comprising at least organic matter in order to obtain a mixture flow M1p having a pressure ranging from 150 to 350 bars, a step of heating the mixture M1p to a temperature ranging from 250 to 350°C, making it possible to obtain a mixture flow M2, an introduction of the flow M2 through an inlet E1 into a hydrotreatment reactor by injection facing an impact plate in order to create a mechanical shock, said impact plate preferably being a siphon partition, a step of vertical injection of water ES1 at a temperature of at least 374°C and at a pressure of at least 225 bars directly into the hydrotreatment reactor through an inlet E2, a recovery of a flow M3 enriched in soluble matter and a flow M4 depleted in soluble matter, the recovery of the flow M4 being carried out through an outlet S2 of the reactor,

[0161] exit S2 and entrance E2 each being located at a lower altitude than entrance E1,

[0162] exit S2 being at a higher altitude than entrance E2.

[0163] According to a particular embodiment of the invention, the hydrotreatment process comprises: pressurizing the mixture M1 comprising at least organic matter in order to obtain a mixture flow M1p having a pressure ranging from 150 to 350 bars, a step of heating the mixture M1p to a temperature ranging from 250 to 350°C, making it possible to obtain a mixture flow M2, an introduction of the flow M2 through an inlet E1 into a hydrotreatment reactor by injection facing an impact plate in order to create a mechanical shock, said impact plate preferably being a siphon partition, a step of vertical injection of water ES1 at a temperature of at least 374°C and at a pressure of at least 225 bars directly into the hydrotreatment reactor through an inlet E2, a recovery of a flow M3 enriched in soluble matter and a flow M4 depleted in soluble matter, the recovery of the flow M4 being carried out through an outlet S2 of the reactor,

[0164] exit S2 and entrance E2 each being located at a lower altitude than entrance E1,

[0165] exit S2 being at a higher altitude than entrance E2,

[0166] the M3 stream being recovered downstream of a filter preferably present in the hydrotreatment reactor, said filter having at least one filtration layer having a mesh size of less than 40 µm.

[0167] According to a particular embodiment of the invention, the hydrotreatment process comprises: pressurizing the mixture M1 comprising at least organic matter in order to obtain a mixture flow M1p having a pressure ranging from 150 to 350 bars, a step of heating the mixture M1p to a temperature ranging from 250 to 350°C, making it possible to obtain a mixture flow M2, said heating step comprising at least one step of injecting water ES at a temperature of at least 374°C and at a pressure of at least 225 bars, an introduction of the flow M2 through an inlet E1 into a hydrotreatment reactor by injection facing an impact plate in order to create a mechanical shock, said impact plate preferably being a siphon partition, a step of vertical injection of water ES1 at a temperature of at least 374°C and at a pressure of at least 225 bars directly into the hydrotreatment reactor through an inlet E2,a recovery of a flow M3 enriched in soluble materials and a flow M4 depleted in soluble materials, the recovery of the flow M4 being implemented by an outlet S2 of the reactor,

[0168] exit S2 and entrance E2 each being located at a lower altitude than entrance E1,

[0169] exit S2 being at a higher altitude than entrance E2,

[0170] the M3 flow being recovered downstream of a filter preferably present in the hydrotreatment reactor, said filter having at least one filtration layer having a mesh size of less than 40 µm,

[0171] the M2 mixing flow feeding a static turbulator present upstream of the hydrotreatment reactor.

