Key information

Title
Hydrothermal liquefaction with alkaline regeneration using lime
Application number
20250030
Case type
National
Status
10.01.2025 Andre og senere realitetsskriv foreligger
Filed
10.01.2025
Effective date
10.01.2025
Publicly available
13.07.2026
Next annual fee due
31.01.2027
Applicant
SILVA BIOFUEL AS (NO)
Inventor
Claus Uhrenholt Jensen (DK) et al.
Agent
ACAPO ONSAGERS AS (NO)

Abstract and drawing

Disclaimer: This text has been machine-scanned and may contain errors – please refer to "Publications" for legally binding content.
The present disclosure provides an alkaline HTL-process for production of biofuel from a carboncontaining Feedstock (1) such as biomass, especially from lignocellulosic biomass, wherein an aqueous phase is recycled to a Feedstock vessel (2) via a pH-regulation unit (5).

Publications

A1
Checking availability of the latest published version...

Documents

 Expand Download files (22)
Date
 Date Doc. No. Process Case number In/Out Journal description To/from
 04.09.2026 10-01 Saksbehandling 20250030 UT PT Bekreftelse på fristutsettelse ACAPO ONSAGERS AS
 04.09.2026 02-01 Overdragelse av søknad/rettighet 2026/06689 UT Tilbakemelding på generell henvendelse ACAPO ONSAGERS AS
 02.09.2026 01-03 Overdragelse av søknad/rettighet 2026/06689 INN P29814NO00 - ASSIGNMENT SIGNED - SGF -SBF ACAPO ONSAGERS AS
 02.09.2026 01-02 Overdragelse av søknad/rettighet 2026/06689 INN NIPO_GPOA Silva Biofuel AS_7653187 ACAPO ONSAGERS AS
 02.09.2026 01-01 Overdragelse av søknad/rettighet 2026/06689 INN Generell henvendelse ACAPO ONSAGERS AS
 04.06.2026 09-01 Saksbehandling 20250030 UT Substantive Examination ACAPO ONSAGERS AS
 17.04.2026 08-04 Saksbehandling 20250030 INN P29814NO00 substitute sheest pages 1 to 16 - with annotations 1311658 ACAPO ONSAGERS AS
 17.04.2026 08-03 Saksbehandling 20250030 INN P29814NO00 substitute sheest pages 1 to 16 - clean copy 1311659 ACAPO ONSAGERS AS
 17.04.2026 08-02 Saksbehandling 20250030 INN p29814no 00 brev til Patentstyret med besvarelse av første uttalelse 1316824 ACAPO ONSAGERS AS
 17.04.2026 08-01 Saksbehandling 20250030 INN Korrespondanse (Hovedbrev inn) ACAPO ONSAGERS AS
 05.01.2026 06-01 Saksbehandling 20250030 UT Henlagt manglende svar ENG ACAPO ONSAGERS AS
 24.06.2025 05-02 Saksbehandling 20250030 UT PT report 01:35:18
24.06.2025 05-01 Saksbehandling 20250030 UT Substantive Examination ACAPO ONSAGERS AS
 28.02.2025 04-03 Saksbehandling 20250030 INN P29814NO00Declaring rights to invention form ACAPO ONSAGERS AS
 28.02.2025 04-02 Saksbehandling 20250030 INN P29814NO00 Fullmakt_Jan_13,_2025 ACAPO ONSAGERS AS
 28.02.2025 04-01 Saksbehandling 20250030 INN Korrespondanse (Hovedbrev inn) ACAPO ONSAGERS AS
 13.01.2025 03-01 Saksbehandling 20250030 UT Formal Examination 1 ACAPO ONSAGERS AS
 13.01.2025 02-01 Saksbehandling 20250030 UT Informasjon til oppfinner Anders Tagmose Lundsfryd
 10.01.2025 01-03 Saksbehandling 20250030 INN P29814NO00 Patent application draft 1202995 ACAPO ONSAGERS AS
 10.01.2025 01-02 Saksbehandling 20250030 INN P29814NO00 Figures final 1205485 ACAPO ONSAGERS AS
 10.01.2025 01-01 Saksbehandling 20250030 INN Søknadsskjema Patent ACAPO ONSAGERS AS
 07-02 Saksbehandling 20250030 INN Korrespondanse (Hovedbrev inn) ACAPO ONSAGERS AS

