WO1994019119A1 - Method and plant for biological treatment of waste materials - Google Patents
Method and plant for biological treatment of waste materials Download PDFInfo
- Publication number
- WO1994019119A1 WO1994019119A1 PCT/DK1994/000066 DK9400066W WO9419119A1 WO 1994019119 A1 WO1994019119 A1 WO 1994019119A1 DK 9400066 W DK9400066 W DK 9400066W WO 9419119 A1 WO9419119 A1 WO 9419119A1
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- WO
- WIPO (PCT)
- Prior art keywords
- waste
- organic
- biogas
- receiving
- industrial waste
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000002699 waste material Substances 0.000 title claims abstract description 20
- 239000010791 domestic waste Substances 0.000 claims abstract description 25
- 239000002440 industrial waste Substances 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 33
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 12
- 229930195729 fatty acid Natural products 0.000 claims description 12
- 239000000194 fatty acid Substances 0.000 claims description 12
- 150000004665 fatty acids Chemical class 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 8
- 239000010802 sludge Substances 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 238000005342 ion exchange Methods 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 239000000835 fiber Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000010815 organic waste Substances 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 244000005700 microbiome Species 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 150000002632 lipids Chemical class 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 4
- 239000002689 soil Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 150000001720 carbohydrates Chemical class 0.000 claims description 3
- 235000014633 carbohydrates Nutrition 0.000 claims description 3
- 210000003608 fece Anatomy 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000010871 livestock manure Substances 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 102000004169 proteins and genes Human genes 0.000 claims description 3
- 108090000623 proteins and genes Proteins 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000002361 compost Substances 0.000 claims description 2
- 229910052631 glauconite Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 1
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 claims 1
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000008235 industrial water Substances 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 230000031018 biological processes and functions Effects 0.000 abstract description 4
- 230000001580 bacterial effect Effects 0.000 description 4
- 239000003337 fertilizer Substances 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000009280 upflow anaerobic sludge blanket technology Methods 0.000 description 4
- 241001465754 Metazoa Species 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 230000020477 pH reduction Effects 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 238000006356 dehydrogenation reaction Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 241001072332 Monia Species 0.000 description 1
- 230000000789 acetogenic effect Effects 0.000 description 1
- 230000002053 acidogenic effect Effects 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- -1 ammonia ions Chemical class 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000003134 recirculating effect Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B1/00—Dumping solid waste
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F17/00—Preparation of fertilisers characterised by biological or biochemical treatment steps, e.g. composting or fermentation
- C05F17/10—Addition or removal of substances other than water or air to or from the material during the treatment
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F17/00—Preparation of fertilisers characterised by biological or biochemical treatment steps, e.g. composting or fermentation
- C05F17/40—Treatment of liquids or slurries
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F17/00—Preparation of fertilisers characterised by biological or biochemical treatment steps, e.g. composting or fermentation
- C05F17/70—Controlling the treatment in response to process parameters
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M21/00—Bioreactors or fermenters specially adapted for specific uses
- C12M21/04—Bioreactors or fermenters specially adapted for specific uses for producing gas, e.g. biogas
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M41/00—Means for regulation, monitoring, measurement or control, e.g. flow regulation
- C12M41/30—Means for regulation, monitoring, measurement or control, e.g. flow regulation of concentration
- C12M41/32—Means for regulation, monitoring, measurement or control, e.g. flow regulation of concentration of substances in solution
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M45/00—Means for pre-treatment of biological substances
- C12M45/02—Means for pre-treatment of biological substances by mechanical forces; Stirring; Trituration; Comminuting
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M45/00—Means for pre-treatment of biological substances
- C12M45/03—Means for pre-treatment of biological substances by control of the humidity or content of liquids; Drying
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M45/00—Means for pre-treatment of biological substances
- C12M45/04—Phase separators; Separation of non fermentable material; Fractionation
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M47/00—Means for after-treatment of the produced biomass or of the fermentation or metabolic products, e.g. storage of biomass
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M47/00—Means for after-treatment of the produced biomass or of the fermentation or metabolic products, e.g. storage of biomass
- C12M47/02—Separating microorganisms from the culture medium; Concentration of biomass
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
- Y02P20/145—Feedstock the feedstock being materials of biological origin
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/40—Bio-organic fraction processing; Production of fertilisers from the organic fraction of waste or refuse
Definitions
- the invention is based on the use of a low content of dry matter, 10-15 % in the feed material and 2-8 % in the reactor tank, in order to ensure an optimum contact between the substrate and the micro-organisms.
- the method comprises special measures for pre-treatment of the waste material and the separation of plastic bags from the solid organic household waste.