[0172] According to a particular embodiment of the invention, the hydrotreatment process comprises:pressurizing the mixture M1 comprising at least organic matter in order to obtain a mixture flow M1p having a pressure ranging from 150 to 350 bars,a step of heating the mixture M1p to a temperature ranging from 250 to 350°C, making it possible to obtain a mixture flow M2, said heating step comprising at least one step of injecting water ES at a temperature of at least 374°C and at a pressure of at least 225 bars,an introduction of the flow M2 through an inlet E1 into a hydrotreatment reactor by an injection facing an impact plate in order to create a mechanical shock, said impact plate preferably being a siphon partition,a step of vertical injection of water ES1 at a temperature of at least 374°C and at a pressure of at least 225 bars directly into the hydrotreatment reactor through an inlet E2,a recovery of a flow M3 enriched in soluble materials and a flow M4 depleted in soluble materials, the recovery of the flow M4 being implemented by an outlet S2 of the reactor,

[0173] exit S2 and entrance E2 each being located at a lower altitude than entrance E1,

[0174] exit S2 being at a higher altitude than entrance E2,

[0175] the M3 flow being recovered downstream of a filter preferably present in the hydrotreatment reactor, said filter having at least one filtration layer having a mesh size of less than 40 µm,

[0176] the hydrotreatment reactor further comprising a baffle system for guiding the upward flow created by the vertical injection of water during step d), before the recovery of the M3 flow enriched in soluble materials downstream of the reactor.

[0177] According to a particular embodiment of the invention, the hydrotreatment process comprises: pressurizing the mixture M1 comprising at least organic matter in order to obtain a mixture flow M1p having a pressure ranging from 150 to 350 bars, a step of heating the mixture M1p to a temperature ranging from 250 to 350°C, making it possible to obtain a mixture flow M2, said heating step comprising at least one step of injecting water ES at a temperature of at least 374°C and at a pressure of at least 225 bars, an introduction of the flow M2 through an inlet E1 into a hydrotreatment reactor by injection facing an impact plate in order to create a mechanical shock, said impact plate preferably being a siphon partition, a step of vertical injection of water ES1 at a temperature of at least 374°C and at a pressure of at least 225 bars directly into the hydrotreatment reactor through an inlet E2,a recovery of a flow M3 enriched in soluble materials and a flow M4 depleted in soluble materials, the recovery of the flow M4 being implemented by an outlet S2 of the reactor,

[0178] exit S2 and entrance E2 each being located at a lower altitude than entrance E1,

[0179] exit S2 being at a higher altitude than entrance E2,

[0180] the M3 flow being recovered downstream of a filter preferably present in the hydrotreatment reactor, said filter having at least one filtration layer having a mesh size of less than 40 µm,

[0181] the hydrotreatment reactor further comprising a baffle system for guiding the upward flow created by the vertical injection of water during step d), before the recovery of the M3 flow enriched in soluble matter downstream of the reactor,

[0182] said method further comprising:

[0183] - a water pressurization step W1 up to a pressure of at least 225 bars,

[0184] - a heat exchange step X1 downstream of said water pressurization, making it possible to recover heat from the flow M3 to at least partially heat the water W1 intended to be injected in step d) and / or in step b) and / or in step f), making it possible to obtain, downstream of the exchange X1, a cooled flow M5' and a flow of heated water W2,

[0185] - an additional heating step implemented on the flow of heated water W2, downstream of said heat exchange X1, making it possible to heat the water to a temperature of at least 374°C before its injection in step d) and / or in step b),

[0186] - a heat exchange step X2, downstream of the heat exchange X1, making it possible to recover heat from the flow M5' to heat the mixture M1p upstream of the water injection during step b) of the process, this heat exchange X2 then making it possible to obtain a cooled flow M5''.

[0187] The invention also relates to an installation for implementing the hydrotreatment process according to the invention.

[0188] The drawings illustrate embodiments of the invention, without limiting its scope.

[0189] The installation according to the invention comprises: a mixture supply line M1, a pressurizing pump 2 supplied by the mixture supply line M1 and comprising a mixture outlet line M1p, a heating device 11 supplied with at least a fraction of the mixture M1p downstream of the pump 2 and having an outlet for the mixture flow M2, downstream of the heating device, a hydrotreatment reactor 1 comprising an inlet E1 for injecting the flow M2, an inlet E2 for injecting water, an outlet S1 for extracting a flow M3 and an outlet S2 for extracting a flow M4, said reactor further comprising at least one impact plate P located opposite the inlet E1 in order to create a mechanical shock during the injection of the flow M2 into the reactor, a water injection device ES1 directly into the reactor allowing a vertical injection from the bottom to the top via the inlet E2 of the reactor 1,

[0190] exit S2 and entrance E2 each being located at a lower altitude than entrance E1.