Description, claims and drawings

Disclaimer: This text has been machine-scanned and may contain errors – please refer to "Publications" for legally binding content. Description
TitleHydrothermal liquefaction with alkaline regeneration using lime.FieldThe present disclosure concerns hydrothermal liquefaction of carbon-containing feedstocks for generating an oil phase (also known as biocrude).BackgroundThermochemical biomass conversion technologies such as gasification, pyrolysis, and hydrothermal liquefaction (HTL) are being developed in order to produce biofuel ingredients from biomass. HTL is currently viewed with the potential to become a competitive and resource-effective pathway to advanced biofuels from lignocellulosic biomass, mainly due to its high energy-efficiency.SummaryThe present disclosure provides a versatile and cost-efficient HTL-system and HTL-process involving recycling of aqueous phase. By providing a calcium source to the aqueous phase (9) to be recycled, beneficial extraction of calcium carbonate from the recycled aqueous phase (9) can be achieved. It is found that by incorporating a calcination loop to extract calcium carbonate and thus increase pH of a recycled aqueous phase (9), the need for expensive KOH/NaOH supply can be reduced by at least 25%. Furthermore, a Calciner (6) can allow capture and/or sequestration of CO2 thus reducing carbon-emissions from the process and ultimately the carbonintensity of the resulting biocrude. In spite of the risk of introducing solid inorganic particles to the recycled aqueous phase, and in spite of potential fouling in case of increased calcium concentration in the recycled aqueous phase, it is found that the calcination loop works well. Suitable filters for removing fines can be used, and no increase in calcium concentration has been observed. Instead, a beneficial slight decrease in the calcium concentration was detected in the recycled aqueous phase (9). Unexpectedly, CaO was shown to be able to slake into Ca(OH)2 in the aqueous phase despite the complex reaction medium, resulting in a beneficial economical and process design, due to the synergy with an exothermic slaking reaction parallel with the endothermic carbonation reaction, making a Lime slaker (7) optional.The present disclosure relates to a system for alkaline hydrothermal liquefaction of a carbon-containing Feedstock, comprisinga) a Feedstock vessel comprising an inlet for carbon-containing Feedstock and an outlet for providing an alkaline feed mixture comprising the carbon-containing Feedstock, b) a hydrothermal liquefaction -reactor comprising an inlet for the alkaline feed mixture comprising carbon-containing Feedstock and an outlet for an HTL product stream,c) a Phase Separator comprising an inlet for the HTL product stream and an outlet for an aqueous product phase and an outlet for an oil product phase, d) a pH-regulation unit comprising an inlet for a calcium source and an outlet for calcium carbonate,wherein the system is configured to recycle aqueous product phase from the Phase Separator back to the Feedstock vessel via the pH-regulation unit.In one aspect of the system, the Calciner is configured to provide the calcium source to the pH-regulation unit, and wherein the pH-regulation unit is configured to provide calcium carbonate to the Calciner.In one aspect of the system, the carbon-containing Feedstock comprises biomass, mixtures of biomass and plastic, lignite, black liquor, industrial waste and/or municipal waste.In one aspect of the system, the carbon-containing Feedstock comprises lignocellulosic biomass.In one aspect of the system, a Calciner is configured to, directly or indirectly, provide CaO and/or Ca(OH)2 into the pH-regulation unit.In one aspect of the system, the pH-regulation unit is configured to extract CaCO3 from the aqueous phase to be recycled.In one aspect of the system, the calcium source is in the form of CaO particles. In one aspect of the system, the calcium source is in the form of Ca(OH)2 particles, Ca(OH)2 slurry or an aqueous solution comprising dissolved Ca(OH)2.In one aspect, the system can further comprise a Lime slaker configured to receive CaO from a Calciner and for providing Ca(OH)2 to the pH-regulation unit.In one aspect, the system can be configured for allowing CaO and/or Ca(OH)2 to increase the pH of the aqueous phase and for allowing CaCO3 to be precipitated and provided to the Calciner.In one aspect, the system can be configured for performing HTL at a temperature in the range of 250 °C to 450 °C and at a pressure in the range of 150 to 400 bar. In one aspect, the system can involve Calciner solids bleed and CaO makeup for mitigating accumulated impurity of the recycled CaO and CaCO3.The present disclosure also provides a method for alkaline recovery in a hydrothermal liquefaction of a carbon-containing Feedstock, comprising the steps a) providing an aqueous feed mixture with alkaline pH comprising a carboncontaining Feedstock,b) subjecting the aqueous feed mixture in step a) to hydrothermal liquefaction for providing an HTL product stream,c) separating an aqueous product phase and an oil product phase from the HTL product stream in step b),d) recirculating and mixing all or a fraction of the aqueous product phase from step c) into to the aqueous feed mixture in step a), ande) adding a calcium source to the recirculating aqueous product phase and extracting solid CaCO3 formed thereof upstream of said mixing of the