- the plant for carrying out the method is provided with a receiving station, cf. Fig. 2, in which sub-atmospheric pressure and bio-filters are used to prevent problems with the smell from the biogas plant.
- the invention also comprises the use of an ion-exchange apparatus on the basis of a soil mineral for removing ammonia from the residual water.
- the plant according to the invention is rather simple and is based on experiences from plants used for biological treatment of animal manure together with household and industrial waste in Denmark.
- the plant is run with a low dry-matter content (3-8%) in the reactor, making the plant cheaper and mechanically less complicated than the plants referred to above.
- the process is divided into the following steps: a) hydrolysis and acidogenic dehydrogenation, b) acetogenic dehydrogenation, and c) methanogenesis.
- the va- rious steps are carried out by various bacterial populations.
- the effectiveness of the process is to a large extent deter- mined by the size and composition of the bacterial biomass.
- the methane potential of the waste materials depends on the composition of the organic content, lipids especially being of importance with a view to a higher methane yield.
- the theoretical methane yields for organic materials are 415, 504 and 1014 ml CH 4 /g respectively of organic material for carbohydrates, proteins and lipids respectively.
- the invention is based upon a biological process, in which solid organic household waste and organic industrial waste are processed together.
- the organic industrial waste is used for optimizing the composition of the feed material with regard to carbohydrates, proteins and lipids.
- the or ⁇ ganic industrial waste may possibly also be used for reducing the dry-matter content in the solid organic household waste, and it may also be utilized for preventing problems with am ⁇ monia inhibition of the process.
- Water resulting from the concentration of the biologically processed material to form a fertilizer product may also be recycled and used for regulating the dry-matter content in the biogas reactor.
- the invention also relates to starting-up of biogas reactors for processing organic waste materials, such as animal ma ⁇ nure, organic industrial waste and/or solid household waste by the use of granular sludge.
- organic waste materials such as animal ma ⁇ nure, organic industrial waste and/or solid household waste.
- the scope of the invention also encompasses the use of granular sludge to increase the yield, e.g. the production of gas from biogas reactors.
- the starting-up of a biogas reactor is frequently a slow process, and months may pass before the process is stabi ⁇ lized. During this period, the biogas plant will not produce as much biogas as under optimum conditions.
- biolo- gically processed material from another biogas reactor preferably operating with the same substrate, the requisite starting-up time will be considerably shortened. It has, however, proved possible to shorten the starting-up time even further by using granular sludge from a UASB reactor ("Up-flow Anaerobic Sludge Blanket") for processing waste water.
- Granular sludge consists of anaerobic micro-organisms, mu ⁇ tually immobilized to form large bacterial lumps with a dia ⁇ meter from 0.5 to several mm. They are used as catalysts in the above-mentioned UASB reactor.
- the heavy bacterial lumps (the granulae) may be produced in a UASB reactor by con ⁇ trolling the linear flow velocity in the plant and in this manner select the micro-organisms being able to immobilize on each other.
- New UASB reactors are frequently started-up by using pre-formed granulae of this kind, for which reason these are often sent from one place to another.
- the invention also relates to monitoring or periodic measure ⁇ ment of the concentration of the volatile fatty acids in plants comprising biological reactors.
- a special application consists in the control and regulating of biogas reactors processing organic waste and waste water and other types of biomass.
- the equipment comprises a pre-treatment section, in which the soluble phase is separated from the particles in the material, and this section consists of a ceramic filter with very fine particles.
- a powerful constant flow through the filter keeps the inside of the ceramic filter clean.
- the pressure in the filter must be low in order to enable the filtrate to diffuse slowly through the filter material. After this, the filtrate is diluted and acidified.
- the detector used is a gas chromatograph equipped with a flame ionization detector.
- the injection into the gas chro ⁇ matograph is carried out by means of an injection valve.
- the data relating to the concentrations of the individual volatile fatty acids obtained from the gas chromatograph are read into a computer, in which they can be used for controlling and regulating the biogas reactor.
- Control and regulation of the biological processes in biogas reactors normally occurs by measuring the gas production of the biogas process, at times supplemented with data relating to the composition of the gas. Such measurements will, how ⁇ ever, provide little information about the state of the biological process. Trials have shown that measurements of the concentration of volatile fatty acids in the biogas reactor may be used for judging the state of the process and predict instability in the process. It is believed that measurements of changes in the concentrations of the in- dividual fatty acids in the biogas reactor, combined with measurements of the gas production, will be valuable tools for devising a programme for controlling the feed to biogas reactors with a view of optimizing the production of biogas. At the present time, there exists no equipment for constantly monitoring volatile fatty acids in complex substrates, such as animal manure and other types of waste material.
