# US 11,299,396 B2 · System for the production of carbon nanotubes from carbon matter, preferably, plastic waste and solar energy; method of production

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- Number: US 11,299,396 B2
- Document ID: US11299396B2
- Status: Granted
- Kind: B2
- Application number: 16/628,490
- Filed: 2018-06-26
- Published: 2020-06-11
- Granted: 2022-04-12
- Earliest claimed: 2017-07-03
- Assignees: Universidad De Chile
- Applicants: Universidad De Chile
- Inventors: Francisco Gracia Caroca; Mauricio Morel Escobar; Vania Jocelyn Rojas Fuentes; Gerardo Cabrera Papamija; Nicolas Carvajal
- Web page: https://patentgrep.com/patent/US11299396B2

## CPC

- C01B 32/16: Preparation
- B01J 19/08: Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor (application of shock waves B01J3/08)
- B01J 19/12: employing electromagnetic waves
- B01J 29/46: Iron group metals or copper
- B29B 17/04: Disintegrating plastics, {e.g. by milling}(B29B9/02, B29B11/02, B29B13/10, {B29B17/02} take precedence)
- C08J 11/04: of polymers
- C10B 49/00: Destructive distillation of solid carbonaceous materials by direct heating with heat-carrying agents including the partial combustion of the solid material to be treated
- F24S 23/30: with lenses
- F24S 30/425: Horizontal axis
- F24S 30/48: with three or more rotation axes or with multiple degrees of freedom
- F24S 50/20: for tracking
- B29B 2017/0496: {Pyrolysing the materials}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- Y02B 10/20: Solar thermal
- Y02E 10/47: Mountings or tracking
- Y02P 20/133: Renewable energy sources, e.g. sunlight
- Y02W 30/20: Waste processing or separation
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B29B: PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- C10B: DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS (cracking oils C10G; underground gasification of minerals E21B43/295)
- F24S: SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS (for producing mechanical power from solar energy F03G6/00)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- Y02B: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02W: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT

## Abstract

The present invention relates to a system for the production of carbon nanotubes from carbonaceous matter, preferably, plastic waste and solar energy; Method of production.

## Claims

### Claim 1

A system for obtaining carbon nanotubes (CNT) from carbonaceous matter using solar radiation as energy source comprising:
a) a solar tracking sub-system along of a length of the system or X axis and at altitude or Y axis to provide solar radiation to two zones of a two-zone solar reactor, comprising:
a.1) an upper support providing stability, housing Fresnel lenses that allow the tracking and concentration of incident solar radiation in at least one focal point;
a.2) at least four upper actuators for positioning at least two Fresnel lenses;
a.3) a central actuator to fit a height of said upper support in relation to said two-zone solar reactor in order to control a circle radius of sunlight generated by the concentration of solar radiation, and
a.4) a photo-detector that cooperates with a balance set for moving said upper support according to the sun's path and keeping the circle radius of sunlight at a same point, wherein said balance set comprises:
i) a hydraulic arm actuator,
ii) a bearing-shaft coupling that receives the hydraulic arm actuator, and
iii) a lower support of the hydraulic arm actuator, which serves as a support point to actuate said actuator and which is adhered to said lower support; wherein said upper support comprises a central structure that supports said central actuator and keeps the center of mass of said upper support;
a control board adhered to said lower support, containing a controller for said central actuator and said photo-detector, in order to automatically or manually control the movement of said upper support along the length of system (X axis) and/or altitude (Y axis) and said at least two Fresnel lenses each independently, based on the information received from the photo-detector, and a base where the solar reactor is coupled in order to be able to rotate together with the upper support structure;
b) a two-zone solar reactor sub-system comprising a two-zone reactor, a carbonaceous matter pyrolysis zone and a carbon nanotube synthesis zone, which may be separated by use of at least one catalyst; and optionally
c) an energy conversion sub-system to convert solar to electrical energy that continuously feeds the controller of said control board with electrical energy, and which comprises a system for solar to electrical energy conversion.

