# US 2018/0023005 A1 · Device and process for the recovery of increased volumes of pure terpenes and terpenoids from scrap polymers and elastomers

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- Number: US 2018/0023005 A1
- Document ID: US20180023005A1
- Status: Published application
- Kind: A1
- Application number: 15/219,128
- Filed: 2016-07-25
- Published: 2018-01-25
- Earliest claimed: 2016-07-25
- Inventors: EARL R. BEAVER; JONATHAN L. WISTROM
- Web page: https://patentgrep.com/patent/US20180023005A1

## CPC

- C10G 1/02: by distillation
- B01D 1/22: by bringing a thin layer of the liquid into contact with a heated surface {(B01D1/065 takes precedence)}
- B01D 1/225: {with blades or scrapers}
- B01D 3/143: {by two or more of a fractionation, separation or rectification step}
- C10B 1/02: Stationary retorts
- C10B 7/10: with conveyor-screws
- C10B 27/06: Conduit details, e.g. valves
- C10B 47/44: with conveyor-screws
- C10B 53/07: {of solid raw materials consisting} of synthetic polymeric materials, e.g. tyres (recovery or working-up of waste materials of organic macromolecular compounds or compositions based thereon by dry-heat treatment for obtaining partially depolymerised materials C08J11/10; production of liquid hydrocarbon mixtures from rubber or rubber waste C10G1/10)
- C10B 57/06: containing additives
- C10G 1/002: {in combination with oil conversion- or refining processes}
- C10G 1/10: from rubber or rubber waste
- C10B 1/06: Horizontal retorts
- Y02P 20/143: the feedstock being recycled material, e.g. plastics
- C10G: CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION (cracking to hydrogen or synthesis gas C01B; cracking or pyrolysis of hydrocarbon gases to individual hydrocarbons or mixtures thereof of definite or specified constitution C07C; cracking to cokes C10B); RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C10B: DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS (cracking oils C10G; underground gasification of minerals E21B43/295)
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

A device and process for the vacuum pyrolization of scrap tires to produce a pyrolytic oil from which valuable terpenes such as limonene and pulegone may be extracted and purified.

## Claims

### Claim 1

A device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone comprising;
a nitrogen blanket bin for accepting shredded, washed, and dried automobile tires;
at least one vacuum-lock valve;
a helical screw which slowly turns to generate a mixture of shredded automobile tires and an additive/catalyst that can flow from the nitrogen blanket bin;
at least one heater for heating the mixture from ambient temperature to about 450 degrees Celsius;
a release valve for controlling the release of at least one of either a material and a vapor from the nitrogen blanket vacuum sealed furnace through a thin film evaporator and into a contactor/separator for recovery of at least one of either a type of terpene or a type of terpenoid from a mixture that has at least one of either the material or the vapor, wherein the contactor/separator can generate a pyrolytic vapor from the at least one of either the material or the vapor after a set of solids is removed from the mixture, and wherein the contactor/separator includes a chiller assembly for reducing the temperature of the pyrolytic vapor, a first heatable distillation column for reheating and cooling the mixture, a second heatable distillation column containing internal components that are at least one of either sieve trays or structured packing, wherein the second distillation column separates types of terpenes and the types of terpenoids that have been extracted from the mixture, wherein the mixture is passed through a small orifice disposed between the first distillation column and the second distillation column to thereby reduce the temperature of the mixture as it enters the second distillation column, wherein the terpenes and terpenoids are removed from the second distillation column through at least one tap mounted on an outside surface of the second distillation column, and
a piping system for transporting the liquid and vapor products that are one of either produced, transferred, recovered, or purified by the device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone.

