FRACTIONED SEPARATION OF VALUABLE SUBSTANCES FROM AQUEOUS MANY-COMPONENT MIXTURES

Abstract

The invention relates to a method for the fractioned separation of valuable substances from aqueous many-component mixtures such as aqueous wastes, sludges and sewage sludge under supercritical conditions. The invention also comprises valuable substance fractions that are enriched after the method according to the invention, more particularly phosphorous-containing and phosphorous- and ammonium-containing compounds such as fertilisers and synthesis gas as an energy source and as a valuable substance for the chemicals industry. The invention comprises devices for carrying out the methods. With the method and devices according to the invention, valuable substances can be completely recovered from wastes, sludges and sewage sludge and given a new use. The methods and devices are particularly suitable for recovering phosphorous and ammonium in the form of plant-available fertiliser, for recovering metals and heavy metals, for producing synthesis gas and for obtaining hydrogen from synthesis gas, i.e. for mobility.

Claims

1. A method for the fractional separation of valuable substances from an aqueous multicomponent mixture, comprising the compression of the aqueous multicomponent mixture to 25 to 35 MPa, heating of the compressed aqueous multicomponent mixture to 200 to 300 degrees Celsius and removal of a first valuable substance fraction, further heating of the compressed aqueous multicomponent mixture to 300 to 400 degrees Celsius and removal of a second valuable substance fraction, further heating of the compressed aqueous multicomponent mixture to 400 to 550 degrees Celsius and removal of a third valuable substance fraction.

2. The method according to claim 1, wherein the compressed aqueous multicomponent mixture, after the separation of the first, second and third valuable substance fractions is heated in a reactor with exclusion of oxygen for one to five minutes to a maximum of 700 degrees Celsius, forming a reaction product that comprises synthesis gas and water.

3. The method according to claim 2, wherein the reaction product is guided into a product line, and the product line containing the reaction product is guided through a heat exchanger in which thermal energy is transferred from the reaction product to compressed aqueous multicomponent mixture, which results in heating of the compressed aqueous multicomponent mixture to 400 to 550 degrees Celsius.

4. The method according to claim 2, wherein the reaction product is guided in a product line through a second heat exchanger in which thermal energy is transferred from the reaction product to compressed aqueous multicomponent mixture, which results in heating of compressed aqueous multicomponent mixture to 300 to 400 degrees Celsius.

5. The method according to claim 2, wherein the reaction product is guided in a product line through a further heat exchanger in which thermal energy is transferred from the reaction product to compressed aqueous multicomponent mixture, which results in heating of compressed aqueous multicomponent mixture to 200 to 300 degrees Celsius.

6. The method according to claim 1, wherein a precipitating agent is added to the compressed aqueous multicomponent mixture at a temperature of 400 to 550 degrees Celsius, and the third valuable substance fraction is separated and isolated.

7. The method according to claim 1, wherein a precipitating agent is added to the reaction product, and a fourth valuable substance fraction is separated and isolated.

8. The method according to claim 6, wherein the precipitating agent is selected from Mg.sup.2+ or Ca.sup.2+ or K.sup.+ or Mg.sup.2+ and Ca.sup.2+ or Mg.sup.2+ and K.sup.+ or Ca.sup.2+ and K.sup.+ or Mg.sup.2+ and Ca.sup.2+ and K.sup.+, and wherein the ions are used in the form of their salts.

9. The method according to claim 1, wherein the aqueous multicomponent mixture is selected from sewage sludge, organic waste, aqueous organic waste, industrial waste, municipal waste, animal waste, agricultural waste, garden waste, animal meal, vegetable waste, marc, fly ash, sewage sludge fly ash, food industry waste, drilling mud, sludge, waste from biogas plants, digestate, liquid manure and waste water.

10. A fertilizer comprising the third valuable substance fraction and/or of the fourth valuable substance fraction of claim 1.

11. An apparatus for carrying out the method according to claim 1, comprising a storage tank for receiving the aqueous multicomponent mixture, a feedstock line for guiding the aqueous multicomponent mixture, a cutting device for comminuting components of the aqueous multicomponent mixture, a pump for compressing the aqueous multicomponent mixture, at least three heat exchangers for heating the compressed aqueous multicomponent mixture in at least three steps to 550 degrees Celsius, at least three separators for separating the first to third valuable substance fractions valves for isolating the valuable substance fractions, a pump and line for precipitating agent for adding the precipitating agent into the third separator.

12. The apparatus according to claim 11, comprising at least one reactor including a superheater for producing the reaction product, a product line for guiding the reaction product, optionally a cooler for cooling the reaction product to below 50 degrees Celsius, at least one valve for expanding the reaction product, at least one separation vessel including a demister for separating the synthesis gas, a synthesis gas line for transferring the synthesis gas for further use, optionally a gas storage unit for temporarily storing the synthesis gas.

13. The apparatus according to claim 11, comprising a fourth separator, at least one pump and a line for precipitating agent for introducing the precipitating agent into the fourth separator for separating the fourth valuable substance fraction, optionally a further separator for separating the fourth valuable fraction, optionally a circulation water line, optionally a power generator.

14. An apparatus for carrying out a method according to claim 1, comprising a storage tank, a feedstock line connected to the storage tank for transporting the aqueous multicomponent mixture with exclusion of oxygen, a pump connected to the feedstock line for compressing the feedstock to 25 to 35 MPa, and guiding the feedstock line through a heat exchange for heating the compressed feedstock to 200 to 300 degrees Celsius and subsequently guiding the feedstock line through a separator for separating the first isolated valuable substance fraction, guiding the feedstock line through a second heat exchanger for heating the compressed feedstock to 300 to 400 degrees Celsius and subsequently guiding the feedstock line through a second separator for separating a second isolated valuable substance fraction guiding the feedstock line through a third heat exchanger for heating the compressed feedstock to 400 to 550 Celsius degrees and subsequently guiding the feedstock line through a third separator for separating a third isolating valuable substance fraction.