### Claim 2 (depends on 1)

The system of claim 1, WHEREIN said lower support is fixed to the ground or has wheels that allow a movement in depth/width (Z axis).

### Claim 3 (depends on 1)

The system of claim 1, WHEREIN said upper support has a range of motion in X and Y axes with respect to the lower support from an angle α=40°, measured counterclockwise from the X axis to an angle β=40°, measured clockwise from the X axis.

### Claim 4 (depends on 1)

The system of claim 1, WHEREIN said radius of the circle of sunlight generated by the concentration of the solar radiation of each of the Fresnel lenses on each solar reactor zone reaches a maximum radius of 20.5 cm.

### Claim 5 (depends on 1)

The system of claim 1, WHEREIN said system for solar to electrical energy conversion is selected from rechargeable batteries, an electrical connection, a regulating device and photovoltaic cells for transforming light energy into electrical energy.

### Claim 6 (depends on 1)

The system of claim 1, WHEREIN a ratio of a total height taken from the base in said lower support to the highest point of said upper support, to a total length referred to a distance between the ends of the axes coupled to said bearing-shaft coupling, to a total length of said upper support, to a length of said reactor, to the height of said reactor, to the maximum coupling point of said hydraulic arm with said bearing-shaft coupling is as 1:1:1:1:1.

### Claim 7 (depends on 1)

The system of claim 1, WHEREIN a ratio of the length of said carbonaceous matter pyrolysis zone to said carbon nanotube synthesis zone is 2:1, 1:1 or 1:2.

### Claim 8 (depends on 1)

The system of claim 1, WHEREIN said carbonaceous matter pyrolysis zone and said carbon nanotube synthesis zone are made of a heat conducting material resistant to temperatures greater than 900° C.

### Claim 9 (depends on 1)

The system of claim 1, WHEREIN said reactor has an insulator.

### Claim 10 (depends on 1)

The system of claim 1, WHEREIN said reactor has a first temperature sensor and a second temperature sensor, said first temperature sensor is located on the outside of the reactor, adjacent to the edge of the sunlight focus which is concentrated by the Fresnel lenses in order to monitor the temperature outside of it, and said second temperature sensor is located in the inner part of each of the carbonaceous matter pyrolysis zone and the carbon nanotube synthesis zone, in order to monitor the temperature inside the carbonaceous matter pyrolysis zone and carbon nanotube synthesis zone.

### Claim 11 (depends on 1)

The system of claim 1, WHEREIN said solar reactor in each of said carbonaceous material pyrolysis zone and said nanotube synthesis zone has pressure sensors.

### Claim 12 (depends on 1)

The system of claim 1, further comprising a vacuum system that allows the evacuation of the air which is located inside the two-zone solar reactor.

### Claim 13 (depends on 1)

The system of claim 1, further comprising an inlet for entering an inert gas into the reactor to help the transportation of the carbonaceous gases generated in the carbonaceous material pyrolysis zone to the synthesis zone and generate a protective environment favorable to the reactions in the carbon nanotube synthesis catalyst.

### Claim 14 (depends on 1)

The system of claim 1, WHEREIN the carbonaceous matter pyrolysis zone and the carbon nanotube synthesis zone comprises a sealant resistant to high temperatures and preventing gas permeation produced in pyrolysis outwards.

### Claim 15 (depends on 1)

The system of claim 1, WHEREIN the carbonaceous matter is plastic waste including polypropylene, high density polypropylene or mixture of both.

### Claim 16 (depends on 1)

The system of claim 1, WHEREIN said carbonaceous matter pyrolysis zone and said carbon nanotubes synthesis zone are connected.

### Claim 17 (depends on 16)

The system of claim 16, WHEREIN said carbonaceous matter pyrolysis zone and said carbon nanotube synthesis zone are connected by a flow regulator.

### Claim 18 (depends on 17)

The system of claim 17, WHEREIN said flow regulator is a valve or a flow valve.

### Claim 19 (depends on 1)

The system of claim 1, WHEREIN said reactor has a first gate and a second gate for feeding the reactor with carbonaceous raw material including polypropylene, high density polyethylene or mixtures of both, at least one plastic pyrolysis catalyst and at least one carbon nanotube synthesis catalyst.

