# US 8,771,627 B2 · Process for producing carbon nanotubes from renewable raw materials

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- Number: US 8,771,627 B2
- Document ID: US8771627B2
- Status: Granted
- Kind: B2
- Application number: 12/062,687
- Filed: 2008-04-04
- Published: 2009-01-08
- Granted: 2014-07-08
- Earliest claimed: 2007-04-06
- Assignees: Arkema France
- Applicants: Serge Bordere; Daniel Cochard; Eric Dutilh; Patrice Gaillard; André Lozowski; Dominique Plee
- Inventors: Serge Bordere; Daniel Cochard; Eric Dutilh; Patrice Gaillard; André Lozowski; Dominique Plee
- Web page: https://patentgrep.com/patent/US8771627B2

## CPC

- C01B 32/162: characterised by catalysts
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES

## Abstract

A subject of the present invention is a process for producing carbon nanotubes, the process comprising: a) the synthesis of alcohol(s) by fermentation of at least one vegetable matter and optionally the purification of the product obtained; b) the dehydration of the alcohol or alcohols obtained in a) in order to produce, in a first reactor, a mixture of alkene(s) and water and optionally the purification of the product obtained; c) the introduction, in particular the introduction into a fluidized bed, in a second reactor, of a powdery catalyst at a temperature ranging from 450 to 850° C., this catalyst comprising at least one catalytic metal supported by an inert solid substrate, the grains of catalyst having a d50 of less than 300 μm; d) bringing the alkene produced in b) into contact with the powdery catalyst of stage c), optionally in a fluidized bed, in order to form carbon nanotubes and hydrogen on the surface of said catalyst by catalytic decomposition of said alkene; e) the recovery of the carbon nanotubes produced in d). The invention also relates to nanotubes capable of being obtained according to the abovementioned process, which can be advantageously used in all the known fields of application of carbon nanotubes.

## Claims

### Claim 1

A process for producing carbon nanotubes, comprising
a) synthesizing alcohol(s) by fermentation of at least one vegetable matter and purifying the product obtained so as to obtain ethanol;
b) dehydrating the ethanol obtained in a) to produce, in a first reactor, a mixture of ethylene and water and optionally purifying the product obtained;
c) introducing, in a second reactor, a powdery catalyst at a temperature ranging from 500 to 700° C., the catalyst comprising iron supported by an inert solid substrate, the grains of catalyst having a d50 of less than 300 μm, wherein the powdery catalyst is produced by impregnating the solid substrate with an aqueous solution of iron then calcination of the solid substrate thus impregnated at a temperature of 200° C. to 400° C.;
d) mixing ethylene with a flow of hydrogen and optionally with at least part of the water produced during the dehydrating of the ethanol in b) and then bringing said mixture into contact with the powdery catalyst of c), in a fluidized bed, to produce hydrogen and form carbon nanotubes on the surface of said catalyst by catalytic decomposition of ethylene;
e) recovering the carbon nanotubes produced in d),
wherein the hydrogen produced in d) is conveyed at least in part to a thermal oxidizer for combustion of the gases produced during stages a) to e).

### Claim 2 (depends on 1)

A process according to claim 1, wherein c), d) and e) are implemented continuously and simultaneously in the second reactor.

### Claim 3 (depends on 1)

A process according to claim 1, wherein the vegetable matter is selected from beet; sugar cane; cereals such as corn, wheat, barley and sorghum; potatoes; and biomass.

### Claim 4 (depends on 3)

A process according to claim 3, wherein the cereal is corn.

### Claim 5 (depends on 1)

A process according to claim 1, wherein b) is carried out by means of a catalyst based on γ-alumina.

### Claim 6 (depends on 1)

A process according to claim 1, wherein the hydrogen produced in d) is recycled at least in part into the second reactor.

### Claim 7 (depends on 1)

A process according to claim 1, wherein the d50 of the grains of powdery catalyst is less than 200 μm.

### Claim 8 (depends on 1)

A process according to claim 1, wherein the d50 of the grains of powdery catalyst is greater than 100 μm.