- Fig. 1 being an overall illustration of the plant
- Fig. 2 being a partial illustration at an enlarged scale of the plant shown in Fig. 1 and showing the receiving station for solid organic household waste and possibly coarse-fibre organic industrial waste
- Fig. 3 illustrating the principle of constant monitoring of the concentration of volatile fatty acids in the reactor and the use of the measurement results for regulating the operation of the reactor.
- Fig. 1 shows in diagram form the principles of the complete plant.
- the part of the plant, in which the waste products are re ⁇ ceived, consists of separate containers for household waste and various types of organic industrial waste.
- the household waste is received in a special sub-section in the form of a receiving station 1, comprising equipment for receiving solid organic household waste from a tipping lorry, and constructed with a view to reducing the smell problems, cf. Fig. 2.
- Said equipment consists of a flexible rubber bellows lb adapted to be secured to the vehicle during the tipping operation, a receiving pit la with a sliding cover lc, a suction ventilator Id for maintaining a reduced pres ⁇ sure in the receiving pit la, as well as a bio-filter le for removing smelling substances from the air.
- the waste material is transferred from the receiving pit la to the receiving container 2 shown in Fig. 1, this container being equipped with special agitating means, adapted to open the bags containing the household waste.
- the solid organic household waste is mixed with 25- 50 % biologically processed material from an anaerobic reac ⁇ tor 7 for carrying out a pre-hydrolysis, and with some of the organic industrial waste, possibly also recycled water, in order to change the dry-matter content to 10-15 %.
- the material is pumped to a drum screen 4, in which the material is pressed through holes with a size of 8 mm.
- Plastic material and other mate ⁇ rials with sizes larger than 8 mm are removed as a separate fraction for incineration.
- the waste material is passed through a fine-comminuting apparatus 5, in which it is cut into pieces with a size of 1-2 mm.
- the organic industrial waste material consists of coarse waste material with a high dry-matter content, it is received in the receiving station 1 for household waste, while if it consists of more fine waste material, i.e. with a low dry-matter content and no coarse materials, it is received in separate storage containers 3.
- the reactor system comprises a fully stirred reactor con ⁇ tainer 7, in which the hydraulic retention time is from 10 to 15 days.
- the biogas process is run at a ther- mophilic temperature (55° C).
- waste material is pumped to the reactor 7 between six and eight times per day. When water has been added, no ma ⁇ terials are removed from the reactor during the first two hours, so as to ensure a proper thermal sanitation of the anaerobic process.
- the retention time and/or the composition of the waste ma ⁇ terial supplied to the plant will be regulated on the basis of the specific concentrations of volatile fatty acids in the reactor, thus ensuring a maximum stability of the pro- duction of biogas and the maximum possible yield of methane for each ton of organic material supplied to the plant.
- the residual material may either be used directly on agricultural soil as a fertilizer, or it may be concentrated in a filter press 9 to a dry-matter content of approximately 30-35 %. The concentrated residual material may find further use as a valuable fertilizer pro ⁇ duct.
- the residual water may be treated in an ion-exchange ap- paratus 8 based on the use of the soil mineral glauconite, in which the concentration of ammonia ions will be reduced.
- the ammonia-containing mine ⁇ ral may be used as a fertilizer, and a part of the water could be used for recycling to the biogas reactor 7 without any risk of ammonia inhibition of the biogas process.
- Residual substances in the waste water possibly having a biological oxygen demand can be removed in an aerobic fixed-film bio-filter 10.
- Fig. 3 shows the measuring and control functions, liquid from the reactor 7 being extracted through a ceramic filter 11, the inlet side of which is maintained clean by constant rinsing, and from which the liquid, through a dilution and acidification section 12 and an injection valve 13, is intro ⁇ lodged into a gas chromatograph 14, the latter on the basis of these measurements and further data relating to the pro ⁇ cess controlling the supply to the reactor 7 and the dilution and/or acidification process in the section 12.
- a gas chromatograph 14 the latter on the basis of these measurements and further data relating to the pro ⁇ cess controlling the supply to the reactor 7 and the dilution and/or acidification process in the section 12.
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- Bioinformatics & Cheminformatics (AREA)
- Wood Science & Technology (AREA)
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Abstract
In a method of anaerobic processing of solid organic household waste and/or organic industrial waste with a high dry-matter content, the novel feature is that prior to the waste materials being introduced in the biogas reactor (7), liquid or semi-liquid organic industrial waste is added in a quantity producing a percentage of organic dry matter (''volatile solids'') of approximately 15 %. By proceeding in this manner, a dry-matter content, optimum with regard to the biological process, is achieved, without it being necessary to add e.g. water.
