# US 11,305,254 B2 · Process and system for producing pulp, energy, and bioderivatives from plant-based and recycled materials

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- Number: US 11,305,254 B2
- Document ID: US11305254B2
- Status: Granted
- Kind: B2
- Application number: 16/802,651
- Filed: 2020-02-27
- Published: 2020-06-18
- Granted: 2022-04-19
- Earliest claimed: 2015-06-11
- Assignees: Circ, LLC
- Applicants: Circ, LLC
- Inventors: Sandeep Kumar; Peter Majeranowski; Igor Kostenyuk; Iulian Bobe; Florin Barla
- Web page: https://patentgrep.com/patent/US11305254B2

## CPC

- B01J 19/0053: {Details of the reactor}
- B01D 11/0207: {Control systems}
- C10G 1/04: by extraction
- C10G 1/065: {in the presence of a solvent}
- C12M 21/12: {for producing fuels or solvents (C12M21/04 takes precedence; liquid carbonaceous fuels C10L1/00, solid fuels C10L5/00)}
- C12M 43/02: {Bioreactors or fermenters combined with devices for liquid fuel extraction; Biorefineries}
- C12P 7/10: substrate containing cellulosic material
- C12P 7/649: Biodiesel, i.e. fatty acid alkyl esters
- D21B 1/14: Disintegrating in mills
- D21C 1/02: with water or steam
- D21C 3/02: with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
- D21C 3/22: Other features of pulping processes
- D21C 5/02: Working-up waste paper (mechanical part D21B1/08, D21B1/32)
- D21C 7/00: Digesters
- D21C 11/0007: {Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for (volatile compounds obtained by decomposition of spent liquors in order to regenerate them D21C11/125; compounds obtained by fractionating the liquors in order to regenerate them D21C11/0042)}
- D21H 11/02: Chemical or chemomechanical {or chemothermomechanical} pulp
- B01J 2219/00051: Controlling the temperature
- B01J 2219/00162: controlling the pressure
- B01J 2219/00353: Pumps
- B01J 2219/00891: Feeding or evacuation
- C10G 2300/1014: of vegetal origin
- Y02E 50/10: Biofuels, e.g. bio-diesel
- Y02P 30/20: using bio-feedstock
- Y02W 30/64: Paper recycling
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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)
- 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
- C12M: APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; {APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS}
- C12P: FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE {(brewing of beer C12C; producing vinegar C12J; producing specific peptides or proteins C07K; producing enzymes C12N9/00; DNA or RNA concerning genetic engineering, vectors, e.g. plasmids, or their isolation, preparation or purification C12N15/00; measuring or testing processes involving enzymes or microorganisms C12Q; measuring or testing processes involving nucleic acid amplification reactions C12Q1/6844; fermentation processes to form a food composition, A21 or A23; compounds in general, see the relevant compound class, e.g. C01, C07)}
- D21B: FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21C: PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21H: PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- 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 presently disclosed subject matter relates to an industrial system for processing various plant materials to produce marketable materials. Particularly, the system integrates subcritical water extraction technology and includes a pre-processing module and a two-stage extractor (processing module) with constant control of temperature, pressure, and/or residence time. In some embodiments, the final product of the disclosed system can include feedstock constituents for biofuel production (sugars and/or oil), biochar, raw materials for various industries (such as pulp for manufacturing paper or cellulose for use in various industries). The disclosed system can be modular or non-modular, stationary or mobile, and can include prefabricated elements with programmed automatic or manual operation so that it can be easily moved and/or assembled on site.

## Claims

### Claim 1

A method of producing pulp comprising:
processing a feedstock into a processing size; and
using a subcritical water treatment process, treating the feedstock with a catalyst that comprises an alkaline catalyst at a concentration of about 1.5 to 10 weight percent or less in a reactor assembly having:
an operating condition at a pressure and a temperature at a constant level that is held for a defined period of time to break down carbohydrates of a first chain strength to produce a pulp product,
wherein the feedstock comprises one or more of seeds and agricultural crop wastes and residues comprising corn stover, wheat straw, rice straw, or sugar cane bagasse.

