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Supercritical CO2 Extraction Method for Black Pepper Oil

pepper oil supercritical CO2 extraction equipment
Black pepper oil CO2 extraction equipment

Black pepper oil extraction method

The extraction of black pepper oleoresin is mostly based on solvent extraction, supplemented by ultrasonic and microwave.

Although the solvent extraction method has a large processing capacity, it has disadvantages such as large solvent consumption, long extraction time, damage to active ingredients and residual organic solvents.

Supercritical CO2 extraction is usually carried out at low temperature, which can effectively prevent the oxidation and dissipation of heat-sensitive components; CO2 is a gas under normal conditions and is non-toxic. The extracted components are easily removed after separation, and there is no solvent residue at all, which effectively solves the traditional extraction.

Supercritical CO2 extraction method
Black pepper oil CO2 extraction equipment

Best black pepper oil CO2 extraction process

  • Extraction temperature: 42°C.
  • Extraction pressure: 340bar.
  • Extraction time: 120 minutes.
  • Granularity: 30-50 mesh.
Supercritical CO2 extraction process
Black pepper oil CO2 extraction equipment

Determination of the Best CO2 Extraction Method for Black Pepper Oil

The yield of black pepper essential oil first increases with the increase in temperature, reaching the maximum at 42°C, and the temperature continues to rise, but the yield of essential oil decreases. Considering comprehensively, the optimal temperature is selected as 42°C.

As the pressure increases, the yield of black pepper essential oil also increases. When the extraction pressure is 34 MPa, the yield reaches the maximum value of 6.46%. The extraction pressure continues to increase, but the yield decreases, so supercritical The best choice for CO2 extraction of black pepper essential oil is 34 MPa.

With the extension of the extraction time, the yield of black pepper essential oil gradually increased, but after the extraction time was 120 minutes, if the extraction time continued to be extended, the extraction yield increased little. Therefore, the optimal extraction time is 120 minutes.

The particle size decreases, the specific surface area increases, the contact area between the particles and the fluid increases, and the mass transfer path of the solute from the particle interior to the fluid becomes shorter. Therefore, the particle size decreases and the extraction rate increases.

However, too fine particle size may aggravate the back-mixing phenomenon of the bed and adversely affect the extraction. Therefore, there is an optimal particle size range.

The particle size range of 30-50 mesh is recommended.

Supercritical CO2 extraction method
Black pepper oil CO2 extraction equipment

A total of 48 aroma substances were identified in the black pepper oleoresin extracted by supercritical CO2.

Among them, in the black pepper oleoresin obtained by supercritical CO2 extraction, a total of 22 aroma components were identified. The main compounds are 0-alcoene (4.81%), 3-elemene (11.00%), and plant elemene (1.48%), ielemene (57.70%), cis-farnesene (3.26%), g-bisabolene (2.20%), nucleolenol (1.61%), piperine⑴.09% ).

Oleoresin is a resinous product that is viscous, slightly darker in color, and contains essential oils extracted from crushed spices by appropriate methods. Almost all aroma and taste components in spices can be extracted. In addition to essential oils, there are also Containing non-volatile spicy ingredients, fats, pigments and other substances that can be dissolved in solvents, these substances can represent the effective ingredients in spices, and their aroma and taste are more balanced, complete and fuller than essential oils.

In addition to aroma substances, black pepper oleoresin also contains pyrrolidine amide alkaloids-piperine.

black pepper oil co2 extraction machine
black pepper oil co2 extraction equipment
ConfigurationParameter
Extraction vesselVolume: customized according to customer requirements, generally 100ml-1000l
Working pressure: 35MPa-100MPa adjustable
Working temperature: room temperature -85℃ adjustable
3 extraction vessels recommended for production equipment
SeparatorVolume: Configured according to the volume of the extraction kettle, generally 50ml-800l
Working pressure: 10MPa-30MPa adjustable
Working temperature: room temperature -85℃ adjustable
Recommend 3 separation kettles
Working pressure: 16MPa
Gas storage tankVolume: According to the overall plan configuration, generally 10l-6000l
Working pressure: 9.9MPa
PumpCO2 high pressure pump and carrier pump, with adjustable flow and pressure
Production equipment equipped with 2 high-pressure pumps
Heat Exchange SystemWorking pressure: 35MPa-100MPa
Working temperature: adjustable from room temperature to 90℃
Refrigeration system5℃-10℃
Security systemThe high pressure pump and the inlet and outlet of all containers are equipped with overpressure protection device, the safety interlocking device is connected with the PLC control system and the safety valve to ensure the safety of the system