Description
METHOD AND PLANT FOR BIOLOGICAL TREATMENT OF WASTE MATERIALS.
At the present time, most of the biogas processes having been developed for treating solid organic household waste are either "dry" processes being run with a high content of dry matter, e.g. the VALORGA process (Valorga Process S.A. ) and the DRANCO process (Organic Waste Systems N.V.), being run with a dry-matter content of 24-28 % in the reactor tank, or a complicated process with two or more stages desig- nated the BTA process, in which the material is separated into a liquid phase and a solid phase, the latter being subjected to alkaline hydrolysis.
With regard to the "dry" processes, the major problems in the known processes for treating organic household waste consist in that the contact between the organic substrate and the micro-organisms is not optimum, for which reason there may be a reduced production of biogas for each kilogram of volatile solids supplied to the plant. Further, recycling of the material frequently causes the hydraulic retention time in the plant to be prolonged. The processes with two or more stages, such as the BTA process, require mechanically complicated plant that is very vulnerable from a mechanical point of view.
There are other serious problems in connection with the separation of inactive materials, such as plastic bags, from the material fed to reactor in order to prevent contamination of the biologically treated material (compost), prevention of problems with smell in the section for receiving the solid organic household waste, and post-treatment of the residual water with a view to recirculating this water without the risk of ammonia inhibition of the biogas processes and in order to ensure a good quality of the discharged water.
Apart from the requisite pre-treatment of the solid organic household waste, the method according to the invention is relatively simple, for which reason it may be considered as being relatively cheap.
The invention is based on the use of a low content of dry matter, 10-15 % in the feed material and 2-8 % in the reactor tank, in order to ensure an optimum contact between the substrate and the micro-organisms.
The method comprises special measures for pre-treatment of the waste material and the separation of plastic bags from the solid organic household waste.
The plant for carrying out the method is provided with a receiving station, cf. Fig. 2, in which sub-atmospheric pressure and bio-filters are used to prevent problems with the smell from the biogas plant.
The invention also comprises the use of an ion-exchange apparatus on the basis of a soil mineral for removing ammonia from the residual water.
Mechanically, the plant according to the invention is rather simple and is based on experiences from plants used for biological treatment of animal manure together with household and industrial waste in Denmark. The plant is run with a low dry-matter content (3-8%) in the reactor, making the plant cheaper and mechanically less complicated than the plants referred to above.
Traditionally, the process is divided into the following steps: a) hydrolysis and acidogenic dehydrogenation, b) acetogenic dehydrogenation, and c) methanogenesis. The va- rious steps are carried out by various bacterial populations. The effectiveness of the process is to a large extent deter-
mined by the size and composition of the bacterial biomass. The methane potential of the waste materials depends on the composition of the organic content, lipids especially being of importance with a view to a higher methane yield. The theoretical methane yields for organic materials are 415, 504 and 1014 ml CH4/g respectively of organic material for carbohydrates, proteins and lipids respectively.
The invention is based upon a biological process, in which solid organic household waste and organic industrial waste are processed together. The organic industrial waste is used for optimizing the composition of the feed material with regard to carbohydrates, proteins and lipids. The or¬ ganic industrial waste may possibly also be used for reducing the dry-matter content in the solid organic household waste, and it may also be utilized for preventing problems with am¬ monia inhibition of the process.
Water resulting from the concentration of the biologically processed material to form a fertilizer product may also be recycled and used for regulating the dry-matter content in the biogas reactor.
The invention also relates to starting-up of biogas reactors for processing organic waste materials, such as animal ma¬ nure, organic industrial waste and/or solid household waste by the use of granular sludge. The scope of the invention also encompasses the use of granular sludge to increase the yield, e.g. the production of gas from biogas reactors.
The starting-up of a biogas reactor is frequently a slow process, and months may pass before the process is stabi¬ lized. During this period, the biogas plant will not produce as much biogas as under optimum conditions. By using biolo- gically processed material from another biogas reactor, preferably operating with the same substrate, the requisite
starting-up time will be considerably shortened. It has, however, proved possible to shorten the starting-up time even further by using granular sludge from a UASB reactor ("Up-flow Anaerobic Sludge Blanket") for processing waste water. Thus, it has proved possible to start a biogas reactor by using 1-10 % by volume of granular sludge and then star¬ ting to feed the reactor with material as if the plant were in full operation. By measuring the production of gas and the concentration of volatile fatty acids in the reactor, the feed rate may adjusted according to need.