aqueous product phase in step d).In one aspect of the method, the carbon-containing Feedstock comprises biomass, mixtures of biomass and plastic, lignite, black liquor, industrial waste and/or municipal waste.In one aspect of the method, the carbon-containing Feedstock comprises biomass, plastic particles, lignite, black liquor, industrial waste or municipal waste, or any mixture thereof.In one aspect of the method, the carbon-containing Feedstock comprises lignocellulosic biomass.In one aspect of the method, the aqueous mixture with alkaline pH comprising a carbon-containing Feedstock also contains a source of carbonate ions, such as dissolved K2CO3.In one aspect of the method, CaCO3 is precipitated from the aqueous phase in step e) and provided to a Calciner which directly or indirectly supplies CaO or Ca(OH)2 into the aqueous phase in step e).In one aspect of the method, the HTL is performed at a temperature in the range of 250 °C to 374 °C and at a pressure in the range of 150 to 400 bar. The present disclosure also provides use of a Calciner for directly or indirectly providing CaO or Ca(OH)2 into an aqueous phase recycled from a Phase Separator to a Feedstock vessel in an alkaline HTL-process, wherein CaCO3 is precipitated from the recycled aqueous phase and provided to the Calciner.Brief description of the figuresFigure 1a shows a conventional system for alkaline hydrothermal liquefaction of biomass. A Feedstock (1) comprising biomass is provided to the Biomass vessel (2a) where an alkaline aqueous mixture is obtained by adding pH-increasing agents like alkali metal hydroxides and water as needed. This alkaline mixture is provided to the HTL-reactor (3) and subjected to HTL. The HTL product stream is provided to a Phase Separator (4). A fraction of both the aqueous phase and the oil phase from the Phase Separator (4) is recycled back to the Biomass vessel (2a).Figure 1b shows a Lime cycle involving calcination, hydration and carbonation (i.e. a calcination loop).Figure 2 shows a system for alkaline hydrothermal liquefaction of a carboncontaining Feedstock (1) comprising a calcination loop. A carbon-containing Feedstock (1), such as biomass, is provided to the Feedstock vessel (2) where an alkaline aqueous mixture is obtained by adding pH-increasing agents like alkali metal hydroxides and water as needed. This alkaline mixture is provided to the HTL-reactor (3) and subjected to HTL. The HTL product stream is provided to a Phase Separator (4). A fraction of the aqueous phase from the Phase Separator (4) is recycled back to the Feedstock vessel (2) via a pH-regulation unit (5). A Calciner (6) in fluid connection with the pH-regulation unit (5) is configured to provide CaO (s) to the pH-regulation unit (5), and the pH-regulation unit (5) is configured to provide CaCO3 (s) to the Calciner (6). Calciner solids bleed and CaO makeup can be implemented for mitigating accumulated impurity of the recycled CaO and CaCO3. A Solid phase can also be separated/rejected from the HTL-reactor (3).Figure 3 shows a system for alkaline hydrothermal liquefaction of a carboncontaining Feedstock (1) comprising a calcination loop. A carbon-containing Feedstock (1), such as biomass, is provided to the Feedstock vessel (2) where an alkaline aqueous mixture is obtained by adding pH-increasing agents like alkali metal hydroxides and water as needed. This alkaline mixture is provided to the HTL-reactor (3) and subjected to HTL. The HTL product stream is provided to a Phase Separator (4). A fraction of the aqueous phase from the Phase Separator (4) is recycled back to the Feedstock vessel (2) via a pH-regulation unit (5). The aqueous phase passes through a water recovery unit (8). A Calciner (6) in fluid connection with the pH-regulation unit (5) is configured to provide CaO (s) to the pH regulation unit (5), and the pH-regulation unit (5) is configured to provide CaCO3 (s) to the Calciner (6).Figure 4 shows a system for alkaline hydrothermal liquefaction of a carboncontaining Feedstock (1) comprising a calcination loop. A carbon-containing Feedstock (1), such as lignocellulosic biomass, is provided to the Feedstock vessel (2) where an alkaline aqueous mixture is obtained by adding pH-increasing agents like alkali metal hydroxides, carbonates and water as needed. This alkaline mixture is provided to the HTL-reactor (3) and subjected to HTL. The HTL product stream is provided to a Phase Separator (4). A fraction of both the aqueous phase and the oil phase from the Phase Separator (4) is recycled back to the Feedstock vessel (2). The aqueous phase passes through a water recovery unit (8) before entering the pH-regulation unit (5). A Calciner (6) in fluid connection with the pH-regulation unit (5) is configured to provide CaO (s) to the pH-regulation unit (5), and the pH-regulation unit (5) is configured to provide CaCO3 (s) to the Calciner (6).Figure 5 shows a system for alkaline hydrothermal liquefaction of a carboncontaining Feedstock (1) comprising a calcination loop. A carbon-containing Feedstock (1), such as biomass, is provided to the Feedstock vessel (2) where an alkaline aqueous mixture is obtained by adding pH-increasing agents like alkali metal hydroxides and water as needed. This alkaline mixture is provided to the HTL-reactor (3) and subjected to HTL. The HTL product stream is provided to a Phase Separator (4). A fraction of the aqueous phase from the Phase Separator (4) is recycled back to the Feedstock (1) vessel. The