15. The apparatus according to claim 14, comprising the guidance of the feedstock line via a superheater into a reactor for heating the compressed feedstock to a maximum of 700 degrees Celsius, preferably 600 to 680 degrees Celsius.

16. The apparatus according to claim 14, comprising a product line for guiding the reaction product through the third heat exchanger for heating compressed aqueous multicomponent mixture to 400 to 550 degrees Celsius, optionally guiding the product line through the second heat exchanger for heating compressed aqueous multicomponent mixture to 300 to 400 degrees Celsius, optionally guiding the product line through the first heat exchanger for heating compressed aqueous multicomponent mixture to 200 to 300 degrees Celsius.

17. The apparatus according to claim 14, comprising one or more coolers for cooling the valuable substance fraction and/or the reaction product.

18. The apparatus according to claim 14, comprising a separation vessel for separating synthesis gas and dischargeable water.

19. The apparatus according to claim 14, comprising a demister for separating synthesis gas.

20. The method according to claim 1, wherein the method is used to purify water, used to produce phosphorus compounds, ammonium compounds, sand, metals, metal salts from aqueous multicomponent mixtures, or used to produce hydrogen and/or generate electricity.

21. (canceled)

22. (canceled)

Description

[0136] The invention is described in more detail in the following figures. However, the figures do not restrict the invention to these embodiments.

[0137] FIG. 1 shows an apparatus for carrying out the method according to the invention with a storage tank 1, cutting device 2, pump 3, feedstock line 12, heat exchanger 4, separator 5, valve 6, reactor 8 with superheater 7, product line 13, cooler/dryer 14, gas storage tank 15, circulation water line 16, power generator 17, e.g. gas turbine, combined heat and power plant, line with precipitating agent 18. The storage tank 1 is filled with feedstock 31. The first valuable fraction 41, the second valuable fraction 42, the third valuable fraction 43 and the fourth valuable fraction 44 are withdrawn via valves. Water 46 can also be discharged or fed into the circulating water line 16. Synthesis gas 45 is collected in a gas storage tank 15 and converted into electric current 47 via a power generator 17. The addition of precipitating agent 32 is carried out via a pump 3 and line with precipitating agent 18 after separation of the synthesis gas 45 from the reaction product in the fourth valuable substance fraction 44.

[0138] FIG. 2 shows an apparatus for carrying out the method according to the invention with a storage tank 1, cutting device 2, pump 3, feedstock line 12, heat exchanger 4, separator 5, valve 6, reactor 8 with superheater 7, product line 13, cooler/dryer 14, gas storage tank 15, circulation water line 16, power generator 17, e.g. gas turbine, combined heat and power plant, line with precipitating agent 18. The storage tank 1 is filled with feedstock 31. The first valuable fraction 41, the second valuable fraction 42, the third valuable fraction 43 and the fourth valuable fraction 44 are withdrawn via valves. Water 46 can also be discharged or fed into the circulating water line 16. Synthesis gas 45 is collected in a gas storage tank 15 and converted into electric current 47 via a power generator 17. The addition of precipitating agent 32 is carried out via a pump 3 and line with precipitating agent 18 in the third valuable substance fraction 43 by adding the precipitating agent to the compressed feedstock 31 in the third separator 5.

[0139] FIG. 3 shows an apparatus for carrying out the method according to the invention with a storage tank 1, cutting device 2, pump 3, feed line 12, heat exchanger 4, separator 5, valve 6, reactor 8 with superheater 7, product line 13, cooler/dryer 14, gas storage tank 15, circulation water line 16, power generator 17 e.g. gas turbine, combined heat and power plant, line with precipitating agent 18. The storage tank 1 is filled with feedstock 31. The first valuable fraction 41, the second valuable fraction 42, the third valuable fraction 43 and the fourth valuable fraction 44 are withdrawn via valves. Water 46 can also be discharged or fed into the circulating water line 16. Synthesis gas 45 is collected in a gas storage tank 15 and converted into electric current 47 via a power generator 17. The addition of precipitating agent 32 is carried out via a pump 3 and line with precipitating agent 18 in the reactor 8 and separation of the fourth valuable substance fraction 44 via a valve 6.

[0140] In the description, the same reference numerals are used for the same and equivalent parts.

[0141] It should be noted at this point that all the above-described parts taken per se individually and in any combination, in particular the details illustrated in the drawings, are claimed as essential to the invention. Variations thereof are familiar to the person skilled in the art.

REFERENCE NUMERALS

[0142] Apparatus for carrying out the method:

[0143] 1 storage tank

[0144] 2 cutting device

[0145] 3 pump

[0146] 4 heat exchanger

[0147] 5 separator

[0148] 6 valve

[0149] 7 superheater

[0150] 8 reactor

[0151] 9 demister (droplet separator)

[0152] 10 separating vessel

[0153] 11 synthesis gas line

[0154] 12 feedstock line

[0155] 13 product line

[0156] 14 cooler/dryer

[0157] 15 gas storage tank

[0158] 15 circulation water line

[0159] 16 electric current generator (gas turbine/combined heat and power unit)

[0160] 18 line with precipitating agent

[0161] Feedstocks:

[0162] 31 feedstock, in particular aqueous multicomponent mixture

[0163] 32 precipitating agent

[0164] Valuable substances:

[0165] 41 first valuable substance fraction

[0166] 42 second valuable substance fraction

[0167] 43 third valuable substance fraction

[0168] 44 fourth valuable substance fraction

[0169] 45 synthesis gas

[0170] 46 water

[0171] 47 electric current