Granular sludge consists of anaerobic micro-organisms, mu¬ tually immobilized to form large bacterial lumps with a dia¬ meter from 0.5 to several mm. They are used as catalysts in the above-mentioned UASB reactor. The heavy bacterial lumps (the granulae) may be produced in a UASB reactor by con¬ trolling the linear flow velocity in the plant and in this manner select the micro-organisms being able to immobilize on each other. New UASB reactors are frequently started-up by using pre-formed granulae of this kind, for which reason these are often sent from one place to another.
Further, it has been shown that adding granular sludge to a biogas reactor in operation will lead to an improved yield, such as a greater production of gas and a lower concentration of volatile fatty acids in the effluent. These findings were especially pronounced in cases when the retention time of the reactor was short.
The invention also relates to monitoring or periodic measure¬ ment of the concentration of the volatile fatty acids in plants comprising biological reactors. A special application consists in the control and regulating of biogas reactors processing organic waste and waste water and other types of biomass. The equipment comprises a pre-treatment section, in which the soluble phase is separated from the particles
in the material, and this section consists of a ceramic filter with very fine particles. A powerful constant flow through the filter keeps the inside of the ceramic filter clean. The pressure in the filter must be low in order to enable the filtrate to diffuse slowly through the filter material. After this, the filtrate is diluted and acidified. The detector used is a gas chromatograph equipped with a flame ionization detector. The injection into the gas chro¬ matograph is carried out by means of an injection valve. The data relating to the concentrations of the individual volatile fatty acids obtained from the gas chromatograph are read into a computer, in which they can be used for controlling and regulating the biogas reactor.
Control and regulation of the biological processes in biogas reactors normally occurs by measuring the gas production of the biogas process, at times supplemented with data relating to the composition of the gas. Such measurements will, how¬ ever, provide little information about the state of the biological process. Trials have shown that measurements of the concentration of volatile fatty acids in the biogas reactor may be used for judging the state of the process and predict instability in the process. It is believed that measurements of changes in the concentrations of the in- dividual fatty acids in the biogas reactor, combined with measurements of the gas production, will be valuable tools for devising a programme for controlling the feed to biogas reactors with a view of optimizing the production of biogas. At the present time, there exists no equipment for constantly monitoring volatile fatty acids in complex substrates, such as animal manure and other types of waste material.
In the following, the invention will be explained in more detail with reference to the plant for treatment of solid organic household waste and organic industrial waste with a view to producing biogas shown in the drawing in a highly
diagrammatic and simplified manner,
Fig. 1 being an overall illustration of the plant,
Fig. 2 being a partial illustration at an enlarged scale of the plant shown in Fig. 1 and showing the receiving station for solid organic household waste and possibly coarse-fibre organic industrial waste, and Fig. 3 illustrating the principle of constant monitoring of the concentration of volatile fatty acids in the reactor and the use of the measurement results for regulating the operation of the reactor.
Fig. 1 shows in diagram form the principles of the complete plant.
The part of the plant, in which the waste products are re¬ ceived, consists of separate containers for household waste and various types of organic industrial waste.
The household waste is received in a special sub-section in the form of a receiving station 1, comprising equipment for receiving solid organic household waste from a tipping lorry, and constructed with a view to reducing the smell problems, cf. Fig. 2. Said equipment consists of a flexible rubber bellows lb adapted to be secured to the vehicle during the tipping operation, a receiving pit la with a sliding cover lc, a suction ventilator Id for maintaining a reduced pres¬ sure in the receiving pit la, as well as a bio-filter le for removing smelling substances from the air.
The waste material is transferred from the receiving pit la to the receiving container 2 shown in Fig. 1, this container being equipped with special agitating means, adapted to open the bags containing the household waste. In this con¬ tainer, the solid organic household waste is mixed with 25- 50 % biologically processed material from an anaerobic reac¬ tor 7 for carrying out a pre-hydrolysis, and with some of
the organic industrial waste, possibly also recycled water, in order to change the dry-matter content to 10-15 %.
From the receiving container 2 the material is pumped to a drum screen 4, in which the material is pressed through holes with a size of 8 mm. Plastic material and other mate¬ rials with sizes larger than 8 mm are removed as a separate fraction for incineration. On its way to a storage container 6, the waste material is passed through a fine-comminuting apparatus 5, in which it is cut into pieces with a size of 1-2 mm.
If the organic industrial waste material consists of coarse waste material with a high dry-matter content, it is received in the receiving station 1 for household waste, while if it consists of more fine waste material, i.e. with a low dry-matter content and no coarse materials, it is received in separate storage containers 3.