aqueous phase passes through a water recovery unit (8) before entering the pH-regulation unit (5). A Calciner (6) in fluid connection with the pH-regulation unit (5) is configured to provide CaO (s) to a Lime slaker (7) which provides Ca(OH)2 (aq) to the pH-regulation unit (5), and the pH-regulation unit (5) is configured to provide CaCO3 (s) to the Calciner (6).Figure 6 shows a system for alkaline hydrothermal liquefaction of a carboncontaining Feedstock (1) comprising a calcination loop. A carbon-containing Feedstock (1), such as biomass, is provided to the Biomass vessel (2a) where an alkaline aqueous mixture is obtained by adding pH-increasing agents like alkali metal hydroxides and water as needed. This alkaline mixture is provided to the HTL-reactor (3) and subjected to HTL. The HTL product stream is provided to a Phase Separator (4). A fraction of both the aqueous phase and the oil phase from the Phase Separator (4) is recycled back to the Feedstock (1) vessel. The aqueous phase passes through a water recovery unit before entering the pH-regulation unit (5). A Calciner (6) in fluid connection with the pH-regulation unit (5) is configured to provide CaO (s) to a Lime slaker (7) which provides Ca(OH)2 (aq) to the pHregulation unit (5), and the pH-regulation unit (5) is configured to provide CaCO3 (s) to the Calciner (6).Figure 7 shows the Calcium concentration in the aqueous phase after carbonation is lower than reference of no carbonation. This is observed regardless of temperature, reaction time and aqueous phase matrix as direct (PW) or up concentrated (Conc) process water from the Phase Separator, except for a overdosing of lime regarding regeneration potential according to TIC (Total Inorganic Carbon), of which the reference concentration is reobtained.Figure 8 shows that the TIC is decreasing after carbonation reaction, indicating formation of calcium carbonate which as precipitated. The decrease is in range of expected values, except for adding an oversaturation of lime, where it is shown to stabilize at a decrease of 90% in direct and 75% in up-concentrated process water form phase separator.Figure 9 shows the pH increases after carbonation, which, based on stable Ca concentration (Figure 7) and decrease of TIC (Figure 8), suggest a regeneration of alkaline hydroxide. The more lime added, the higher the pH increase.Detailed descriptionThe present disclosure focuses on an alkaline HTL-process and system for production of biofuel from biomass, especially from lignocellulosic biomass, wherein an aqueous phase is recycled to a Feedstock vessel (2) such as a Biomass vessel (2a).FeedstocksHowever, based on the present disclosure, the same system and method can utilize other carbon-containing Feedstocks like plastic granulates or powders. Such Feedstock products can be obtained from waste plastic through processes such as crushing, shredding or grinding. Other Feedstock alternatives involve lignite, black liquor, industrial waste and/or municipal waste, and any mixture thereof.As used herein, biomass is biological material derived from recently living organisms such as plant materials like wood, straw, seeds, and leaves, as well as animal manures and organic fractions of municipal solid and sewage wastes.Lignocellulosic biomass is the most abundantly available raw material for the production of biofuels. It comprises cellulose, hemicellulose and lignin. As used herein, any biomass comprising significant amounts of cellulose, hemicellulose and lignin is referred to as lignocellulosic biomass. In the system and methods herein, a carbon-containing Feedstock (1) such as biomass, in particular lignocellulosic biomass, can be mixed with water and alkali metal salts and/or alkaline aqueous solutions for obtaining an alkaline mixture. Accordingly, the Feedstock (1) comprises a carbon-containing material such as biomass, in particular lignocellulosic biomass. The Feedstock (1) may also contain water and solid or dissolved alkali metal salts as needed for obtaining an alkaline mixture. Preferred alkali metal salts include NaOH, KOH and mixtures of these. Potassium hydroxides and/or sodium hydroxides are well known to catalyze the degradation of macromolecules by hydrolysis, decarboxylation, and depolymerization, as well as inhibit formation of tar, char, and coke. A source of carbonate preferably also be included in the Feedstock (1), such as K2CO3, Na2CO3 or mixtures of these. For example, in one particular embodiment, the Feedstock (1) comprises biomass, a source of carbonate and at least one alkali metal hydroxide. For example, in one particular embodiment, the Feedstock (1) comprises lignocellulosic biomass, K2CO3 and NaOH.Aqueous mixtures with alkaline pH comprising carbon-containing Feedstock (1) such as biomass, in particular lignocellulosic biomass, can be pre-made or made in the Feedstock vessel (2) also referred to as Biomass vessel (2a). The aqueous mixtures with alkaline pH comprising carbon-containing Feedstock (1), preferably as a slurry, can preferably be pressurized and heated and subsequently fed to the HTL-reactor (3) where they are subjected to HTL. In one aspect, the temperature of the slurry provided the HTL-reactor (3) may be in the range of 250 to 420°C, such as 300 to 400°C or 350 to 380°C.Feedstock (1) vesselThe vessel for containing the Feedstock (1) (i.e. the Feedstock vessel (1)) can have any size and shape fitting the HTL-reactor (3) to which it is fluidly