# US 11,993,560 B2 · Alcohol solvent recovery and plant oil decarboxylation apparatus and method

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- Number: US 11,993,560 B2
- Document ID: US11993560B2
- Status: Granted
- Kind: B2
- Application number: 17/242,388
- Filed: 2021-04-28
- Published: 2021-11-25
- Granted: 2024-05-28
- Earliest claimed: 2020-05-20
- Assignees: MACH Technologies
- Applicants: MACH Technologies
- Inventors: Robert N. Wirtz; Jason T. Wirtz; John W. Wirtz, II
- Web page: https://patentgrep.com/patent/US11993560B2

## CPC

- B01D 11/0292: {Treatment of the solvent}
- C07C 29/84: by extractive distillation
- B01D 3/002: {by continuous methods}
- B01D 3/145: {One step being separation by permeation}
- B01D 11/0288: {Applications, solvents}
- B01D 11/0296: {Condensation of solvent vapours (condensation in general B01D5/00)}
- B01D 19/00: Degasification of liquids
- B01D 61/027: {Nanofiltration}
- B01D 61/0271: {comprising multiple nanofiltration steps}
- B01D 61/18: Apparatus therefor
- B01J 19/0013: {Controlling the temperature of the process}
- B01J 19/0066: {Stirrers (mixing per se B01F)}
- B01J 19/18: Stationary reactors having moving elements inside (B01J19/08, B01J19/26 take precedence)
- B01J 19/2445: {placed in parallel}
- B01J 19/2465: {externally, i.e. the mixture leaving the vessel and subsequently re-entering it}
- B01J 19/2475: {Membrane reactors}
- C07C 29/76: by physical treatment
- C07C 29/88: by treatment giving rise to a chemical modification of at least one compound (chemisorption C07C29/76)
- B01J 2219/00029: Batch processes
- B01J 2219/00087: with heat exchange elements outside the reactor
- B01J 2219/00123: adding a temperature modifying medium to the reactants
- B01J 2219/00162: controlling the pressure
- 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)
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## Abstract

A method of and apparatus for recovering an alcohol solvent from a liquid mixture of the solvent and plant oil and decarboxylating the plant oil may include, pressurizing the liquid mixture to a super-atmospheric pressure, recirculating the pressurized liquid mixture a plurality of times through at least one membrane separator to separate some of the solvent from the mixture to provide a concentrated mixture of the plant oil with less solvent, reducing the pressure of the liquid concentrated mixture to less than 15 psig, heating it at a pressure of less than 15 psig to a temperature sufficient to vaporize the solvent in the concentrated mixture, removing sufficient heat from the vaporized solvent to condense it to a liquid solvent at atmospheric pressure and temperature conditions, and heating the plant oil to a temperature desirably of at least 215° F. to decarboxylate the plant oil.

## Claims

### Claim 1

An apparatus for recovering an alcohol solvent from a mixture of the solvent and plant oil and decarboxylation of the plant oil, the apparatus comprising;
at least one tank configured to receive a liquid mixture of an alcohol solvent and plant oil;
at least one membrane separator configured to separate at least some of the solvent from the liquid mixture when flowing through the at least one membrane separator to provide a concentrated mixture with less solvent therein compared to the liquid mixture, wherein the at least one membrane separator further comprises a coiled or spiral wound membrane received in a super-atmospheric pressure resistant cylindrical housing, the cylindrical housing being resistant to a super-atmospheric pressure of at least 500 psig;
a pump configured to circulate the liquid mixture through the at least one membrane separator and the at least one tank a plurality of times, wherein the pump is configured to supply the liquid mixture to the at least one membrane separator at a pressure of at least 500 psig;
a reactor configured to heat the concentrated mixture to a temperature high enough to vaporize substantially all of the solvent in the concentrated mixture and to a temperature high enough to decarboxylate the plant oil;
a heat exchanger configured to decrease the temperature of the vaporized solvent sufficiently to condense it to be a liquid at atmospheric pressure and temperature; and
an actuated outlet valve associated with the at least one tank, through which the liquid mixture is supplied from the at least one tank through the actuated outlet valve to the pump and the liquid mixture is returned to and through the at least one tank to an inlet of the pump.

### Claim 2 (depends on 1)

The apparatus of claim 1 which also comprises a pressure reducer configured to decrease the pressure of the concentrated mixture downstream of the at least one membrane separator and through the at least one tank to a pressure not greater than 15 psig.

### Claim 3 (depends on 1)

The apparatus on claim 1 which also comprises a heat exchanger downstream of the at least one membrane separator and upstream of the pump which is configured to remove heat from the concentrated mixture.

### Claim 4 (depends on 3)

The apparatus of claim 3 wherein the heat exchanger is configured to decrease the temperature of the concentrated mixture flowing through it by at least 9° F.