### Claim 2

A device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone comprising;
a nitrogen blanket vacuum sealed furnace for accepting automobile tires;
a heater for heating the nitrogen blanket vacuum sealed furnace to at least about 200 degrees Centigrade;
a vacuum pump for generating a vacuum in the nitrogen blanket vacuum sealed furnace;
an additive/catalyst placed within the nitrogen blanket vacuum sealed furnace for dispersion over the automobile tires;
a release valve for controlling the release of at least one of either a material and a vapor from the nitrogen blanket vacuum sealed furnace a thin film evaporator and into a contactor/separator for recovery of at least one of either a type of terpene or a type of terpenoid from a mixture that has at least one of either the material or the vapor, wherein the contactor/separator can generate a pyrolytic vapor from the at least one of either the material or the vapor after a set of solids is removed from the mixture, and wherein the contactor/separator includes a chiller assembly for reducing the temperature of the pyrolytic vapor, a first distillation column for reheating and cooling the mixture, a second distillation column containing internal components that are at least one of either sieve trays or structured packing, wherein the second distillation column separates types of terpenes and the types of terpenoids that have been extracted from the mixture, wherein the mixture is passed through a small orifice disposed between the first distillation column and the second distillation column to thereby reduce the temperature of the mixture as it enters the second distillation column, wherein the terpenes and terpenoids are removed from the second distillation column through at least one tap mounted on an outside surface of the second distillation column, and
a piping system for transporting the liquid and vapor products that are one of either produced, transferred, recovered, or purified by the device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone.

### Claim 3 (depends on 2)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 2 wherein the contactor/separator can generate a pyrolytic vapor from the at least one of either the material or the vapor after a set of solids is removed from the mixture.

### Claim 4 (depends on 3)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 3 wherein the contactor/separator includes a chiller assembly for reducing the temperature of the pyrolytic vapor.

### Claim 5 (depends on 3)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 3 wherein the contactor/separator includes a first heatable distillation column for reheating and cooling the scrap polymers and elastomers, and a second heatable distillation column which separates one of either a terpene or a terpenoid extracted from the scrap polymers and elastomers.

### Claim 6 (depends on 5)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 5 wherein a small orifice is operatively disposed between the first heatable distillation column and the second heatable distillation column.

### Claim 7 (depends on 6)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 6 wherein the first heatable distillation column further comprises at least one tray.

### Claim 8 (depends on 6)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 6 further comprising a piping system for transporting a residual liquid and a residual vapor that produced, transferred, recovered, and purified by the device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone.

### Claim 9 (depends on 8)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 8 wherein the additive/catalyst is one of either a carbonates or a bicarbonate.

### Claim 10 (depends on 9)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 9 wherein the one of either a carbonates or a bicarbonate contains one of either sodium or potassium.

### Claim 11 (depends on 10)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 10 wherein the one of either a carbonates or a bicarbonate contains is potassium carbonate.

### Claim 12 (depends on 11)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 11 wherein the temperature of the scrap polymers and elastomers is about 470 degrees Centigrade.

### Claim 13 (depends on 12)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 12 wherein the device is a batch system wherein the catalyst/additive is placed in a catalyst container located above the scrap polymers and elastomers within the nitrogen blanket vacuum sealed furnace, and wherein the catalyst container is dumped and its contents dispersed over the polymers and elastomers when the polymers and elastomers reach their melting temperature.

### Claim 14 (depends on 13)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 13 wherein the catalyst/additive is not released into the nitrogen blanket vacuum sealed furnace until the nitrogen blanket vacuum sealed furnace is at a temperature of about 200 degrees centigrade.

### Claim 15 (depends on 12)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 12 wherein the device is a continuous system wherein the catalyst/additive and the scrap polymers and elastomers are blended together in the nitrogen blanket vacuum sealed furnace wherein the scrap nitrogen blanket vacuum sealed furnace includes a material displacement device for moving the scrap polymers and elastomers through the nitrogen blanket vacuum sealed furnace.

### Claim 16 (depends on 15)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 15 wherein the material displacement device for moving material through the nitrogen blanket vacuum sealed furnace in substantially in the shape of a tube within which a screw moves the scrap polymers and elastomers through the nitrogen blanket vacuum sealed furnace.

### Claim 17 (depends on 16)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 16 further comprising a broad spectrum ultraviolet lamp to irradiate the residual liquid for a period of between two hours and four hours to increase the concentration a pyrolytic oil that is produced using the device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone.

### Claim 18 (depends on 17)

The device for the pyrolysis of tires to form pyrolytic oils containing limonene and pulegone in accordance with claim 17 further comprising a refrigeration system to remove excess heat generated from the use of the broad spectrum ultraviolet lamp on the pyrolytic oil.