[0191] According to a preferred embodiment, the inlet E2 is at a lower altitude than the outlet S2.

[0192] According to one embodiment of the installation, the heating device 11 is chosen from one or more elements among: a water injection device, an external heating device, said external heating device being able to be chosen from an electric heating device, a heat exchanger by a hot fluid (gas / liquid), a microwave heating device, or a combination of these.

[0193] According to a preferred embodiment of the invention, the heating device 11 comprises at least one water injection device ES into the mixing line M1p. This embodiment is illustrated in the Figures.

[0194] According to one embodiment, the heating device 11, 11' comprises a heat exchanger 8 and a water injection device ES in the mixing line M1p, preferably, the heat exchanger 8 is upstream of the water injection device ES. This embodiment is illustrated in the.

[0195] According to one embodiment, the hydrotreatment reactor 1 further comprises at least one filter F1, the filter preferably being arranged within the reactor, on the outlet line of the hydrotreated organic matter M3 arranged in such a way that the hydrotreated organic matter M3 passes through the filter before leaving the reactor via the outlet S1. An embodiment implementing a filter in the reactor is illustrated in.

[0196] According to one embodiment, the hydrotreatment reactor 1 comprises an impact plate P and a baffle system C1, C2 making it possible to guide the upward flow created by the vertical injection of water ES1 via the inlet E2 before its extraction via the outlet S1, the outlet S1 preferably being in the upper part of the reactor, allowing vertical extraction from the bottom to the top of the flow M3. This embodiment is illustrated in, and.

[0197] The baffle system may comprise two plates C1 and C2, a first plate C1 for guiding the upward flow in a vertical direction and a second plate C2, the upper end of which is at a higher altitude than that of the plate C1, to allow the flow arriving at the upper end of the plate C1 to be directed towards the bottom of the reactor. Preferably, the lower end of the plate C2 is at a lower altitude than that of the filter. This thus allows the soluble matter of the flow to be sucked by the filter and the insoluble matter of the flow to descend towards the bottom of the reactor.

[0198] According to one embodiment, the installation further comprises a static turbulator 10 supplied by the flow line M2, said static turbulator being upstream of the hydrotreatment reactor 1. The mixture leaving the turbulator 10 supplies the hydrotreatment reactor 1. This embodiment is illustrated in the.

[0199] The static turbulator may be chosen from a propeller, blades or elbows or combinations thereof. Thus, for example, the mixing flow supply line M2 located between the water injection device ES and the hydrotreatment reactor 1 may comprise one or more elbows making it possible to provide turbulence, thus improving the exchanges between the water and the sludge.

[0200] According to an embodiment illustrated in the, the hydrotreatment reactor 1 implemented in the invention comprises:an inlet E1 for the inlet of the flow M2 into the reactor,an impact plate P located opposite the inlet E1 in order to create a mechanical shock during the injection of the flow M2 into the reactor,an outlet S1 for extracting a flow M3 enriched in soluble materials,an outlet S2 for extracting a flow M4 depleted in soluble materials, the outlet S2 being at a lower altitude than the inlet E1,an inlet E2 for injecting water directly into the reactor, the inlet E2 being at a lower altitude than the inlet E1,a filter F1 on the outlet line of the flow M3 arranged in such a way that the flow M3 passes through the filter F1 before leaving the reactor via the outlet S1,

[0201] preferably, the S2 exit is at a higher altitude than the E2 entrance.