### Claim 2 (depends on 1)

The method of claim 1, wherein the method provides for continuous flow of material through the reactor such that the process provides for continuous manufacture of paper pulp product, cellulose, or combinations thereof.

### Claim 3 (depends on 1)

The method of claim 1, wherein the method is modular and scalable, stationary or mobile; and
wherein when in mobile form, a system executing the method can be mounted on one or more truck trailers, rail cars, shipping containers, other platforms used to transport from one site to another, or combinations thereof.

### Claim 4 (depends on 1)

Fiberized biomass, pulp, powdered cellulose, nano-cellulose, and dissolving cellulose produced from the method of claim 1.

### Claim 5

A method of producing a hemp bio-derivative comprising:
processing a plant-related industrial waste comprising hemp into a processing size; and
using a subcritical water treatment process, treating the plant-related industrial waste with an alkaline catalyst at a concentration of about 2.5 to 3 weight percent in a reactor assembly having:
an operating condition at a pressure and a temperature at a constant level that is held for a defined period of time to break down carbohydrates of a first chain strength to produce a pulp product.

### Claim 6 (depends on 5)

The method of claim 5, wherein the defined period of time is about 20 minutes.

### Claim 7 (depends on 5)

The method of claim 5, further comprising:
recovering cellulose from the pulp product; and
bleaching the cellulose with a bleaching agent comprising hydrogen peroxide at about 70° C.

### Claim 8 (depends on 5)

The method of claim 5, wherein the plant-related industrial waste in the reactor assembly has a concentration of about 2 to 3 weight percent.

### Claim 9 (depends on 5)

The method of claim 5, wherein the pressure is about 90 psi to 200 psi, and wherein the temperature is about 160° C. to 180° C.

### Claim 10

A system comprising:
a pre-processing portion having a mechanical processor/material handler for a preparation of feedstock material comprising hemp; and
an extractor portion comprising a reactor assembly to which the feedstock material and subcritical water is supplied, the reactor assembly having:
an operating condition at a pressure and a temperature at a constant level that is held for a defined period of time to break down carbohydrates of a first chain strength;
an assembly of one or more reactor(s) comprising continuous-type reactor(s) or batch-type reactor(s) followed by one or more pressure control valve(s);
heat exchangers for cooling down the output from the one or more reactor(s); and
separators to collect material from a water phase and consequently recycle the water.

### Claim 11 (depends on 10)

The system according to claim 10, further including:
a high pressure pump for increasing a pressure in the system, wherein a variable speed and flow rate are provided;
a pressure control valve for maintaining pressure in the operating condition; and
a heating element for providing direct heating or indirect heating.

### Claim 12 (depends on 10)

The system according to claim 10, wherein the operating condition comprises a pressure of about 0-300 psi and temperature of up to about 180° C.

### Claim 13 (depends on 10)

The system of claim 10,
wherein the pre-processing and the operating condition are controlled and monitored by a centralized computer software able to maintain constant a desired pressure, temperature, and flow rate for a desired period of time;
wherein the system comprises multiple sensors that are installed and connected to centralized computer managing software comprising a network in which technical information about major parameters such as pressure, temperature, flow, content level, is collected in real time, relayed to a managing system, and analyzed;
wherein the above parameters are controlled and modified in real time.

### Claim 14 (depends on 10)

The system of claim 10, wherein the system is configured to produce one or more of fiberized biomass, pulp, cellulose, and raw materials for industrial commodities as its final product.

### Claim 15 (depends on 10)

The system of claim 10, wherein the system is modular and scalable, stationary or mobile; wherein when in mobile form, the system can be mounted on one or more truck trailers, rail cars, shipping containers, other platforms used to transport from one site to another, or combinations thereof.

### Claim 16

A method of producing pulp comprising:
processing a feedstock into a processing size; and
using a subcritical water treatment process, treating the feedstock with a catalyst that comprises an alkaline catalyst at a concentration of about 1.5 to 10 weight percent or less in a reactor assembly having:
an operating condition at a pressure and a temperature at a constant level that is held for a defined period of time to break down carbohydrates of a first chain strength to produce a pulp product,
wherein the feedstock comprises hemp.