A device for efficiently removing plasticizer content in astaxanthin oil and a processing technology thereof

Abstract

The application relates to the technical field of astaxanthin oil purification, in particular to a device for efficiently removing plasticizer content in astaxanthin oil and a processing technology thereof, which comprises a vertical concentration tank, the outer wall of the concentration tank is provided with a jacket heating layer filled with heat-conducting oil, and an electric heating wire is arranged in the jacket heating layer; a plurality of microporous gas distributors are annularly and radially arranged at the bottom of the concentration tank; a plurality of condensation recovery towers are connected to the top of the concentration tank through pipelines, the internal refrigeration temperatures of the plurality of condensation recovery towers are different, and the farther the distance from the concentration tank, the lower the temperature in the tower. The double-layer microporous gas distributor arranged at the bottom of the concentration tank pumps air into the tank, and cooperates with a rotating membrane scraping mechanism to complete dynamic updating of a gas-liquid interface, improve the plasticizer removal rate in the oil and improve the astaxanthin retention rate; through the boiling point fractional condensation design of the three-stage gradient condensation recovery tower, directional separation of the plasticizer and the solvent is completed, and the solvent recovery rate and the discharge gas standard are improved.

Description

TECHNICAL FIELD

[0001] The present application relates to astaxanthin oil purification technology field, specifically to a device for efficiently removing plasticizer content in astaxanthin oil and a processing technology thereof. BACKGROUND

[0002] As a strong antioxidant, astaxanthin oil extract is widely used in food and medicine fields. The extraction process of astaxanthin is easily contaminated by pipe dissolved plasticizer and heavy metals brought by raw materials, such as DEHP, DBP and other phthalate substances released by PVC pipes and plastic storage tanks contacted in the production process; such as heavy metal pollution from microalgae cultured raw materials absorbing lead, mercury in water, and chromium and nickel residues in stainless steel equipment corrosion.

[0003] In the prior art, ethyl acetate, ethanol, acetone and other fat-soluble solvents are usually used to extract astaxanthin. The traditional purification technology has significant defects: the molecular distillation method needs high temperature operation, which leads to thermal degradation loss of astaxanthin, and the removal rate of plasticizer is low; although the activated carbon adsorption method can remove part of the impurities, the adsorption capacity is low and the heavy metals cannot be removed simultaneously. Therefore, it is an urgent need in the industry to develop an integrated system for low-loss and multi-pollutant simultaneous removal. SUMMARY

[0004] In order to overcome the defects in the prior art, the purpose of the present application is to provide a device for efficiently removing plasticizer content in astaxanthin oil and a processing technology thereof, to solve the problems raised in the background art.

[0005] To achieve the above purpose, on the one hand, the present application provides a device for efficiently removing plasticizer content in astaxanthin oil, which comprises a vertical concentration tank, the inner wall of which is provided with a polytetrafluoroethylene coating, the outer wall is provided with a jacket heating layer, and is filled with heat conducting oil, and an electric heating wire is installed in the jacket heating layer; the bottom of the concentration tank is embedded with a plurality of microporous gas distributors in a ring-shaped radial manner, the microporous gas distributor is composed of double-layer sintered metal filter element, and a gas hole with a pore size of 50-100 μm is formed on the top surface of the two-layer filter element; a pulse pump for pumping nitrogen into the microporous gas distributors is installed on one side of the top of the concentration tank;

[0006] A plurality of condensation recovery towers are connected to the top of the concentration tank through pipelines, the internal refrigeration temperatures of the plurality of condensation recovery towers are different, and the lower the temperature in the tower far from the concentration tank, the more active carbon adsorption layers are provided in the outer condensation recovery tower;

[0007] A heavy metal trap is connected in series at the discharge port of the concentration tank, and is internally provided with a mercapto-modified MIL-101(Cr) adsorbent, which is a three-dimensional mesoporous framework with a pore size of 2.9x3.4 nm, and uncoordinated carboxylic acid oxygen atoms provide heavy metal adsorption sites;

[0008] The online monitoring system comprises an infrared spectrum probe embedded in the middle of the concentration tank and an inductively coupled plasma probe embedded in the heavy metal trap, and is connected with a PLC controller.

[0009] As a further improvement of the technical solution, the nitrogen gas inlet rate of the microporous gas distributor is (0.8-1.2):1 (L / min·L) with respect to the volume of oil, and the pulse frequency of the pulse pump is 10-20 Hz.

[0010] As a further improvement of the technical solution, the temperature of the condensation recovery tower is divided into first-stage condensation: ethanol cooling at-5 to 0 DEG C; and second-stage condensation: ethylene glycol cooling at-20 to-15 DEG C.

[0011] As a further improvement of the technical solution, the height-diameter ratio of the heavy metal trap is 3:1, and the operating temperature is 40-50 DEG C.

[0012] As a further improvement of the technical solution, the bottom center of the concentration tank is provided with a rotating shaft, and the top of the rotating shaft is provided with a plurality of fan-shaped scrapers in a radial manner, the gap between the edge of the fan-shaped scraper and the tank wall is 0.3-0.5 mm, and the outer surface is provided with a PTFE coating.