[0202] According to an embodiment illustrated in the, the hydrotreatment reactor 1 comprises: an inlet E1 for the inlet of the flow M2 into the reactor, an impact plate P located opposite the inlet E1 in order to create a mechanical shock during the injection of the flow M2 into the reactor, an outlet S1 for extracting a flow M3 enriched in soluble materials, an outlet S1' separate from the outlet S1 for extracting a flow M3' enriched in soluble materials, an outlet S2 for extracting a flow M4 depleted in soluble materials, the outlet S2 being at a lower altitude than the inlet E1, an inlet E2 for injecting water directly into the reactor, the inlet E2 being at a lower altitude than the inlet E1, a first filter F1 on the outlet line of the flow M3 arranged in such a way that the flow M3 passes through the first filter F1 before leaving the reactor via the outlet S1,and a second filter F1' on the outlet line of the flow M3' arranged in such a way that the flow M3' passes through the second filter F1' before leaving the reactor via the outlet S1',

[0203] preferably the exit S2 is at a higher altitude than the entrance E2,

[0204] preferably the exit S1' is at a higher altitude than the entrance E1,

[0205] preferably the outputs S1 and S1' are substantially at the same altitude.

[0206] According to the embodiment implementing two filters, preferably, the installation according to the invention comprises a recombination of the flow lines M3 and M3'. This embodiment is illustrated in the.

[0207] Illustrates an embodiment of the invention, where the installation comprises: a mixture supply line M1, a pressurizing pump 2 supplied by the mixture supply line M1 and having an outlet for the mixture M1p, a heating device 11 comprising at least one water injection device ES in the mixture supply line M1p downstream of the pump 2, a hydrotreatment reactor 1 comprising: an inlet E1 for the inlet of the flow M2, an impact plate P located opposite the inlet E1 in order to create a mechanical shock during the injection of the flow M2 into the reactor, an outlet S1 for extracting a flow M3 enriched in soluble matter, an outlet S2 for extracting a flow M4 depleted in soluble matter, an inlet E2 for injecting water ES1, the inlet E2 being at a lower altitude than the inlet E1, a filter F1 on the outlet line of the flow M3 arranged in such a way that the flow M3 passes through filter F1 before exiting the reactor through outlet S1,

[0208] preferably, the outlet S1 is in the upper part of the reactor and allows extraction of the flow M3 vertically, from bottom to top, and

[0209] preferably, the inlet E2 is in the lower part of the reactor and allows vertical water injection, from bottom to top, possibly a valve V1 allowing control of the flow outlet M3.

[0210] It differs from the in that: a baffle system is present, and a turbulator 10 is present upstream of the reactor and is fed by the flow line M2.

[0211] As illustrated in the, the baffle system, for example consisting of two plates C1 and C2, can be present in the reactor and allows to guide the upward flow created by the vertical injection of water via the inlet E2 before its extraction by the outlet S1. In the case of the, the flow around the baffle system is illustrated by the two dotted arrows, with an upward flow circulating on one side of the first plate C1 then a downward flow circulating on the other side of the plate C1, between the plates C1 and C2, this downward flow is allowed thanks to a plate C2 whose upper end is at a higher altitude than that of the plate C1. As illustrated in the, the lower end of the plate C2 is preferably located at a lower altitude than that of the filter, in order to allow the soluble matter of the flow to be sucked by the filter and the insoluble matter (solid) to descend towards the bottom of the reactor.

[0212] As illustrated in, the turbulator 10 may be a system of elbows.

[0213] Illustrates one embodiment of the invention, wherein the method further comprises at least one step of preheating the water to a temperature of at least 374°C.

[0214] The installation illustrated in shows a heat exchange step X1 via a heat exchanger 6. The heat exchanger 6 makes it possible to recover the heat present in the flow M3 leaving the hydrotreatment reactor 1 to transfer it to the water in order to heat the water intended to be injected into the process of the invention, i.e. the water used during step d), and / or where appropriate the water used during step b) and / or where appropriate the water used during step f).