### Claim 20 (depends on 19)

The system of claim 19, WHEREIN said at least one carbon nanotube synthesis catalyst is a catalyst based on nickel, cobalt, iron, aluminum and zeolite, or combinations thereof.

### Claim 21 (depends on 19)

The system of claim 19, WHEREIN said first gate and second gate are located at each end of each carbonaceous matter pyrolysis zone and carbon nanotube synthesis zone of the reactor.

### Claim 22 (depends on 21)

The system of claim 21, WHEREIN said first gate and second gate comprise sliding rails for sliding and positioning the mixture of carbonaceous material and optionally the mixture of carbonaceous material and said at least one plastic pyrolysis catalyst, in the carbonaceous material pyrolysis zone.

### Claim 23 (depends on 22)

The system of claim 22, WHEREIN said at least one plastic pyrolysis catalyst is a catalyst based on aluminum oxides, silicon oxides, mixtures in aluminosilicates, optionally with the presence of alkali and alkaline earth metals.

### Claim 24 (depends on 22)

The system of claim 22, WHEREIN said rails enter directly into each zone of the reactor or through an arm support that allows an operator to move away from the incident radiation on the reactor.

### Claim 25 (depends on 22)

The system of claim 22, WHEREIN said rails are made of a heat conducting material that resists temperatures above 1400° C.

### Claim 26 (depends on 25)

The system of claim 25, WHEREIN said heat conducting material is stainless steel.

### Claim 27 (depends on 19)

The system of claim 19, WHEREIN said at least one plastic pyrolysis catalyst and at least one carbon nanotube synthesis catalyst is mixed with a support.

### Claim 28 (depends on 27)

The system of claim 27, WHEREIN said support is a silicate or zeolite aluminum.

### Claim 29

A method for producing carbon nanotubes (CNT) from carbonaceous matter and using solar radiation as an energy source characterized by comprising:
a) placing a solar reactor on a lower support medium supported on a base medium and anchored through fastening bolts to said base medium,
b) placing carbonaceous raw matter including polypropylene, high density polyethylene or mixtures of both and at least one plastic pyrolysis catalyst in a carbonaceous matter pyrolysis zone and a carbon nanotube synthesis catalyst including a catalyst based on nickel, cobalt, iron and a combination of two or more thereof, optionally with a support in a carbon nanotube synthesis zone of the reactor by entering through a first gate and a second gate of the solar reactor and by sliding rails,
c) controlling temperature and pressure in the carbonaceous matter pyrolysis zone and the carbon nanotube synthesis zone,
d) activating a solar tracking system in order to orient an upper support medium in the direction of the largest solar radiation,
e) actuating the actuator mediums for positioning the Fresnel lenses so that the focus of concentrated light is positioned on the carbonaceous matter pyrolysis zone and the carbon nanotube synthesis zone,
f) preheating the carbonaceous matter pyrolysis zone and the carbon nanotubes production zone of the reactor from room temperature to a reaction temperature in the range of from 500 to 800° C. in the carbonaceous matter pyrolysis zone and in the carbon nanotube synthesis zone.

### Claim 30 (depends on 29)

The method of claim 29, WHEREIN after stage b), stage b′ is performed which comprises setting the solar reactor by emptying inside it or by making vacuum and allowing inert gases to enter inside.

### Claim 31 (depends on 29)

The method of claim 29, WHEREIN the carbonaceous matter is plastic waste comprising polypropylene, high density polypropylene or mixture of both.

### Claim 32 (depends on 29)

The method of claim 29, WHEREIN before stage a), stage a′ is performed which comprises preparing the solar reactor to ensure cleanliness of the carbonaceous matter pyrolysis zone and the carbon nanotube synthesis zone.

### Claim 33 (depends on 32)

The method of claim 32, WHEREIN cleaning stage a′ is carried out with an organic solvent, a mechanical-abrasive medium or a combination of both.