connected. The Feedstock vessel (2) can have one or more inlets for Feedstock (1) ingredients. The Feedstock vessel (2) can contain means for mixing aqueous solutions with carboncontaining Feedstock (1), such as biomass, in particular lignocellulosic biomass. Such means include impellers, baffles and any other suitable equipment contributing to thorough mixing. The Feedstock vessel (2) can have one or more heaters for heating the Feedstock (1).HTLIn the HTL-reactor (3), carbon-containing Feedstock (1) such as biomass, in particular lignocellulosic biomass, preferably in the form of a slurry, is subjected to temperatures in the range of 250 to 420°C, such as 300 to 400°C or 350 to 374°C. The pressure in the reactor is preferably in the range of 150 to 500 bar, such as 250 to 400 bar. Generally, HTL is often considered to take place mainly via ionic type of reactions near or below the critical point at temperatures of approximately 280 to 374°C and at a pressure of at least the saturation pressure of water to avoid boiling. A general concept of HTL-reactors (3) for biomass and their energy sources, is described in US2015099275A1 titled “Systems and methods for converting biomass to biocrude via hydrothermal liquefaction”. The technical information therein is incorporated herein.A typical process layout of a hydrothermal liquefaction process is presented in a process flow diagram as shown in figure 18.4 in Handbook of biofuels production, edited by Rafael Luque, Juan Campelo and James Clark © Woodhead Publishing Limited, 2011. The typical hydrothermal liquefaction process for producing a crude biooil is a continuous process where a Biomass Feedstock is added a catalyst and passed to a hydrothermal liquefaction reactor via a pump and heating section comprising a heat exchanger and a heater, lifting the pressure and temperature of the biomass feed flow to HTL-conditions before entry in an HTL-reactor which converts the biomass feed flow into a product flow which exits the HTL-reactor. During this treatment, the carbon-containing Feedstock (1) such as biomass, in particular lignocellulosic biomass, is essentially converted into mixture comprising some solids, a desired oil phase, a gas phase and an aqueous phase. This mixture is the HTL product stream.The HTL product stream can conveniently pass through a heat-exchanger and a cooling unit lowering the temperature as desired. It can also pass through a pressure regulation unit lowering the pressure of the product flow to a suitable pressure for a Phase Separator (4).Phase SeparatorThe HTL product stream can be provided to a Phase Separator (4) allowing separation of a desired oil phase, an aqueous phase (also referred to as Process Water, PW), a solid phase and a gas phase. When entering the Phase Separator (4), the HTL product stream will normally have a temperature in the range of 100 to 200°C, and a pressure in the range of 1 to 50 bar.The aqueous phase comprises water, water-soluble organics such as alcohols, ketones, phenols, organic acids and dissolved salts. Recirculation of all or parts of this mixture reduces makeup alkali metal salts, and the water-soluble organics are beneficial during pre-treatment and conversion in the Feedstock vessel (2). In particular, it may contribute to producing a pumpable slurry. The aqueous phase exiting from the Phase Separator (4) can have a temperature in the range of 60 to 130°C, such as 80 to 100°C, such as around 90°C, and it can have a pH in the range of 7.5 to 10, such as 8 to 9.Secondary separators can also be implemented for further purification. Finally, the aqueous phase and/or the oil phase may be partly recycled to the Feedstock (1) vessel.pH-regulation unitA pH-regulation unit (5) is fluidly connected to the Phase Separator (4) and the Feedstock (1) vessel, thus allowing a calcium source such as CaO (s), Ca(OH)2 (s) or Ca(OH)2 (aq) etc. to be added to the aqueous phase to be recycled. This will increase the pH. It also allows precipitation of CaCO3 (s) from the aqueous phase to be recycled. By providing such CaCO3 (s) to a Calciner (6), a calcination loop can be formed where the generated CaO can be directly or indirectly (e.g. after dissolving in water or via a Lime slaker (7)) provided to the aqueous phase to be recycled. The temperature of the mixture in the pH-regulation unit (5) can be in the range of 20 to 200 °C, such as 50 to 120°C, with operating pressure higher than saturation pressure of water at the operation temperature. The pH-regulation unit (5) can contain means for mixing aqueous solutions with suspended particles, other aqueous solutions or slurries. Such means include impellers, baffles and any other suitable equipment contributing to thorough mixing. The pH-regulation unit (5) can also comprise means for solids separation facilitating filtering, settling etc. to separate CaCO3 from the aqueous phase.CalcinerCalcination can be carried out in furnaces or reactors referred to Calciners.The systems and methods disclosed herein can comprise or involve a Calciner (6) in fluid connection with the pH-regulation unit (5), wherein the Calciner (6) is configured to provide the calcium source to the pH-regulation unit (5), and wherein the pH-regulation unit (5) is configured to provide calcium carbonate to the Calciner (6). The calcium carbonate can preferably be in solid form and provided directly. Alternatively, the calcium carbonate can be in solid form and provided indirectly.Calciners can have