# US 4,400,398 A · Method for obtaining aromatics and dyestuffs from bell peppers

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- Number: US 4,400,398 A
- Document ID: US4400398A
- Status: Granted
- Kind: A
- Application number: 06/365,473
- Filed: 1982-04-05
- Granted: 1983-08-23
- Earliest claimed: 1981-04-10
- Assignees: Fried. Krupp Gesellschaft mit beschrankter Haftung
- Inventors: Hubert Coenen; Rainer Hagen; Manfred Knuth
- Web page: https://patentgrep.com/patent/US4400398A

## CPC

- B01D 11/0203: {with a supercritical fluid}
- A23L 5/43: using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
- A23L 27/11: {obtained by solvent extraction}
- 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)
- A23L: FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF (preservation thereof A23B)

## Abstract

Method for obtaining aromatics and/or dyestuffs from bell peppers wherein red pepper is extracted with a solvent which is in a supercritical state and is gaseous under normal conditions. The extraction takes place at a pressure of &gt;P.sub.k to 350 bar and a temperature of &gt;T.sub.k to 70.degree. C. The extracted aromatics and/or dyestuffs are separated from the separated supercritical gas phase by lowering the density of the gas phase.

## Claims

### Claim 1

Process for treating bell peppers which contain aromatics and dyestuffs by extraction of the peppers with a solvent, comprising:
extracting dried, comminuted red pepper with a solvent which is in the supercritical state with respect to pressure and temperature and which under normal conditions is a gas, at a pressure of &gt;p.sub.k to 350 bar and a temperature of &gt;T.sub.k to 70.degree. C. to form (a) a charged supercritical gas phase containing an extract which comprises at least the aromatics or the dyestuffs and (b) an extraction residue;
separating the charged supercritical gas phase from the extraction residue; and
separating the extract from the separated, charged supercritical gas phase by a reduction in the density of the gas phase.

### Claim 2 (depends on 1)

Process as defined in claim 1, wherein carbon dioxide, ethane, ethene or a mixture of ethane and ethene is used as the gaseous solvent.

### Claim 3 (depends on 1, 2)

Process as defined in claim 1 or 2, wherein the gaseous solvent contains an entrainer.

### Claim 4 (depends on 3)

Process as defined in claim 3, wherein the entrainer is ethanol.

### Claim 5 (depends on 1, 2)

Process as defined in claim 1 or 2, wherein the density of the charged supercritical gas phase is lowered by a reduction of the pressure.

### Claim 6 (depends on 1, 2)

Process as defined in claim 1 or 2, wherein the density of the charged supercritical gas phase is lowered by a reduction of the pressure and a change in temperature.

### Claim 7 (depends on 1, 2)

Process as defined in claim 1 or 2, wherein:
the dried and comminuted pepper is extracted in a first extraction stage with a gaseous solvent which is in the supercritical stage at a pressure of &gt;p.sub.k to 150 bar to form (a) a first charged supercritical gas phase containing aromatics and (b) a first extraction residue which is pepper free of aromatics,
the first charged supercritical gas phase is separated from the first extraction residue,
the extracted aromatics are separated from the charged supercritical gas phase of the first extraction stage,
the pepper which is free of aromatics is extracted in a second extraction stage with a gaseous solvent which is in the supercritical state at a pressure from 150 to 350 bar to and form (a) a second charged supercritical gas phase containing dyestuffs and (b) a second extraction residue, and
the second charged supercritical gas phase is separated from the second extraction residue, and
the extracted dyestuffs are separated from the separated, charged, supercritical gas phase of the second extraction stage.

### Claim 8 (depends on 7)

Process according to claim 7, wherein the same gaseous solvent is used in both extraction stages.

### Claim 9 (depends on 1, 2)

Process as defined in claim 1 or 2, wherein:
the dried and comminuted pepper is extracted at 150 to 350 bar to obtain (a) a charged supercritical gas phase containing aromatics and dyestuffs and (b) an extraction residue,
the charged supercritical gas phase containing aromatics and dyestuffs is separated from the extraction residue,
first the dyestuffs are separated, in at least one fraction, from the separated, charged, supercritical gas phase by stepwise reduction of the density of the gas phase, and
then the aromatics are separated, in at least one fraction, from the separated, charged, supercritical gas phase by stepwise reduction of the density of the gas phase.