The reactor system comprises a fully stirred reactor con¬ tainer 7, in which the hydraulic retention time is from 10 to 15 days. In order to ensure a good hygienic quality in the residual product, the biogas process is run at a ther- mophilic temperature (55° C). From the storage containers 3, waste material is pumped to the reactor 7 between six and eight times per day. When water has been added, no ma¬ terials are removed from the reactor during the first two hours, so as to ensure a proper thermal sanitation of the anaerobic process.
The retention time and/or the composition of the waste ma¬ terial supplied to the plant will be regulated on the basis of the specific concentrations of volatile fatty acids in the reactor, thus ensuring a maximum stability of the pro- duction of biogas and the maximum possible yield of methane for each ton of organic material supplied to the plant.
After the biological processing, the residual material may either be used directly on agricultural soil as a fertilizer, or it may be concentrated in a filter press 9 to a dry-matter content of approximately 30-35 %. The concentrated residual material may find further use as a valuable fertilizer pro¬ duct.
The residual water may be treated in an ion-exchange ap- paratus 8 based on the use of the soil mineral glauconite, in which the concentration of ammonia ions will be reduced. After the ion-exchange process, the ammonia-containing mine¬ ral may be used as a fertilizer, and a part of the water could be used for recycling to the biogas reactor 7 without any risk of ammonia inhibition of the biogas process.
Residual substances in the waste water possibly having a biological oxygen demand can be removed in an aerobic fixed-film bio-filter 10.
Fig. 3 shows the measuring and control functions, liquid from the reactor 7 being extracted through a ceramic filter 11, the inlet side of which is maintained clean by constant rinsing, and from which the liquid, through a dilution and acidification section 12 and an injection valve 13, is intro¬ duced into a gas chromatograph 14, the latter on the basis of these measurements and further data relating to the pro¬ cess controlling the supply to the reactor 7 and the dilution and/or acidification process in the section 12.
LIST OF PARTS
I Receiving station la Receiving pit lb Rubber bellows lc Sliding cover Id Suction ventilator le Bio-filter If Hydraulic device 2 Receiving container
3 Storage containers
4 Drum screen
5 Fine-comminuting apparatus
6 Storage container 7 Anaerobic reactor, container
8 Ion-exchange apparatus
9 Filter press
10 Aerobic bio-filter
II Ceramic filter 12 Dilution and acidification section
13 Injection valve
14 Gas chromatograph
15 Computer
Claims
1. Method of anaerobic processing of organic waste materials from households and industry, characterized in a) that separate receiving sections are used, on the one hand for solid organic household waste and coarse-fibre organic industrial waste required to be comminuted, on the other hand for various types of liquid or semi-liquid organic industrial waste materials, b) that the solid organic household waste and/or the coarse-fibre organic industrial waste is/are mixed with biologically processed material from the biogas reactor in order to improve the pre-hydrolysis of these organic waste materials, c) that the dry-matter content in the solid organic household waste and/or the coarse-fibre organic in¬ dustrial waste is adjusted to approximately 15 % organic dry matter by mixing with liquid or semi-liquid organic industrial waste, d) that the residual water is post-treated by ion ex¬ change and aerobic bio-filtering, and e) that the process in the biogas reactor is regulated by adjusting the supply rates for the various waste materials on the basis of measurements of the con¬ centrations of certain volatile fatty acids.
2. Plant for carrying out the method according to claim 1, characterized by a receiving pit (la) for recei- ving solid organic household waste and coarse-fibre organic industrial waste, said pit being equipped with a flexible rubber membrane or bellows (lb) adapted to be secured to a vehicle, from which the material is tipped down into the receiving pit.
3. Plant according to claim 2, characterized in that the receiving pit (la) is equipped with a sliding cover (lc).
4. Plant according to claim 2 or 3, characterized in that the receiving pit (la) is adapted to be held under reduced pressure while waste materials are being received, e.g. by means of a suction ventilator (Id).
5. Plant according to any one or any of the claims 2-4, characterized in that the air aspirated from the recei- ving pit (la) is led through a bio-filter (le), said filter being filled with pieces of bark with a view to removing smelling substances from the air.
6. Plant according to any one or any of the claims 2-5, characterized in that the receiving pit (la) is equipped with a hydraulic device (If) for conveying the waste material from the receiving pit to a receiving container (2).
7. Plant according to claim 6, characterized in that the receiving container (2) comprises stirring or agitating means adapted to open and/or comminute plastic bags.
8. Method according to claim 1, characterized in that the solid organic household waste and/or the coarse-fibre organic industrial waste in the receiving con¬ tainer (2) is/are mixed with 25-50 % biologically processed material being recycled directly from the biogas reactor (7) with a view to improving the pre-hydrolysis of the solid organic household waste and/or the organic industrial waste.