Further reading

CO2 Extractio Method

There are a total of 7 processes in the common CO2 extraction method:

  1. Biomass drying
  2. Grinding
  3. Fill Biomass
  4. Pressurize with CO2
  5. Run in Closed Loop
  6. Periodically
  7. Depressurize
supercritical CO2 extraction method
supercritical CO2 extraction process diagram
Supercritical CO2 extraction method
Low temperature drying for roses

Biomass (flowers, leaves, seeds, rhizomes, etc.) is much easier to buck when it includes less than 10% moisture.
Dry biomass to moisture content below 10%.
As an alternative to machinery, many farmers let their crops dry in the field. This works well as long as the harvest time is cool and dry.

Supercritical CO2 extraction method
Grinding for cannabis

Once the biomass has been dried, it is granulated. In general, smaller particles (30-80 mesh) are desirable and tighter particle diameter distributions are better for extraction throughput.
Important: Before grinding (pulverizing) large chunks of biomass, it needs to be divided into flakes and sent to a pulverizer for grinding. This avoids the high temperature generated by the high-speed pulverization of biomass in the pulverizer, which destroys the characteristics of the extract and loses part of the essential oil.

CO2 extractor
CO2 extracting kettle

Load Extraction Vessel with biomass.

Bring each vessel to working pressure using CO2 from supply cylinders.

In Extraction Vessel, compounds are pulled from biomass into solution.
Solvent (CO2) is boiled out of solution in Separator 1.
Evaporated CO2 is condensed into liquid and stored in Accumulator.

Supercritical CO2 extraction method
Supercritical CO2 extraction method

Open valve on the separator to collect extract.

After allotted run time, system is depressurized by releasing CO2 through Separator 3.

Black pepper oil supercritical CO2 extraction equipment
Black pepper oil supercritical CO2 extraction equipment

Black pepper oil

Piper nigrum L.

Black Peppercorns

Supercritical Fluid Extraction Process (SCFE) also called Co2 Extraction process.

Black pepper seeds, black pepperInline with oleoresin of black pepper.

The black pepper essential oil produced by the supercritical extraction process is one of the highest quality black pepper essential oils. This oil is free from solvent, pesticide residues and heavy metal traces and therefore is ideal for high quality pharmaceutical, cosmetic, cosmoceutical, nutraceutical formulations and food products.

Black pepper Eessential oil is extracted from berries of black pepper and light greenish in appearance.

Supercritical CO2 fluid extraction of black pepper oil
  • Black peppercorns contain compounds called alkaloids and one of most important is piperine.
  • It acts as a central nervous system depressant and suppresses fever and pain.
  • It is known to be anti-inflammatory and insecticidal.
  • It is known to cause skin pigmentation and is used in vitiligo.

Pepper is one of the oldest and the world’s most important spice.
It is the dried fruit of Piper nigrum L.

Native of Madagascar and Malabar Coast of South Western India, pepper is also known as the King of Spices. The berries start turning from red to black as they mature, black pepper is dried, developed unripe fruit.

black pepper oil co2 extraction equipment
black pepper oil co2 extraction equipment
  • Pepper can be used in tonic and is also used as a flavour ingredient in food products.
    In meat products it is used for curing and preserving.
  • The fruits are acrid, bitter, carminative, aphrodisiac, diuretic, digestive and stimulant. They are of use in arthritis, asthma, fever, cough, dysentery, dyspepsia, obesity and flatulence by aiding in digestion.
  • Black pepper oil is also good for muscle aches and pain.
  • Black Pepper’s woody warm aroma comes from the volatile oils found mostly in the flesh and skin. The pungency of its bite comes from the alkaloids and resins found in seeds. The essential oil goes into perfumes and flavourings. It is used for reducing stomach and intestinal gas and has been found to stimulate the activities of the heart and kidneys.
  • Piperine also works as an insecticide against houseflies and is used for spraying against different types of pests in gardening.
  • Cubeb pepper comprises of substances that are carminative, antiseptic, and diuretic. Since these substances relieves throat inflammation cubeb oil is used in throat Lozenges.

Black pepper blends well with rosemary, lavender, frankincense, sandalwood, marjoram, and other spices. As for safety, black pepper is non-sensitizing and non-toxic. In high concentrations it may be an irritant and redden the skin.

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