[0215] According to an embodiment illustrated in the, the installation according to the invention further comprises:

[0216] - a heat exchanger 6 downstream of the hydrotreatment reactor, said heat exchanger 6 making it possible to recover the heat from the flow M3, possibly combined with the flow M3', to obtain a cooled flow M6' and to transfer this heat to the water W1 upstream of the water injection device ES1 and / or the water injection device ES1 and / or upstream of the water injection device ES2 to obtain a flow of heated water W2, and

[0217] - a water heating device 7, downstream of the heat exchanger 6 and upstream of the water injection device ES, said heating device 7 being supplied by the water W2 and making it possible to obtain water at a temperature of at least 374°C, this water can then advantageously supply the water injection device ES and / or the water injection device ES1 and / or the water injection device ES2.

[0218] Preferably, when the installation comprises a water injection line ES2, said water ES2 is introduced into the flow line M3 via a water supply line leaving the heating device 7 (case 1a) or leaving a branch of the water supply line ES.

[0219] According to an embodiment shown in , the water heating device 7 makes it possible to supply water to all the water injection devices at a temperature of at least 374°C present in the installation, for example, the water injection device ES1, the water injection device ES and the water injection device ES2.

[0220] According to an embodiment not shown, the installation according to the invention comprises on the water supply line W1, a pressurization pump advantageously making it possible to bring the water to a pressure of at least 225 bars (before heating it).

[0221] Advantageously, the installation further comprises a control unit for controlling the water injection ES2 and the outlet S2. Indeed, preferably, the outlet S2 is open (thanks to the valve V2) when water is injected via the supply line ES2.

[0222] According to an embodiment illustrated in the, the installation further comprises: a cooling device 4 supplied with at least a fraction of the flow M5' making it possible to produce steam and a cooled flow M6, a device 3 for injecting said steam produced into the mixture flow M1 upstream of the pressurizing pump 2, said injection device 3 possibly being a reactor, a cooling device 9 downstream of the cooling device 4 making it possible to cool at least a fraction of the flow M6 to obtain a flow M6', and a digester 5 supplied by the flow M6'.

[0223] According to an embodiment not shown in the but advantageous, the water heating device 7 also makes it possible to supply water to the water injection device ES1. In particular, the installation illustrated in the will further advantageously comprise a water supply line connecting the heating device 7 and the injection device ES1.

[0224] As in the embodiment illustrated in the, the installation of the comprises a baffle system (C1, C2).

[0225] Illustrates an embodiment of the method according to the invention comprising two heat exchanges X1 and X2.

[0226] Thus, according to an embodiment illustrated in the, the installation according to the invention comprises: a heat exchanger 6 downstream of the hydrotreatment reactor, said heat exchanger making it possible to recover the heat from the flow M3, possibly combined with the flow M3', to obtain a flow M3' and to transfer this heat to the water W1 upstream of a heating device 7, making it possible to obtain heated water W2, a water heating device 7, downstream of the heat exchanger 6 supplied by the heated water W2 and upstream of the water injection device ES1 and / or upstream of the water injection device ES and / or upstream of the water injection device ES2, a heat exchanger 8 making it possible to recover heat from the mixture M3' to obtain a mixture M3'' and to transfer this heat to the mixture M1p upstream of the water injection device ES,a cooling device 4 supplied with at least a fraction of the flow M3' making it possible to produce steam and a cooled flow M6, a device for injecting said steam produced into the mixture flow M1 upstream of the pressurizing pump 2, said injection device 3 possibly being a reactor, a cooling device 9 downstream of the cooling device 4 making it possible to cool at least a fraction of the flow M6 to obtain a flow M6', and a digester 5 supplied by the flow M6'.,

[0227] According to an embodiment illustrated in the, the heating device 11, 11' comprises a heat exchanger 8 and a water injection device ES. According to the embodiment illustrated in the, the heating step b) of the method comprises two sub-steps: a first sub-step of heat exchange between the flow M1p and flow M3, said flow M3 having optionally been subjected to one or more heat exchanges between the outlet of the reactor and this heat exchange with M1p, a second sub-step of injection of water ES at a temperature of at least 374°C and preferably at a pressure of at least 225 bars, in the flow line M1p downstream of the first sub-step.