various designs including shaft furnaces, rotary kilns, multiple hearth furnaces, and fluidized bed reactors. They are suitable for a decomposition process that occurs at 525 to 1050°C and the chemical reaction can be represented: CaCO3(s) → CaO(s) CO2(g). The CO2 (g) can be captured and/or sequestered as desired, while the CaO can be directly supplied as powder to the aqueous phase to be recycled. Alternatively, the CaO can react with water to obtain a powder, slurry or suspension comprising Ca(OH)2 to be supplied to the aqueous phase to be recycled. Another alternative involves dissolving Ca(OH)2 in water to obtain an alkaline aqueous solution to be supplied to the aqueous phase to be recycled.Lime slakerThe systems and methods disclosed herein can comprise a Lime slaker (7) configured to receive CaO from a Calciner (6), mix it with a source of water, and subsequently for providing Ca(OH)2 to the pH-regulation unit (5).Water recovery unitA Water recovery unit (8) can be configured to evaporate water from the aqueous phase (9) to be recycled back to the Feedstock vessel (2) or Biomass vessel (2a) as appropriate. The aqueous phase can thus be concentrated while purified water may be directed for other uses. Such Water recovery units (8) can be installed either upstream or downstream from the pH-regulation unit.A bleed of 5–35% of the aqueous phase can be beneficial for preventing buildup of unwanted trace components such as chloride. The bleed can be further treated and purified to dischargeable or recyclable water quality.General equipmentThe systems disclosed herein may of course comprise valves, sensors, heaters, pumps, piping, filters etc. as needed for establishing a viable industrial process , preferably a continuous process. Such general and ubiquitous equipment is not necessarily described herein in detail because it is so well known for skilled persons within this field.Unless specifically defined herein, all technical and scientific terms used have the same meaning as commonly understood by a skilled person.It is to be noted that the term “a” or “an” entity refers to one or more of that entity; for example, “a reactor”, is understood to represent one or more reactors. As any skilled person will understand, a system comprising a Biomass vessel (2a) may of course comprise numerous such Biomass vessel (2a)s and other types of vessels as well. As such, the terms “a” (or “an”), “one or more”, and “at least one” can be used interchangeably herein. As used herein, the term “in fluid connection”, means that two or more components of a device/system or of a process/method are connected such that they may exchange a fluid between them. The fluid connection may be obtained by the components being in direct contact with each other or by the components being spaced apart from each other. In the latter case, the components will be connected to each other by a conduit, pipeline or in any other way known to the skilled person being suited for transporting a fluid between the components.All publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety. In case of conflict, the present specification, including definitions, will prevail.Where a numerical limit or range is stated herein, the endpoints are included. Also, all values and sub ranges within a numerical limit or range are specifically included as if explicitly written out.Headings have been used for organizational purposes and should not be construed as limiting the subject-matter herein.Example 1An aqueous phase sample was retrieved from an HTL phase separator, wherein the HTL process was executed at a feedstock flow of 1414 kg/hr containing 20% biomass of wood (dry basis), 0.2% CMC, 0.5% K2CO3 and 2% NaOH, 20% recycled oil, and 37.5% recycled upconcentrated aqueous phase on weight basis. The feedstock was reacted at around 350°C and 280 bar. The HTL product stream was provided to a Phase Separator (4) and separated to solids, gas, oil and aqueous products. A 50 mL aqueous phase sample was retrieved from the phase separated aqueous stream and analysis was collected for pH regulation batch experiment. Lime was added as 0.35 g of Ca(OH)2 and reacted for 4 hours at a temperature of 80°C. Sample was filtered and aqueous phase and solids was separated. Analysis of aqueous phase after reaction and filtration was conducted. The results are shown in Table 1.Table 1 – Results of experiment described in Example 1Received solids from filtration weighed 1.5 g, 0.5 g. With a 43% mass increase compared to lime added.Example 2An aqueous phase sample was retrieved from an HTL phase separator, wherein the HTL process was executed at a feedstock flow of 1160 kg/hr containing 20% biomass of wood (dry basis), 0.2% CMC, 1.1% K2CO3 and 2% NaOH, 18% recycled oil, and 40% recycled upconcentrated aqueous phase on weight basis. The feedstock was reacted at around 350°C and 280 bar. The HTL product stream was provided to a Phase Separator and separated to solids, gas, oil and aqueous products. A 50 mL aqueous phase sample was retrieved from the phase separated aqueous stream and analysis was collected for pH regulation batch experiment. Lime was added as 3 g of CaO and reacted for 1 hour. Sample was filtered and aqueous phase and solids was separated. Analysis of aqueous phase after reaction and filtration was conducted. The results are shown in Table 2.Table 2 – Results of experiment described in Example 2Solids received from filtration weighed 7.3 g, 4.7 after drying, and 2.7 after calcination at 775°CExample 3A 45 mL aqueous phase sample from same phase separated aqueous phase obtained in Example 2 was retrieved. Analysis was collected for pH regulation batch experiment. Lime was added as 2.7 g of acquired calcined precipitate from Example 1 and reacted for 1 hour. Sample was filtered and aqueous phase and solids was separated. Analysis of aqueous phase after reaction and filtration was conducted. The results are shown in Table 3. Table 3 – Results of experiment described in Example 3Solids received from filtration weighed 5.8 g, 4.2 after drying, and 2.4 g after calcination at 775°C.