### Claim 10

Process for obtaining dyestuffs from bell peppers which are substantially free of capsaicin by extraction of the peppers with a solvent, comprising:
extracting dried, comminuted red pepper which is substantially free of capsaicin in an extraction stage with a solvent which is in the supercritical state with respect to pressure and temperature and which under normal conditions is a gas, at a pressure of 150 to 350 bar and a temperature of &gt;T.sub.k to 70.degree. C. to form (a) a charged supercritical gas phase containing extracted dyestuff and (b) an extraction residue;
separating the charged supercritical gas phase from the extraction residue; and
separating the extracted dyestuffs from the separated, charged supercritical gas phase by a reduction in the density of the gas phase.

### Claim 11 (depends on 10)

Process as defined in claim 10, wherein carbon dioxide, ethane, ethene or a mixture of ethane and ethene is used as the gaseous solvent.

### Claim 12 (depends on 10, 11)

Process as defined in claim 10 and 11, wherein the gaseous solvent contains an entrainer.

### Claim 13 (depends on 12)

Process as defined in claim 12, wherein the entrainer is ethanol.

### Claim 14 (depends on 10, 11)

Process as defined in claim 10 to 11, wherein the density of the charged supercritical gas phase is lowered by a reduction of the pressure.

### Claim 15 (depends on 10, 11)

Process as defined in claim 10 or 11, wherein the density of the charged supercritical gas phase is lowered by a reduction of the pressure and a change in temperature.

### Claim 16

Process for treating paprika oleoresin which contains aromatics and dyestuffs by extraction of the paprika oleoresin with a solvent, comprising:
extracting paprika oleoresin with a solvent which is in the supercritical state with respect to pressure and temperature and which under normal conditions is a gas, at a pressure of &gt;p.sub.k to 350 bar and a temperature of &gt;T.sub.k to 70.degree. C. to form (a) a charged supercritical gas phase containing an extract which comprises at least the aromatics and (b) an extraction residue which comprises at least the dyestuffs;
separating the charged supercritical gas phase from the extraction residue, and
separating the extract from the separated, charged supercritical gas phase by a reduction in the density of the gas phase.

### Claim 17 (depends on 16)

Process as defined in claim 16, wherein carbon dioxide, ethane, ethene or a mixture of ethane and ethene is used as the gaseous solvent.

### Claim 18 (depends on 16, 17)

Process as defined in claim 16 or 17, wherein the gaseous solvent contains an entrainer.

### Claim 19 (depends on 17)

Process as defined in claim 17, wherein the entrainer is ethanol.

### Claim 20 (depends on 16, 17)

Process as defined in claim 16 to 17, wherein the density of the charged supercritical gas phase is lowered by a reduction of the pressure.

### Claim 21 (depends on 16, 17)

Process as defined in claim 16 or 17, wherein the density of the charged supercritical gas is lowered by a reduction of the pressure and a change in temperature.

### Claim 22 (depends on 16, 17)

Process as defined in claim 16 or 17, wherein:
the paprika oleoresin is extracted in a first extraction stage with a gaseous solvent which is in the supercritical state at a pressure of &gt;p.sub.k to 150 bar to form (a) a first charged supercritical gas phase containing aromatics and (b) a first extraction residue which is paprika oleoresin free of aromatics,
the first charged supercritical gas phase is separated from the first extraction residue,
the extracted aromatics are separated from the charged supercritical gas phase of the first extraction stage,
the paprika oleoresin which is free of aromatics is extracted in a second extraction stage with a gaseous solvent which is in the supercritical state at a pressure from 150 to 350 bar to form (a) a second charged supercritical gas phase and (b) a second extraction residue,
the second charged supercritical gas phase is separated from the second extraction residue, and
the extracted dyestuffs are separated from the separated, charged, supercritical gas phase of the second extraction stage.

### Claim 23 (depends on 21)

Process according to claim 21, wherein the same gaseous solvent is used in both extraction steps.

### Claim 24 (depends on 16, 17)

Process as defined in claim 16 or 17, wherein:
the paprika oleoresin is extracted at 150 to 350 bar to obtain (a) a charged supercritical gas phase containing aromatics and dyestuffs and (b) an extraction residue,
the charged supercritical gas phase containing aromatics and dyestuffs is separated from the extraction residue,
first the dyestuffs are separated, in at least one fraction, from the separated, charged, supercritical gas phase by stepwise reduction of the density of the gas phase, and
then the aromatics are separated, in at least one fraction, from the separated, charged, supercritical gas phase by stepwise reduction of the density of the gas phase.

### Claim 25 (depends on 16, 17)

Process according to claim 16 or 17, wherein the extraction is conducted at a pressure of &gt;p.sub.k to 150 bar to extract aromatics into the supercritical gas phase.
