Search

CN-122012176-A - Double-zero double-low deodorization and byproduct efficient recovery method for sunflower seed oil

CN122012176ACN 122012176 ACN122012176 ACN 122012176ACN-122012176-A

Abstract

The invention relates to the technical field of edible oil processing, and discloses a double-zero double-low deodorization and byproduct efficient recovery method for sunflower seed oil. The extracted phase sequentially passes through a multistage analysis system, namely a refined sunflower seed oil finished product is separated out through depressurization and cooling in a first stage analysis kettle, the refined sunflower seed oil finished product is converted into a subcritical state in a second stage analysis kettle, the beta-CD-PU porous crosslinked microspheres filled in the second stage analysis kettle are utilized for selectively intercepting and separating out phytosterol, the vitamin E is separated out through depressurization in a third stage analysis kettle, and finally the refined sunflower seed oil finished product enters a flash tank for gasifying carbon dioxide, so that free fatty acid and peculiar smell micromolecule leftovers are separated out. The invention avoids the loss of nutrient components and the generation of trans-fatty acid caused by high-temperature deodorization, and realizes the gradual and accurate separation and independent recovery of grease deodorization and various byproducts.

Inventors

  • GUO KUNPENG

Assignees

  • 山东圣道尔农业科技发展有限公司

Dates

Publication Date
20260512
Application Date
20260408

Claims (10)

  1. 1. The double-zero double-low deodorization and byproduct efficient recovery method for sunflower seed oil is characterized by comprising the following steps of: pumping the degummed pretreatment crude oil into the middle part of an extraction tower continuously, pumping high-pressure pure carbon dioxide fluid into the bottom of the extraction tower for supercritical extraction, and collecting a supercritical extraction phase discharged from the top of the extraction tower; Introducing a supercritical extraction phase discharged from the top of the extraction tower into a first-stage analysis kettle, reducing the pressure and the temperature, and collecting refined sunflower seed oil finished products separated from the bottom of the first-stage analysis kettle; Introducing the carbon dioxide fluid containing byproducts discharged from the top of the first-stage analysis kettle into a second-stage analysis kettle filled with beta-CD-PU porous crosslinked microspheres, reducing the pressure and the temperature to convert the carbon dioxide fluid containing byproducts into subcritical fluid, and collecting plant sterol enriched matters separated out from the bottom of the second-stage analysis kettle; Introducing the fluid in the subcritical state flowing out of the second-stage analysis kettle into a third-stage analysis kettle, reducing the pressure, and collecting vitamin E enriched matters separated out from the bottom of the third-stage analysis kettle; and (3) introducing the fluid flowing out of the third-stage desorption kettle into a flash tank, reducing the pressure and the temperature to gasify the carbon dioxide, and collecting free fatty acid and peculiar smell micromolecular offcuts separated out from the bottom of the flash tank.
  2. 2. The method for double zero double low deodorization and high-efficiency recovery of byproducts of sunflower seed oil according to claim 1, wherein the step of degumming the pressed sunflower seed crude oil before pumping into an extraction tower comprises the following steps: Heating the crude sunflower seed oil obtained by squeezing to 45-55deg.C, adding deionized water with an amount of 1.5-2.5% of the crude sunflower seed oil obtained by squeezing and citric acid aqueous solution with an amount of 45-55wt% of the crude sunflower seed oil obtained by squeezing with an amount of 0.05-0.15% of the crude sunflower seed oil obtained by squeezing, and mechanically stirring for 25-35min; and (3) delivering the stirred crude sunflower seed oil into a centrifuge for centrifugal separation to remove heavy-phase colloid, thereby obtaining the degumming pretreatment crude oil.
  3. 3. The method for double zero double low deodorization and high-efficiency recovery of byproducts of sunflower seed oil according to claim 1, wherein the conditions for controlling supercritical extraction are as follows: The pressure in the extraction tower is 30-35MPa, the temperature is 45-55 ℃, and the mass ratio of the high-pressure pure carbon dioxide fluid to the degummed pretreatment crude oil is (25-35): 1.
  4. 4. The method for double zero double low deodorization and high-efficiency recovery of byproducts of sunflower seed oil according to claim 1, wherein the pressure in the first-stage analysis kettle is controlled to be reduced to 20-25MPa, and the temperature is controlled to be 45-50 ℃; In the second-stage analysis kettle, the pressure in the second-stage analysis kettle is controlled to be reduced to 12-15MPa, and the temperature is controlled to be reduced to 25-30 ℃.
  5. 5. The method for double zero double low deodorization and high-efficiency recovery of byproducts of sunflower seed oil according to claim 1, wherein the pressure in the third-stage analysis kettle is controlled to be reduced to 8.0-10MPa, and the temperature is maintained at 25-30 ℃; In the flash tank, the pressure in the flash tank is controlled to be reduced to 3.0-4.0MPa, and the temperature is controlled to be 35-40 ℃.
  6. 6. The method for double zero double low deodorization and efficient recovery of byproducts of sunflower seed oil according to claim 1, further comprising the steps of: condensing the gaseous carbon dioxide discharged from the top of the flash tank, delivering the condensed gaseous carbon dioxide into a compressor unit for pressurization to 30-35MPa and heating to 45-55 ℃, and returning the condensed gaseous carbon dioxide to the bottom of the extraction tower for recycling.
  7. 7. The sunflower seed oil double-zero double-low deodorization and byproduct efficient recovery method according to claim 1, wherein the beta-CD-PU porous crosslinked microsphere is prepared by the raw material crosslinking reaction of the following parts by weight: 100 parts of anhydrous beta-cyclodextrin; 15-20 parts of polyethylene glycol; 45-55 parts of hexamethylene diisocyanate; 0.5-1.0 parts of dibutyl tin dilaurate.
  8. 8. The method for double zero double low deodorization and high-efficiency recovery of byproducts of sunflower seed oil according to claim 7, wherein the particle size of the beta-CD-PU porous crosslinked microspheres is 100-200 meshes.
  9. 9. The method for double zero double low deodorization and efficient recovery of byproducts of sunflower seed oil according to claim 7, wherein the preparation steps of the beta-CD-PU porous crosslinked microsphere comprise: Dissolving fully vacuum dried anhydrous beta-cyclodextrin in anhydrous N, N-dimethylformamide, introducing nitrogen for protection, heating to 65-70 ℃, and mechanically stirring until the anhydrous beta-cyclodextrin is completely dissolved to obtain a dissolution system; adding polyethylene glycol into the solution system, uniformly mixing, and then dropwise adding dibutyl tin dilaurate; Dissolving hexamethylene diisocyanate in anhydrous N, N-dimethylformamide, slowly dripping the solution into a dissolution system, and maintaining the system temperature at 65-70 ℃ for continuous reaction to obtain crosslinked polymer gel; Cooling the obtained crosslinked polymer gel to room temperature, crushing, and sequentially extracting and washing with absolute ethyl alcohol and acetone respectively; and (3) after washing, vacuum drying, grinding and sieving the washing product to obtain the beta-CD-PU porous crosslinked microsphere.
  10. 10. The sunflower seed oil double-zero double-low deodorization and byproduct efficient recovery method according to claim 9, wherein the dropwise adding time of slowly dropwise adding hexamethylene diisocyanate is controlled to be 1.5-2.0h, and the continuous reaction time is controlled to be 6-8h; the extraction and washing mode is Soxhlet extraction for 10-14h, and vacuum drying is carried out at 55-65deg.C for 20-28h.