[0228] As in the embodiment illustrated in the, the installation of the comprises a baffle system (C1, C2).

[0229] According to an embodiment not shown in the but advantageous, the water heating device 7 also makes it possible to supply water to the water injection device ES1.

[0230] In particular, the installation illustrated in will further advantageously comprise a water supply line connecting the heating device 7 and the injection device ES1.

[0231] According to an embodiment not shown in the Figures, the installation according to the invention further comprises at least one post-treatment device supplied by at least a fraction of the flow M3 downstream of the hydrotreatment reactor 1. When the installation further comprises at least one heat exchanger 6, then said post-treatment device is upstream of said heat exchanger 6. Preferably, said post-treatment device is chosen from a complementary heating step, a hydrothermal gasification step.

Claims

A method for hydrotreating a mixture M1 comprising at least organic matter, said method comprising:pressurizing the mixture M1 comprising at least organic matter to a pressure ranging from 20 to 350 bars, in order to obtain a mixture flow M1p,a step of heating the mixture M1p to a temperature ranging from 170 to 430°C, making it possible to obtain a mixture flow M2,an introduction of the flow M2 through an inlet E1 into a hydrotreatment reactor by injection facing an impact plate in order to create a mechanical shock,a step of vertical injection of water ES1 at a temperature of at least 374°C directly into the hydrotreatment reactor through an inlet E2,a recovery of a flow M3 enriched in soluble matter and a flow M4 depleted in soluble matter, the recovery of the flow M4 being implemented through an outlet S2 of the reactor,the outlet S2 and the inlet E2 each being located at an altitude lower than entrance E1. Hydrotreatment process according to claim 1, wherein the recovery of the M3 stream enriched in soluble materials during step e) is carried out through at least one filter, said filter comprising at least one filtration layer preferably having a mesh size of less than 100 µm, preferably less than 50 µm, more preferably less than 40 µm, said filter preferably being in the hydrotreatment reactor. Hydrotreatment process according to claim 1 or 2, in which step b) comprises at least one step of injecting ES water at a temperature of at least 374°C into the flow of mixture M1p in order to obtain the flow M2, the injected water preferably being at a pressure of at least 225 bars. Hydrotreatment process according to any one of claims 1 to 3, in which the recovery of the M3 stream during step e) is controlled by determining the pressure difference between the pressure in the hydrotreatment reactor and the pressure in the M3 stream at the outlet of the reactor, where appropriate downstream of the filter. A hydrotreatment process according to any one of claims 1 to 4, wherein the hydrotreatment reactor is maintained at a temperature ranging from 150°C to a temperature below 374°C. Hydrotreatment process according to any one of claims 2 to 5, further comprising, downstream of the filter and downstream of the reactor, a step f) of injecting water at a temperature of at least 374°C into the flow M3, counter-current to said flow, where appropriate said water preferably being at the same temperature and at the same pressure as the water injected during step b). Hydrotreatment process according to claim 6, wherein, when the countercurrent water injection of step f) is implemented, then the outlet S2 of the reactor is opened in order to extract a stream M4. Hydrotreatment process according to any one of claims 1 to 7, in which the hydrotreatment reactor further comprises a baffle system making it possible to guide the upward flow created by the vertical injection of water ES1 before extraction of the flow M3 during step e) by an upper part of the reactor, preferably through a filter. Hydrotreatment process according to any one of claims 1 to 8, further comprising; at least one heat exchange step X1 making it possible to recover heat from the flow M3 to at least partially heat the water intended to be injected for the heating step b), a cooled flow M5' then being obtained, and optionally comprising at least one additional water heating step, downstream of the heat exchange X1 making it possible to heat the water to the temperature of at least 374°C before its injection in step d) and / or where appropriate before its injection in step b) and / or where appropriate before its injection in step f), and optionally at least one heat exchange step X2 making it possible