Claims
CLAIMS1. A system for alkaline hydrothermal liquefaction of a carbon-containing Feedstock (1), comprisinga) a Feedstock vessel (2) comprising an inlet for carbon-containing Feedstock (1) and an outlet for providing an alkaline feed mixture comprising the carbon-containing Feedstock (1),b) a hydrothermal liquefaction (HTL)-reactor comprising an inlet for the alkaline feed mixture comprising the carbon-containing Feedstock (1) and an outlet for an HTL product stream,c) a Phase Separator (4) comprising an inlet for the HTL product stream and an outlet for an aqueous phase and an outlet for an oil phase, d) a pH-regulation unit (5) comprising an inlet for a calcium source and an outlet for calcium carbonate,wherein the system is configured to recycle aqueous product phase from the Phase Separator (4) back to the Feedstock vessel (2) via the pH-regulation unit (5).2. A system according to claim 1, comprising a Calciner (6) in fluid connection with the pH-regulation unit (5), wherein the Calciner (6) is configured to provide the calcium source to the pH-regulation unit (5), and wherein the pH-regulation unit (5) is configured to provide calcium carbonate to the Calciner (6).3. A system according to claim 1 or 2, wherein the carbon-containing Feedstock (1) comprises biomass, mixtures of biomass and plastic, lignite, black liquor, industrial waste and/or municipal waste.4. A system according to any one of claims 1 to 3, wherein the carbon-containing Feedstock (1) comprises lignocellulosic biomass.5. A system according to any one of claims 2 to 4, wherein the Calciner (6) is configured to, directly or indirectly, provide CaO and/or Ca(OH)2 into the pH-regulation unit (5).6. A system according to any one of claims 1 to 5, wherein the pH-regulation unit (5) is configured to extract CaCO3 from the aqueous phase to be recycled.7. A system according to any one of claims 1 to 6, wherein the calcium source is in the form of CaO particles.8. A system according to any one of claims 1 to 6, wherein the calcium source is in the form of Ca(OH)2 particles, Ca(OH)2 slurry or an aqueous solution comprising dissolved Ca(OH)2.9. A system according to any one of claims 2 to 8, further comprising a Lime slaker (7) configured to receive CaO from the Calciner (6) and for providing Ca(OH)2 to the pH-regulation unit (5).10. A system according to claim any one of claims 2 to 9, configured for allowing CaO and/or Ca(OH)2 to increase the pH of the aqueous phase and for allowing CaCO3 to be precipitated and provided to the Calciner (6).11. A system according any one of claims 1 to 10, configured for performing HTL at a temperature in the range of 250 °C to 450 °C and at a pressure in the range of 150 to 400 bar.12. A system according any one of claims 1 to 11, involving Calciner solids bleed and CaO makeup for mitigating accumulated impurity of the recycled CaO and CaCO3.13. A method for alkaline hydrothermal liquefaction of a carbon-containing Feedstock (1) comprising the stepsa) providing an aqueous feed mixture with alkaline pH comprising a carboncontaining Feedstock,b) subjecting the aqueous feed mixture in step a) to hydrothermal liquefaction for providing an HTL product stream,c) separating an aqueous product phase and an oil product phase from the HTL product stream in step b),d) recirculating and mixing all or a fraction of the aqueous product phase from step c) into to the aqueous feed mixture in step a), ande) adding a calcium source to the recirculating aqueous product phase and extracting solid CaCO3 formed thereof upstream of said mixing of the aqueous product phase in step d).14. The method according to claim 13, wherein the carbon-containing Feedstock (1) comprises biomass, mixtures of biomass and plastic, lignite, black liquor, industrial waste and/or municipal waste.15. The method according to claim 13, wherein carbon-containing Feedstock (1) comprises lignocellulosic biomass.16. The method according to any one of claims 13 to 15, wherein the aqueous mixture with alkaline pH comprising a carbon-containing Feedstock (1) also contains a source of carbonate ions, such as dissolved K2CO3.17. The method according to any one of claims 13 to 16, wherein CaCO3 is precipitated from the aqueous phase in step e) and provided to a Calciner (6) which directly or indirectly supplies CaO or Ca(OH)2 into the aqueous phase in step e).18. The method according to any one of claims 13 to 17, wherein the HTL is performed at a temperature in the range of 250 °C to 374 °C and at a pressure in the range of 150 to 400 bar.19. Use of a Calciner (6) for directly or indirectly providing CaO or Ca(OH)2 into an aqueous phase recycled from a Phase Separator (4) to a Feedstock vessel (2) in an alkaline HTL-process, wherein CaCO3 is precipitated from the recycled aqueous phase and provided to the Calciner (6).
Drawings