Description

Double-zero double-low deodorization and byproduct efficient recovery method for sunflower seed oil Technical Field The invention relates to the technical field of edible oil processing, in particular to a double-zero double-low deodorization and byproduct efficient recovery method for sunflower seed oil. Background The sunflower seed oil contains vitamin E, phytosterol and other nutrient components, but free fatty acid and volatile peculiar smell substances need to be removed in the processing and refining process to ensure the quality of the oil. The traditional deodorization technology mainly adopts a vacuum high-temperature steam deodorization method. The method is usually carried out at a higher temperature, and isomerization reaction in an oil system is easily initiated under the action of long-time high-temperature heat, so that harmful substances such as trans-fatty acid or polycyclic aromatic hydrocarbon are generated. At the same time, the high temperature environment can destroy heat sensitive micronutrients, resulting in massive decomposition of these high value components or volatilization of the same with steam into the deodorized distillate, reducing the nutritional value of the finished oil. In order to avoid deterioration of the quality of the oil and fat caused by high temperature, non-high temperature deodorization techniques typified by supercritical carbon dioxide fluid are attracting attention. However, when processing sunflower seed oil systems containing multiple minor components, the existing supercritical fluid extraction and resolution processes have difficulty in achieving precise stepwise separation of the components. The solubility change rule of high-value byproducts such as phytosterol, vitamin E and the like in the supercritical fluid is relatively close. In conventional fluid depressurization and temperature reduction resolution processes, these close molecular weight and polar species tend to co-precipitate due to lack of selective retention mechanisms for specific molecules, resulting in the separation of the species from the resolution pot as a mixture containing various byproducts. To extract high purity phytosterols or vitamin E from such mixed distillates, additional complex secondary separation or chemical purification procedures are required. This not only increases the operating steps and equipment costs of the commercial process, but also results in a decrease in the overall recovery efficiency of byproducts. Therefore, how to separate and extract the high-value byproducts mixed in the fluid step by step and independently in a continuous process flow while realizing low-temperature deodorization of the grease is a practical problem to be solved in the field. Disclosure of Invention The invention solves the technical problems that heat-sensitive nutrient components are always lost and harmful substances such as trans-fatty acid are even generated when sunflower seed oil is treated by the traditional high-temperature steam deodorization process, and in addition, the step-by-step accurate separation and independent recovery of plant sterol, vitamin E and free fatty acid are difficult to realize in the prior art aiming at a byproduct system generated by deodorization. In order to solve the problems, the invention provides the following technical scheme: in a first aspect, the invention provides a sunflower seed oil double-zero double-low deodorization and byproduct efficient recovery method, which adopts the following technical scheme: A sunflower seed oil double-zero double-low deodorization and byproduct efficient recovery method comprises the following steps: pumping the degummed pretreatment crude oil into the middle part of an extraction tower continuously, pumping high-pressure pure carbon dioxide fluid into the bottom of the extraction tower for supercritical extraction, and collecting a supercritical extraction phase discharged from the top of the extraction tower; Introducing a supercritical extraction phase discharged from the top of the extraction tower into a first-stage analysis kettle, reducing the pressure and the temperature, and collecting refined sunflower seed oil finished products separated from the bottom of the first-stage analysis kettle; Introducing the carbon dioxide fluid containing byproducts discharged from the top of the first-stage analysis kettle into a second-stage analysis kettle filled with beta-CD-PU porous crosslinked microspheres, reducing the pressure and the temperature to convert the carbon dioxide fluid containing byproducts into subcritical fluid, and collecting plant sterol enriched matters separated out from the bottom of the second-stage analysis kettle; Introducing the fluid in the subcritical state flowing out of the second-stage analysis kettle into a third-stage analysis kettle, reducing the pressure, and collecting vitamin E enriched matters separated out from the bottom of the third-stage analysis kettle; and (3) intr