Removing carbon nanotubes from a water system

• US 9,975,793 B2
• Filed: 04/10/2013
• Issued: 05/22/2018
• Est. Priority Date: 04/18/2012
• Status: Active Grant

• Current Assignee: Exxonmobil Upstream Research Company (Exxon Mobil Corporation), Solid Carbon Products LLC
• Original Assignee: Exxonmobil Upstream Research Company (Exxon Mobil Corporation), Solid Carbon Products LLC
• Inventors: Denton, Robert D., Noyes, Dallas B., Koveal, Jr., Russell J., Ring, Terry A.
• Primary Examiner(s): Robinson, Renee
• Application Number:
  US14/395,450
• Publication Number:
  US 20150114819A1
• Time in Patent Office: 1,868 Days
• CPC Class Codes: B01D 21/267 by using a cyclone
• CPC Class Codes: B03D 1/24 Pneumatic mixing gases or vapours with liquids B01F23/20
• CPC Class Codes: C01B 32/16 Preparation
• CPC Class Codes: C01B 32/168 After-treatment
• CPC Class Codes: C02F 1/04 by distillation or evaporation
• CPC Class Codes: C02F 1/24 by flotation C02F1/465 takes precedence
• CPC Class Codes: C02F 1/283 using coal, charred products, or inorganic mixtures containing them
• CPC Class Codes: C02F 1/38 by centrifugal separation
• CPC Class Codes: C02F 1/441 by reverse osmosis
• CPC Class Codes: C02F 1/52 by flocculation or precipitation of suspended impurities C02F1/463 takes precedence
• CPC Class Codes: C02F 1/56 Macromolecular compounds
• CPC Class Codes: C02F 1/72 by oxidation C02F1/4672 takes precedence
• CPC Class Codes: C02F 1/725 by catalytic oxidation
• CPC Class Codes: C02F 1/74 with air aeration of stretches of water C02F7/00
• CPC Class Codes: C02F 1/78 with ozone C02F1/4672 takes precedence
• CPC Class Codes: C02F 2101/10 Inorganic compounds
• CPC Class Codes: C02F 2103/34 from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
• CPC Class Codes: C02F 2103/36 from the manufacture of organic compounds
• CPC Class Codes: C02F 2305/08 Nanoparticles or nanotubes
• CPC Class Codes: C02F 9/00 Multistage treatment of water, waste water or sewage
• CPC Class Codes: Y02P 20/129 : Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Abstract

Methods and a system for removing carbon nanotubes from a water stream are provided herein. The system includes a purification vessel, wherein the purification vessel is configured to form a carbon oxide from the carbon nanotubes within the water stream.

Claims

1. A method comprising:

forming carbon nanotubes in a reactor in a Bosch reaction;

separating the carbon nanotubes from a reactor effluent stream, forming a waste gas stream;

condensing water in the waste gas stream giving a water stream;

removing carbon nanotubes from the water stream to give a purified water stream, wherein removing the carbon nanotubes comprises forming carbon oxide from the carbon nanotubes within the water stream to give the purified water stream.

2. The method of claim 1, comprising discharging the reactor effluent stream overhead from the reactor, wherein the reactor comprises a fluidized bed reactor, and wherein forming carbon oxide comprises air sparging the water stream in a vessel to form the carbon oxide from the carbon nanotubes within the water stream.

3. The method of claim 1, wherein removing further comprises adding a flocculant to the water stream to effect a separation of the carbon nanotubes from the water stream.

4. The method of claim 1, wherein removing further comprises sparge mixing an ozone stream with the water stream to form a froth in a vessel to effect a separation of the carbon nanotubes from the water stream, and wherein forming carbon oxide comprises oxidizing carbon nanotubes via the sparge mixing of the ozone stream with the water stream to form the carbon oxide.

5. The method of claim 1, wherein separating comprises separating the carbon nanotubes from the reactor effluent stream via a cyclonic separator, and wherein removing further comprises flowing the water stream through a hydrocyclone to remove the carbon nanotubes from the water stream.

6. The method of claim 1, wherein removing further comprises filtering the carbon nanotubes out of the water stream through reverse osmosis.

7. The method of claim 1, wherein condensing water in the waste gas stream gives a dry waste gas stream, wherein the method further comprises compressing the dry waste gas stream and condensing water in dry waste gas stream, and wherein forming carbon oxide comprises forming the carbon oxide from the carbon nanotubes within the water stream through oxidation of the carbon nanotubes.

8. The method of claim 1, wherein forming carbon oxide comprises producing an underwater flame via an underwater burner to degrade the carbon nanotubes to form the carbon oxide from the carbon nanotubes.

9. The method of claim 1, comprising providing feed gas to the reactor, wherein forming the carbon nanotubes comprises forming the carbon nanotubes from the feed gas in the reactor, wherein forming carbon oxide comprises passing the water stream through a flame degradation vessel to combust the carbon nanotubes into ash and the carbon oxide, and removing water and carbon oxide from the flame degradation vessel through formation of steam.

