Extraction method and operation process
Turn on the main power, heating, cooling and cold cycle switches of the supercritical extraction device, add rosemary leaves to the extraction tank, add entrainer, and pass CO2.
After the set temperature and pressure are balanced, start the high-pressure pump, adjust the communication valve between the extraction tank and the separator I and the separator II to keep it at the required pressure and start timing.
When the extraction is over, turn off the high-pressure pump, heating, cooling, cold cycle, and main power switches in order. The discharge valve of separator I discharges solid rosemary antioxidant and the discharge valve of separator II releases Liquid rosemary essential oil and entrainer.
Adjust the communication valve between the extraction tank and the separator I and the separator II.
After the pressure is balanced, make part of the CO return to the cylinder. Close the related communication valve, open the drain valve, open the extraction tank, and take the rosemary leaf residue
Analysis of influencing factors of supercritical Co2 extraction (SCDE)
Therefore, only the effect of SCDE factors on the yield of antioxidants was studied.
According to preliminary experiments, factors such as extraction and separation temperature, extraction pressure, extraction time, and amount of entrainer are considered to be the main influencing factors of the rosemary antioxidant SCDE.
Therefore, a 4 factor and 3 level test scheme was designed. The extraction temperature refers to The water bath temperature of the extraction tank, the separation temperature refers to the water bath temperature of the separator I, and the water bath temperature of the separator II is fixed to 40 l; the extraction pressure refers to the pressure of the extraction tank, and the pressure of the separator I and the separator II are both 4 ~ 5 MPa; fixed circulation flow rate; rosemary leaves are crushed, and the feeding scale is 50g.
The preferred conditions for supercritical Co2 extraction (SCDE) of rosemary essential oil and antioxidants are: extraction time 4 h, mass ratio of entrainer 95% ethanol to rosemary leaves 2: 5, temperature of extraction tank and separator I The temperature is 50°C and 70°C, the temperature of separator II is 40°C, the extraction pressure is 20 MPa, and the separation pressure is 4 to 5 MPa.
Average yield of rosemary oiO was 1.80 % .
Resultr of ccnstituent analysia of rosemary oit ohowed that the essentiat oit mainly ccntains 1,8-cineeIe, camphor, a-terpineoI, borneel, verbenone, terpinen-4-oI, bornyS acctate and linaloI.
Average yield oS rosemary antioxidant was 11.93 % .
Main active ccmponentr oS rosemary antioxidant were ccrnosic acid, ccrnosol, and rosmarinic acid, whose ccntentr were 23.61 % , 7.33% and 5. 13 % , respectively.
- Pulverization degree: 50 mesh
- Extraction pressure: 20 MPa
- Extraction temperature: 40°C
- Extraction time: 240 min
- Separate pressure I: 5 MPa
- Separate I temperature: 70°C
- Separate pressure II: 4 MPa
- Separate II temperature: 40°C