9. Method according to claim 1, characterized in that the dry-matter content of the material in the receiving container (2) is adjusted to 15 % organic dry matter by adding liquid or semi-liquid organic industrial waste and/or water recycled from the ion exchange with a view to improving the contact between the substrate and the micro-organisms.
10. Plant according to any one or any of the claims 2-7, characterized by a drum screen (4) inserted between the receiving container (2) and the reactor (7), said drum screen being adapted to press the material through holes with a diameter of 8 mm and to separate out plastic and other coarse materials for incineration.
11. Plant according to claim 10, characterized by a fine-comminuting apparatus (5) adapted to cut the material into pieces of 1-2 mm.
12. Plant according to any one or any of the claims 2-7, 10 and 11, characterized by an ion-exchange apparatus (8) for reducing the ammonia concentration in the residual water from a separating unit (9), said ion exchange being based on the soil mineral glauconite exchanging NH4* with Na* or K* .
13. Method according to any one or any of the claims
1, 8 and 9, characterized in that the residual water pro¬ duced by concentrating compost materials is treated in a fixed-film aerobic bio-filter (10) with a view to removing residual substances having a biological oxygen demand from the residual water, before the latter is transferred to the environment.
14. Method according to any one or any of the claims 1, 8, 9 and 13, characterized in a) that gas-chromatographic measurements of the con¬ centrations of certain volatile fatty acids in the biogas reactor are carried out, b) that the rates, with which the various waste products are introduced into the biogas reactor, are regulated on the basis of the relative changes in the measured concentrations of acetate, iso-butyrate and butyrate, possibly also further relevant process parameters, such as the biogas production, the percentage of methane in the biogas, temperature, pH and ammonia concentration, whereas c) the selection of waste products with a view to regu¬ lating is based on the composition of the individual waste materials with regard to organic dry matter, lipids, proteins and carbohydrates.
15. The use of granular sludge in biogas reactors for processing organic waste materials, such as do¬ mestic-animal manure, organic industrial waste and solid organic household waste.
16. The use of a ceramic filter, an injection valve and a gas chromatograph for monitoring or periodically mea¬ suring the concentration of volatile fatty acids in biolo¬ gical reactors.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU61544/94A AU6154494A (en) | 1993-02-18 | 1994-02-17 | Method and plant for biological treatment of waste materials |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DK0190/93 | 1993-02-18 | ||
DK19093A DK19093A (en) | 1993-02-18 | 1993-02-18 | Process and plant for biological treatment of waste materials |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1994019119A1 true WO1994019119A1 (en) | 1994-09-01 |
Family
ID=8090793
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/DK1994/000066 WO1994019119A1 (en) | 1993-02-18 | 1994-02-17 | Method and plant for biological treatment of waste materials |
Country Status (3)
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AU (1) | AU6154494A (en) |
DK (1) | DK19093A (en) |
WO (1) | WO1994019119A1 (en) |
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0799812A1 (en) * | 1996-04-03 | 1997-10-08 | CT Umwelttechnik AG | Loading device for a fermentation plant |
EP0806404A2 (en) * | 1996-05-11 | 1997-11-12 | ML Entsorgungs- und Energieanlagen GmbH | Process for treating household waste and similar wastes |
WO2000039036A1 (en) * | 1998-12-23 | 2000-07-06 | Norsk Hydro Asa | Method for treatment of organic material in a two-step anaerobic biochemical reactor |
EP1508386A1 (en) * | 2003-08-13 | 2005-02-23 | Lassila & Tikanoja Oyj | Method for waste treatment |
WO2005047452A1 (en) * | 2003-11-07 | 2005-05-26 | Saroko Energy Systems Ltd | Bioreactor |
WO2008117096A2 (en) * | 2007-03-28 | 2008-10-02 | Fövárosi Csatornázási Müvek Zrt. | Method and apparatus for processing biomass waste |
WO2009071053A2 (en) * | 2007-12-07 | 2009-06-11 | Eltaga Licensing Gmbh | Device and method for producing biogas from organic matters |
