Removing carbon nanotubes from a continuous reactor effluent

Patent metadata

Field	Value
Publication number	US-10343104-B2
Application number	US-201314395447-A
Country	US
Kind code	B2
Filing date	Apr 10, 2013
Priority date	Apr 18, 2012
Publication date	Jul 9, 2019
Grant date	Jul 9, 2019

Abstract

Systems and a method for removing carbon nanotubes from a continuous reactor effluent are provided herein. The method includes flowing the continuous reactor effluent through a separation vessel, separating carbon nanotubes from the continuous reactor effluent in the separation vessel, and generating a stream including gaseous components from the continuous reactor effluent.

First claim

What is claimed is:

1. A system for producing carbon nanotubes, comprising:
a reactor to receive and react a feed gas comprising feedstock and a recycle stream with catalyst particles to form carbon nanotubes, and to discharge overhead a continuous reactor effluent comprising the carbon nanotubes and catalyst particles;
a first separation vessel to:
isolate catalyst particles from the carbon nanotubes in the continuous reactor effluent; and
return the catalyst particles via a recycle line to the reactor;

a second separation vessel comprising a cyclonic separator to:
isolate the carbon nanotubes from the continuous reactor effluent; and
generate a waste stream comprising gaseous components from the continuous reactor effluent;
a heat exchanger to condense water in the waste stream to give a dry waste stream; and
a gas fractionation system to process the dry waste stream to give the recycle stream and an excess feed stream, wherein the waste stream comprises residual carbon nanotubes.

2. The system of claim 1 , comprising:
a compressor to compress the dry waste gas stream; and
a gas fractionation system to process the compressed dry waste gas stream to give the recycle stream enriched in methane and an excess feed stream enriched in carbon dioxide, wherein the heat exchanger comprises an ambient-temperature heat exchanger, and wherein the recycle line couples the first separation vessel to the reactor.

3. The system of claim 2 , comprising a mixer to add the recycle stream to the feedstock to give the feed gas to the reactor, wherein the reactor comprises a fluidized bed reactor.

4. The system of claim 1 , comprising a gas fractionation system comprising cryogenic distillation to process the dry waste stream to give the recycle stream and an excess feed stream, wherein the first separation vessel comprises a cyclonic separator.

5. The system of claim 1 , wherein the continuous reactor effluent comprises the gaseous components comprising unreacted feed gas, wherein the cyclonic separator comprises a multicyclonic separator to discharge the carbon nanotubes as a product stream.

6. The system of claim 1 , wherein the cyclonic separator comprises a swirl element comprising swirl vanes that rotate to impart the radical acceleration or the tangential velocity, or both.

7. The system of claim 1 , comprising a mixer to add the recycle stream to the feedstock upstream of the reactor to give the feed gas, wherein the continuous reactor effluent comprises the gaseous components comprising unreacted feed gas, and wherein the dry waste stream comprises a dew point greater than −5° C.

8. The system of claim 7 , wherein the mixer comprises a static mixer.

9. The system of claim 1 , comprising a filter to remove residual carbon nanotubes from the waste stream, wherein the continuous reactor effluent comprises unreacted feed gas with the carbon nanotubes and catalyst particles, and wherein the heat exchanger comprises an ambient-temperature heat exchanger.

10. The system of claim 9 , wherein the second separation vessel to discharge as a product stream the carbon nanotubes isolated from the continuous reactor effluent, wherein the filter to discharge the residual carbon nanotubes into the product stream, and wherein the filter comprises a sintered ceramic filter, a sintered metal filter, a fabric bag filter, or a fluidized bed filter, or any combinations thereof.

11. The system of claim 9 , wherein the filter is configured to perform a self-cleaning procedure to remove any remaining carbon nanotubes.

12. The system of claim 1 , comprising:
a water separation vessel to receive the condensed water from the heat exchanger, wherein the condensed water to settle in the water separation vessel and discharge from a bottom of the water separation vessel, and wherein the water separation vessel is not a component of the heat exchanger; and
a compressor to compress the dry waste stream to give a compressed dry waste gas stream.

13. The system of claim 1 , comprising:
a compressor to compress the dry waste stream to give a compressed dry waste gas stream;
a second heat exchanger to condense water in the compressed dry waste gas stream; and
a gas fractionation system to process the compressed dry waste gas stream to give the recycle stream enriched in methane and an excess feed stream enriched in carbon dioxide.

14. The system of claim 13 , comprising a mixer to add the recycle stream to the feedstock to give the feed gas fed to the reactor, wherein the second heat exchanger comprises an ambient-temperature heat exchanger.

15. The system of claim 1 , comprising another heat exchanger to heat the feed gas with waste heat from the waste stream.

16. The system of claim 15 , wherein the another heat exchanger comprises a shell-and-tube heat exchanger.

17. A method for producing carbon nanotubes, comprising:
combining a feedstock and a recycle gas to give a feed gas fed to a reactor;
reacting the feed gas with a catalyst in the reactor to form carbon nanotubes;
discharging overhead from the reactor a continuous reactor effluent comprising the carbon nanotubes and catalyst particles;
flowing the continuous reactor effluent through a catalyst separation vessel that isolates catalyst particles from the carbon nanotubes in the continuous reactor effluent and returns the catalyst particles via a recycle line to the reactor;
flowing the continuous reactor effluent from the catalyst separation vessel through a carbon-nanotube separation vessel comprising a cyclonic separator comprising a multicyclonic separator having a swirl element that imparts radial acceleration and a tangential velocity component to the continuous reactor effluent; and
separating carbon nanotubes from the continuous reactor effluent in the carbon- nanotube separation vessel, generating a waste stream comprising gaseous components from the continuous reactor effluent.

18. The method of claim 17 , comprising:
separating from the waste stream via cryogenic distillation a first stream enriched in methane and a second stream enriched in carbon dioxide, wherein the recycle stream comprises the first stream, and wherein combining comprises adding the recycle stream to the feedstock upstream of the reactor to give the feed gas; and
heating, via a heat exchanger, the feed gas comprising the feedstock and the recycle gas upstream of the reactor with waste heat from the waste stream.

19. The method of claim 17 , wherein the recycle line couples the catalyst separation vessel to the reactor, and wherein separating the carbon nanotubes from the continuous reactor effluent in the carbon-nanotube separation vessel comprises isolating via the swirl element by gravity the carbon nanotubes from the waste stream comprising gaseous components and discharging the carbon nanotubes as a product stream.

20. The method of claim 17 , wherein the swirl element comprises swirl vanes that rotate to impart the radical acceleration and the tangential velocity component.

21. The method of claim 17 , comprising heating, via a heat exchanger, the feed gas with waste heat from the waste stream, wherein the swirl element imparts the radial acceleration and the tangential velocity component through the rotation of twisted swirl vanes on the swirl element.

22. The method of claim 19 , comprising:
filtering the waste stream to remove residual carbon nanotubes from the waste stream;
condensing, via a heat exchanger, water in the waste stream; and
adding

Assignees

• Exxonmobil Upstream Res Co
• Solid Carbon Prod Llc

Inventors

• Denton Robert D
• Noyes Dallas B
• Koveal Jr Russell J
• Ring Terry A

Classifications

• C01B32/164

  involving continuous processes · CPC title

• B01D45/12

  by centrifugal forces (centrifuges B04B; cyclones B04C) · CPC title

• C01B32/17

  Purification · CPC title

• B01D46/38

  as fluidised bed · CPC title

• C01B32/15 Primary

  Nano-sized carbon materials · CPC title