10. The method of claim 9, comprising:

heating the feed gas with waste heat from the waste gas stream; and

condensing the steam via a heat exchanger to recover water.

11. The method of claim 1, wherein removing further comprises flowing the water stream through a filter to remove carbon nanotubes from the water stream.

12. The method of claim 1, wherein condensing comprises condensing water in the waste gas stream via an ambient-temperature heat exchanger, and wherein forming carbon oxide comprises sparging at least one of air, oxygen, or ozone into the water stream in a vessel to oxidize carbon nanotubes to form carbon oxide from carbon nanotubes.

13. The method of claim 1, wherein giving the water stream comprises separating the water stream from the waste gas stream, and wherein removing the carbon nanotubes comprises flowing the water stream into a purification vessel.

14. A method for producing carbon nanotubes including purifying a water stream comprising carbon nanotubes, comprising:

reacting a feed gas with a catalyst in a reactor in a Bosch reaction to form carbon nanotubes;

discharging a reactor effluent from the reactor;

separating product carbon nanotubes from the reactor effluent, forming a waste gas stream comprising residual carbon nanotubes;

condensing, via a first heat exchanger, water in the waste gas stream to give a water stream; and

flowing the water stream into a purification vessel;

injecting air into the purification vessel; and

effecting a separation of the carbon nanotubes from the water stream through an interaction of the air with the carbon nanotubes through air sparging within the purification vessel to give a purified water stream.

16. The method of claim 14, comprising heating the feed gas via a second heat exchanger with waste heat from the waste gas stream, wherein effecting the separation comprises removing the carbon nanotubes from the purification vessel by flowing the carbon nanotubes over a weir and into a collection vessel.

15. A method for producing carbon nanotubes including purifying a water stream comprising carbon nanotubes, comprising:

reacting a feed gas with a catalyst in a reactor in a Bosch reaction to form carbon nanotubes;

discharging a reactor effluent from the reactor;

separating product carbon nanotubes from the reactor effluent, forming a waste gas stream comprising residual carbon nanotubes;

condensing water in the waste gas stream to give a water stream;

flowing the water stream into a purification vessel;

injecting ozone into the purification vessel; and

effecting a separation of the carbon nanotubes from the water stream through an interaction of the ozone with the carbon nanotubes through ozonolysis within the purification vessel to give a purified water stream.

17. A system comprising:

a reactor to form carbon nanotubes from feed gas in a Bosch reaction, the reactor comprising an inlet to receive the feed gas and an outlet to discharge the reactor effluent;

a separation device to separate carbon nanotubes from the reactor effluent, forming a waste gas stream;

a heat exchanger to condense water in the waste gas stream to give a dry waste gas stream and a water stream; and

a purification system to remove carbon nanotubes from the water stream to give a purified water stream, comprising the purification system to form carbon oxide from the carbon nanotubes within the water stream.

18. The system of claim 17, wherein the separation device comprises a cyclonic separator, wherein the purification system comprises a purification vessel comprising an air sparge vessel to receive the water stream and inject air to form the carbon oxide and also to remove carbon nanotubes from the water stream by forming a froth phase having carbon nanotubes separated from a clean water phase.

19. The system of claim 18, comprising a second heat exchanger to heat the feed gas with waste heat from the waste gas stream, wherein the sparger vessel comprises a sparger ring.

20. The system of claim 17, wherein the separation device comprises an inlet to receive the reactor effluent, a first outlet to discharge the carbon nanotubes, and a second outlet to discharge the waste gas stream, and wherein the purification system is configured to inject flocculant into the water stream to remove carbon nanotubes from the water stream.

21. The system of claim 17, wherein the purification system is configured to form the carbon oxide from the carbon nanotubes within the water stream through ozonolysis or oxidation.

22. The system of claim 17, comprising a hydrocyclone to remove large carbon nanotubes from the water stream before the water stream is flowed into a purification vessel of the purification system.

23. The system of claim 17, wherein the purification system comprises a semipermeable membrane permeable to water but impermeable to carbon nanotubes to remove the carbon nanotubes from the water stream through reverse osmosis.

24. The system of claim 17, wherein the purification system comprises a purification vessel comprising an underwater burner to produce an underwater flame to degrade carbon nanotubes in the water stream received in the purification vessel to form the carbon oxide.

25. The system of claim 17, wherein the purification system comprises a purification vessel comprising a flame degradation vessel configured to oxidize the carbon nanotubes to form the carbon oxide, and to discharge carbon oxide and water through formation of steam.

26. The system of claim 17, comprising a separation vessel to cooperate with the heat exchanger to give the dry waste gas stream and the water stream, the separation vessel to discharge the water stream from a bottom portion of the separation vessel to the purification system.

27. The system of claim 17, comprising:

a compressor to compress the dry waste gas stream; and

a second heat exchanger to receive the dry waste gas stream from the compressor and condense water in the dry waste gas stream.