WO2013006086A1 (en) * | 2011-07-06 | 2013-01-10 | МАНДЕЛЬШТАМ, Александр Семенович | Multi-functional biogas complex |
DE102011109430A1 (en) * | 2011-08-04 | 2013-02-07 | Hans Friedmann | Fermenter system and process for continuous fermentation |
ITTO20120456A1 (en) * | 2012-05-25 | 2013-11-26 | Vm Press Srl | PROCESS FOR THE PRODUCTION OF COMBUSTIBLE GAS FROM URBAN SOLID WASTE. |
US9328323B2 (en) | 2011-07-08 | 2016-05-03 | Aikan North America, Inc. | Systems and methods for digestion of solid waste |
RU2601973C1 (en) * | 2015-05-13 | 2016-11-10 | Владимир Васильевич Слюсаренко | Method cleaning oil sludge and oil contaminated soil |
CN113195120A (en) * | 2018-10-10 | 2021-07-30 | 格拉斯波特生物有限公司 | Treatment of organic waste |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AUPM452094A0 (en) * | 1994-03-17 | 1994-04-14 | University Of Queensland, The | Waste treatment plant and process |
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US4652374A (en) * | 1983-09-09 | 1987-03-24 | Gist-Brocades N.V. | Process for anaerobic fermentation of solid wastes in water in two phases |
GB2230004A (en) * | 1989-04-08 | 1990-10-10 | Pallett Ivor | Method for treating solid waste |
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1993
- 1993-02-18 DK DK19093A patent/DK19093A/en not_active Application Discontinuation
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1994
- 1994-02-17 WO PCT/DK1994/000066 patent/WO1994019119A1/en active Application Filing
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Cited By (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0799812A1 (en) * | 1996-04-03 | 1997-10-08 | CT Umwelttechnik AG | Loading device for a fermentation plant |
EP0806404A2 (en) * | 1996-05-11 | 1997-11-12 | ML Entsorgungs- und Energieanlagen GmbH | Process for treating household waste and similar wastes |
EP0806404A3 (en) * | 1996-05-11 | 1998-01-14 | ML Entsorgungs- und Energieanlagen GmbH | Process for treating household waste and similar wastes |
WO2000039036A1 (en) * | 1998-12-23 | 2000-07-06 | Norsk Hydro Asa | Method for treatment of organic material in a two-step anaerobic biochemical reactor |
US6551510B1 (en) | 1998-12-23 | 2003-04-22 | Norsk Hydro Asa | Method for treatment of organic material in a two-step anaerobic biochemical reactor |
EP1508386A1 (en) * | 2003-08-13 | 2005-02-23 | Lassila & Tikanoja Oyj | Method for waste treatment |
WO2005047452A1 (en) * | 2003-11-07 | 2005-05-26 | Saroko Energy Systems Ltd | Bioreactor |
US8100354B2 (en) | 2007-03-28 | 2012-01-24 | Veolia Bioenergy Europe Kft. | Apparatus for processing utility waste with biodegradable organic material content |
WO2008117096A2 (en) * | 2007-03-28 | 2008-10-02 | Fövárosi Csatornázási Müvek Zrt. | Method and apparatus for processing biomass waste |
WO2008117096A3 (en) * | 2007-03-28 | 2008-12-11 | Foevarosi Csatornazasi Muevek | Method and apparatus for processing biomass waste |
EA016173B1 (en) * | 2007-03-28 | 2012-02-28 | Веолиа Байоэнерджи Юроп Кфт. | Method and apparatus for processing utility waste with organic material content |
WO2009071053A3 (en) * | 2007-12-07 | 2009-12-03 | Eltaga Licensing Gmbh | Device and method for producing biogas from organic matters |
WO2009071053A2 (en) * | 2007-12-07 | 2009-06-11 | Eltaga Licensing Gmbh | Device and method for producing biogas from organic matters |
WO2013006086A1 (en) * | 2011-07-06 | 2013-01-10 | МАНДЕЛЬШТАМ, Александр Семенович | Multi-functional biogas complex |
US9328323B2 (en) | 2011-07-08 | 2016-05-03 | Aikan North America, Inc. | Systems and methods for digestion of solid waste |
DE102011109430A1 (en) * | 2011-08-04 | 2013-02-07 | Hans Friedmann | Fermenter system and process for continuous fermentation |
ITTO20120456A1 (en) * | 2012-05-25 | 2013-11-26 | Vm Press Srl | PROCESS FOR THE PRODUCTION OF COMBUSTIBLE GAS FROM URBAN SOLID WASTE. |
US20130316428A1 (en) * | 2012-05-25 | 2013-11-28 | Vm Press S.R.L. | Process for the production of fuel gas from municipal solid waste |
RU2601973C1 (en) * | 2015-05-13 | 2016-11-10 | Владимир Васильевич Слюсаренко | Method cleaning oil sludge and oil contaminated soil |
CN113195120A (en) * | 2018-10-10 | 2021-07-30 | 格拉斯波特生物有限公司 | Treatment of organic waste |
Also Published As
Publication number | Publication date |
---|---|
DK19093D0 (en) | 1993-02-18 |
DK19093A (en) | 1994-08-19 |
AU6154494A (en) | 1994-09-14 |
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