Priority

No priority

Patent classes

IPC classesC10G 1/00C10G 3/00CPC classesC10G 1/00C10G 3/00

Citations

EP 4306620 A1 (A1)US 2021284916 A1 (A1)

Applicants, owners and inventors

Applicants
SILVA BIOFUEL AS
SILVA BIOFUEL AS

Org. number: 936672965

Name and address are automatically synchronized with the Brønnøysund Register Centre.

Open in The Brønnøysund Register Centre
c/o Joakim Sværen Filtvetveien 42 3480 FILTVET NO (ASKER Municipality, Akershus county)Org. number: 936672965Inventors
Claus Uhrenholt Jensen
Katrineborgvej 6 9310 VODSKOV DK
Anders Tagmose Lundsfryd
Tagensvej 2E 9000 AALBORG DK

Agent

ACAPO ONSAGERS AS
ACAPO ONSAGERS AS

Org. number: 932214636

Name and address are automatically synchronized with the Brønnøysund Register Centre.

Open in The Brønnøysund Register Centre
Edvard Griegs vei 1 5059 BERGEN NO (BERGEN Municipality, Vestland county)
Org. number: 932214636
Reference: P29814NO00

Status history

Payment history

Oppositions and appeals

No oppositions or appeals

Administrative limitation

No administrative limitation

Liens and licences

No liens or licenses registered

Gazette entries

No Gazette entries foundOnly events from 2024.03.04 and onwards are shown.