Method for producing multi-walled carbon nanotubes, multi-walled carbon nanotubes and carbon nanotube powder

Patent metadata

Field	Value
Publication number	US-2016101979-A1
Application number	US-201414894140-A
Country	US
Kind code	A1
Filing date	Jun 5, 2014
Priority date	Jun 7, 2013
Publication date	Apr 14, 2016
Grant date	—

Abstract

The invention relates to temperature-stable rigid foams which can be cold formed and have a density of 0 to 100 kg/m (according to DIN 53420), an elongation at break (according to DIN 53430) of 12 to 35%, a percentage of open cells (according to DIN ISO 4590-86) of 51% to 98% and a storage module of the foam (according to DIN EN ISO 6721 B:1996-12) in the temperature range of 60 DEG to 190 DEG C of, on average, greater or equal 0.1 MPa, and to composite materials produced with said foams.

First claim

1 .- 16 . (canceled)

17 . A process for producing multi-wall carbon nanotubes which comprises the following steps:
initial charging of a substrate composed of carbon nanotubes in an agitated bed of a reactor, introduction of a carbon-containing precursor into the agitated bed, reaction of the precursor in the agitated bed under suitable process conditions which bring about graphitic deposition of carbon on the carbon nanotubes of the substrate, discharge of the carbon nanotubes from the reactor.

18 . The process as claimed in claim 17 , wherein a process temperature in the range from 850° C. to 1300° C. is set for the process conditions which bring about graphitic deposition.

19 . The process as claimed in claim 17 , wherein a process temperature in the range from 950° C. to 1300° C., is set for the process conditions which bring about graphitic deposition.

20 . The process as claimed in claim 17 , wherein the proportion of catalysts which bring about length growth of carbon nanotubes in the agitated bed during the process is less than 5000 ppm.

21 . The process as claimed in claim 17 , wherein cleaned, in particular acid-cleaned, carbon nanotubes are used for the substrate.

22 . The process as claimed in claim 17 , wherein the process conditions, in particular temperature, pressure and/or gas composition in the reactor, are selected so that the ratio of the kinetic constant for thickness growth of the carbon nanotubes to the kinetic constant for the length growth of the carbon nanotubes caused by catalyst constituents is greater than 1.

23 . The process as claimed in claim 17 , wherein a fluidized bed of a fluidized-bed reactor is used as agitated bed.

24 . The process as claimed in claim 17 , wherein a precursor input into the reactor of from 0.0001 to 1 g per gram of substrate and per minute is set for the process conditions which bring about graphitic deposition.

25 . The process as claimed in claim 17 , wherein the carbon-containing precursor contains or consists of an optionally substituted aliphatic, cyclic, heterocyclic, aromatic and/or heteroaromatic compound or a mixture thereof.

26 . The process as claimed in claim 24 , wherein the aliphatic or heterocyclic compound is at least partially unsaturated.

27 . The process as claimed in claim 17 , wherein the carbon-containing precursor contains or consists of a compound comprising carbon and at least one heteroatom from the group consisting of nitrogen, boron, phosphorus and silicon; or the carbon-containing precursor contains at least two compounds of which at least one comprises carbon and at least one other of which comprises an element from the group consisting of nitrogen, boron, phosphorus and silicon.

28 . A multi-wall carbon nanotube, in particular one which can be produced by a process as claimed in claim 17 , having at least one first graphene-like layer and a second graphene-like layer, where the second layer is arranged outside the first layer in the cross section of the carbon nanotube,
wherein, one of the two layers has a first doping and the other of the two layers has a second, different doping or is undoped.

29 . The carbon nanotube as claimed in claim 27 , wherein one of the layers is doped with nitrogen, boron, phosphorus or silicon.

30 . A carbon nanotube powder comprising carbon nanotubes as claimed in claim 27 .

31 . The carbon nanotube powder as claimed in claim 29 , wherein the carbon nanotubes have an average diameter in the range from 3 to 100 nm.

32 . The carbon nanotube powder as claimed in claim 29 , wherein the carbon nanotubes have an average diameter in the range from 10 to 25 nm and the carbon nanotube powder has a diameter ratio D90/D10 of less than 3.

33 . The carbon nanotube powder as claimed in claim 29 , wherein the carbon nanotube powder has a diameter ratio D90/D10 of less than 4.

34 . The carbon nanotube powder as claimed in claim 29 , wherein the carbon nanotube powder has a bulk density of from 20 to 500 kg/m 3 .

Assignees

• Covestro Deutschland Ag

Inventors

• Hocke Heiko
• Shlüter Oliver Felix-Karl
• Michele Volker
• Mleczko Leslaw

Classifications

• C01B32/168 Primary

  After-treatment · CPC title

• C01P2006/11

  Powder tap density · CPC title

• C23C16/442 Primary

  using fluidised bed process · CPC title

• C23C16/26

  Deposition of carbon only · CPC title

• C01B2202/06

  Multi-walled nanotubes · CPC title