to recover heat from the flow M5' to heat the mixture M1p upstream of the water injection of step b), a flow M5'' then being obtained. Hydrotreatment process according to claim 9, further comprising:at least one step of cooling at least a fraction of the stream M5' or where appropriate of the stream M5'' making it possible to obtain steam and a stream M6 comprising hydrotreated organic matter, anda step of injecting at least a portion of said steam to preheat the mixture M1 upstream of step a) of pressurizing, said mixture M1 preferably being preheated to a temperature ranging from 50 to 170°C, preferably from 50 to 90°C,optionally a step of cooling at least a fraction of the stream M6 to obtain a cooled stream M6' and optionally a step of digesting the stream M6'. Hydrotreatment method according to one of claims 1 to 11, in which the impact plate comprises an excess thickness which resists erosion. Installation for implementing the hydrotreatment process according to any one of claims 1 to 11, said installation comprising: a mixture supply line M1, a pressurizing pump (2) supplied by the mixture supply line M1 and comprising a mixture outlet line M1p, a heating device (11) supplied with at least a fraction of the mixture M1p downstream of the pump 2 and having an outlet for the mixture flow M2, downstream of the heating device, a hydrotreatment reactor (1) comprising an inlet E1 for injecting the flow M2, an inlet E2 for injecting water ES1, an outlet S1 for extracting a flow M3 and an outlet S2 for extracting a flow M4, said reactor further comprising at least one impact plate located opposite the inlet E1 in order to create a mechanical shock during the injection of the flow M2 into the reactor,a water injection device ES1 directly into the reactor allowing vertical injection from bottom to top via the inlet E2 of the reactor (1), the outlet S2 and the inlet E2 each being located at a lower altitude than the inlet E1., Installation according to claim 12, in which the hydrotreatment reactor (1) further comprises: at least one first filter F1, said first filter being arranged in such a way that the flow M3 enriched in soluble matter passes through the filter before leaving the reactor via the outlet S1, and optionally at least one second filter F1', said second filter F1' being arranged in such a way that the flow M3' enriched in soluble matter passes through said second filter F1' before leaving the reactor (1) via an outlet S1', preferably, the outlets S1 and S1' are located in the upper part of the hydrotreatment reactor 1 and preferably allow vertical extraction, from the bottom to the top of the flows M3 and M3' respectively. Installation according to claim 12 or 13, in which the hydrotreatment reactor (1) further comprises a baffle system making it possible to guide the upward flow created by the vertical injection of water via the inlet E2 before its extraction via the outlet S1, the outlet S1 preferably being in the upper part of the reactor, allowing a vertical outlet from the bottom to the top. Installation according to any one of claims 12 to 14, in which the heating device (11) comprises at least one water injection device ES in the mixing line M1p, said installation preferably further comprising: a heat exchanger (6) downstream of the hydrotreatment reactor (1), said heat exchanger making it possible to recover the heat in the flow line M3, possibly combined with the flow line M3', to obtain a flow M5' and to transfer this heat to the water upstream of the water injection device ES1 and / or upstream of the water injection device ES, and optionally a water heating device (7), downstream of the heat exchanger (6) and upstream of the water injection device ES and upstream of the water injection device ES1, said heating device (7) advantageously comprising at least two outlet lines,a line connected to the water injection device ES1 and a line connected to the water injection device ES,said installation preferably further comprising:optionally a heat exchanger (8) for recovering heat from the mixture M5' to obtain a mixture M5'' and transferring this heat to the mixture M1p upstream of the water injection device ES,A cooling device (4) supplied by at least a fraction of the flow M5' or, where appropriate, M5'', for producing steam and a cooled flow M6,A device (3) for injecting said steam produced into the mixture flow M1 upstream of the pressurizing pump (2),optionally a cooling device (9) downstream of the cooling device (4) supplied by at least a fraction of the flow M6 for cooling at least a fraction of the flow M6 to obtain a flow M6', andoptionally a digester (5) supplied by the flow M6'.,