### Claim 5 (depends on 1)

The apparatus on claim 1 wherein the pump is configured to recirculate the liquid mixture through the at least one membrane separator at least until a ratio by volume in the concentrated mixture of the solvent to the plant oil is not greater than 5 parts solvent to 1 part plant oil.

### Claim 6 (depends on 1)

The apparatus of claim 1 which also comprises a vacuum pump configured to apply a vacuum to the reactor and the heat exchanger to facilitate flow of the vaporized solvent from the reactor and into the heat exchanger.

### Claim 7 (depends on 1)

The apparatus of claim 1 which also comprises a solvent tank configured to receive liquid solvent from the heat exchanger downstream of the reactor, and a vacuum pump configured to apply a vacuum to the reactor, the heat exchanger, and the solvent tank to facilitate the flow of vaporized solvent from the reactor into this downstream heat exchanger and liquid solvent from this downstream heat exchanger into the solvent tank.

### Claim 8 (depends on 1)

The apparatus of claim 1 which also comprises another pump configured to transfer liquid solvent from the solvent tank.

### Claim 9 (depends on 1)

The apparatus of claim 1 which also comprises a recovered solvent tank configured to receive the separated liquid solvent from the at least one membrane separator.

### Claim 10 (depends on 7)

The apparatus of claim 7 which also comprises a recovered solvent tank configured to receive the separated liquid solvent from the at least one membrane separator and receive liquid solvent from the solvent tank configured to receive liquid solvent from the heat exchanger.

### Claim 11 (depends on 1)

The apparatus of claim 1 which also comprises a heat exchanger configured to heat to an elevated temperature the concentrated mixture supplied to the reactor.

### Claim 12 (depends on 1)

The apparatus of claim 1 which also comprises a recovered solvent tank configured to receive the separated liquid solvent from the at least one membrane separator and receive liquid solvent from a solvent tank configured to receive liquid solvent from the heat exchanger.

### Claim 13 (depends on 1)

The apparatus of claim 1 which also comprises a pressure reducer downstream of the at least one membrane separator configured to decrease a pressure of the concentrated mixture to not greater than 15 psig and a tank downstream of the pressure reducer and upstream of the reactor configured to receive the concentrated mixture from the pressure reducer.

### Claim 14 (depends on 1)

The apparatus of claim 1 wherein the reactor is configured for heating the plant oil therein to a temperature of at least 215° F. for decarboxylation of the plant oil.

### Claim 15 (depends on 1)

The apparatus of claim 1 wherein the at least one tank comprises a first tank and a second tank each configured to alternate with the other to supply a separate batch of liquid mixture of solvent and plant oil to the pump for circulation of such batch through the at least one membrane separator and the tank associated with such batch.

### Claim 16 (depends on 1)

The apparatus of claim 1, wherein the reactor is configured to first heat the concentrated mixture to a temperature high enough to vaporize substantially all of the solvent and then configured to heat the plant oil to a temperature high enough to decarboxylate the plant oil.

### Claim 17 (depends on 1)

A method of recovering an alcohol solvent from a mixture of the solvent and plant oil and decarboxylating the plant oil by using the apparatus recited in claim 1 comprising:
pressurizing a liquid mixture of an alcohol solvent and plant oil to a super-atmospheric pressure of at least 500 psig;
recirculating the pressurized liquid mixture, a plurality of times through at least one membrane separator to separate some of the solvent from the mixture to provide a liquid concentrated mixture of the plant oil with less solvent in the concentrated mixture;
reducing the pressure of the liquid concentrated mixture to less than 15 psig;
heating the liquid concentrated mixture at a pressure of less than 15 psig to a temperature sufficient to vaporize the solvent in the liquid concentrated mixture;
removing sufficient heat from the vaporized solvent to condense the vaporized solvent to be a liquid solvent at atmospheric pressure and temperature conditions; and
heating the plant oil resulted from the liquid concentrated mixture after removing the vaporized solvent to a temperature of at least 215° F. to decarboxylate the plant oil.

### Claim 18 (depends on 17)

The method of claim 17 wherein the pressurized liquid mixture is recirculated through the at least one membrane separator a sufficient number of times for the liquid mixture to have a ratio by volume of not more than 5 parts of solvent to 1 part of plant oil.

### Claim 19 (depends on 17)

The method of claim 17 wherein the liquid concentrated mixture is heated in a reactor to vaporize the solvent in the mixture and also comprises applying a vacuum to the reactor to remove the vaporized solvent from the reactor.

### Claim 20 (depends on 17)

The method of claim 17 which also comprises heating the liquid concentrated mixture to a temperature of at least 150° F. and passing it into a reactor, in the reactor heating the liquid concentrated mixture to a higher temperature to vaporize substantially all of the solvent in the liquid concentrated mixture, removing the vaporized solvent from the reactor and heating the plant oil remaining in the reactor to a high enough temperature for a period of time of at least 15 minutes to decarboxylate the plant oil.