[0013] In another aspect, the application provides a processing technology for efficiently removing the content of plasticizers in astaxanthin oil, which uses the device for efficiently removing the content of plasticizers in astaxanthin oil, and comprises the following steps:

[0014] S1, heating the oil containing plasticizers in the concentration tank to 40-60 DEG C;

[0015] S2, starting the pulse pump to pass through the plurality of microporous distributors to introduce pulsed nitrogen, and maintaining the vacuum degree at-0.08 to-0.095 MPa;

[0016] S3, the water vapor volatilized from the concentration tank is first captured by the plurality of condensation recovery towers for high-boiling plasticizers and macromolecular fat-soluble impurities through second-stage condensation, then captured for low-boiling organic solvents and trace plasticizers, and finally purified and discharged by passing through activated carbon to adsorb aerosol particles;

[0017] S4, the degassed oil in the concentration tank flows through the heavy metal trap, and the concentration of heavy metal ions is reduced through the specific adsorption of the mercapto-modified MIL-101(Cr) adsorbent, so that the pollutant is treated in a separate phase;

[0018] S5, the infrared spectrum probe penetrates the oil sample through the diamond crystal total reflection probe, and collects spectrum data every 30 seconds, and when the peak area reduction rate at 1725 cm-1 is less than 0.5% / min, the PLC adjusts the nitrogen flow rate of the pulse pump;

[0019] S6, the inductively coupled plasma probe detects Pb 2When Hg2+>0.1 ppm or Hg2+>0.05 ppm, the heating wire of the heavy metal trap is activated to 50 DEG C, the adsorption kinetics is improved, the vacuum degree of the concentration tank is reduced to -0.08 MPa, and the residence time is prolonged.

[0020] As a further improvement of the technical solution, the gas stripping is terminated when the infrared spectrum probe detects that the peak intensity at 1725 cm-1 decreases by more than 95%.

[0021] As a further improvement of the technical solution, the heavy metal trap is regenerated by using a mixed solution of 0.5M nitric acid and thiourea for elution.

[0022] As a further improvement of the technical solution, the PLC controller executes a fuzzy PID algorithm with a response time of less than 5 seconds.

[0023] As a further improvement of the technical solution, the treated oil meets the requirements of phthalate content of less than 0.05 ppm, lead and mercury content of less than 0.1 ppm, and astaxanthin retention rate of more than 98%.

[0024] Compared with the prior art, the present application has the following advantages:

[0025] 1. The device and process for efficiently removing plasticizer content in astaxanthin oil, which pumps gas into the tank through the double-layer microporous gas distributor arranged at the bottom of the concentration tank, and cooperates with the rotating membrane scraping mechanism to complete dynamic updating of the gas-liquid interface, improve the removal rate of plasticizer in oil and the retention rate of astaxanthin; through the boiling point fractional condensation design of the three-stage gradient condensation recovery tower, the directional separation of plasticizer and solvent is completed, and the solvent recovery rate and discharged gas standard are improved.

[0026] 2. The device and process for efficiently removing plasticizer content in astaxanthin oil, which completes targeted capture of heavy metal ions through the specific coordination of the mercapto-modified MIL-101(Cr) adsorbent of the heavy metal trap, eliminates Pb 2 + / Hg2+residues, and increases the adsorption capacity;

[0027] 3. The device and process for efficiently removing plasticizer content in astaxanthin oil, which monitors the concentration tank by setting an infrared spectrum probe, the infrared light penetrates the oil sample through the diamond crystal total reflection probe, and the spectrum data is collected every 30 seconds to trigger the PLC to adjust the nitrogen flow rate; the heavy metal trap is monitored by setting an inductively coupled plasma probe, the heating wire of the heavy metal trap is activated to improve the adsorption kinetics and reduce the vacuum degree of the concentration tank to meet the requirements of reducing heavy metal content and improving the retention rate of astaxanthin. BRIEF DESCRIPTION OF DRAWINGS

[0028] The drawings described herein are for purposes of illustration only and are not intended to limit the scope of the present disclosure in any way. Additionally, although the drawings represent possible implementations in accordance with the present disclosure, the drawings are not necessarily to scale and certain features can have been enlarged or distorted for the sake of clarity. Skilled persons, with the benefit of the teachings of the present disclosure, will appreciate that various alternatives to the implementations described herein are possible.

[0029] Figure 1 is a schematic diagram of the overall structure of the present application;

[0030] Figure 2 is a schematic diagram of the astaxanthin oil processing process structure of the present application;

[0031] Figure 3 is a schematic diagram of the astaxanthin oil processing process structure of the present application;

[0032] The meanings of the various reference numbers in the drawings are as follows:

[0033] 100, concentration tank; 200, condensation recovery column; 300, heavy metal trap. DETAILED DESCRIPTION

[0034] The details of the application can be better understood with reference to the drawings and detailed description of the application. However, the specific embodiments of the application described herein are intended for purposes of illustration only and are not intended to be limiting in any way. The teachings of the present application are applicable to any possible variations and thus should be construed to cover any substitutions or equivalents of the features described herein. The terms "mounting", "connected" should be construed broadly and can mean direct connection or indirect connection through an intermediate medium.

[0035] The terms "central axis", "vertical", "horizontal", "front", "back", "up", "down", "left", "right", "top", "bottom", "inner", "outer" and the like as used herein to indicate orientation or positional relationships based on the orientation or positional relationships shown in the drawings, are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the present application. In addition, in the description of the present application, the meaning of "several" is two or more, unless otherwise specifically limited.

[0036] Please refer to Figures 1-3As shown, the present application provides a device for efficiently removing plasticizer content in astaxanthin oil, which comprises a vertical concentration tank 100, the inner wall of which is provided with a polytetrafluoroethylene coating, the coating thickness is 0.5-1mm, the surface roughness Ra≤0.8μm, thereby forming an anti-sticking layer; the outer wall is provided with a jacket heating layer, and is filled with heat conducting oil, and the jacket heating layer is provided with an electric heating wire; the concentration tank 100 is made of 316L stainless steel, the wall thickness is 8-12mm, and the design pressure is-0.1~0.5Mpa; a pulse pump for pumping nitrogen into a plurality of microporous gas distributors is installed on one side of the top of the concentration tank 100; a plurality of microporous gas distributors are embedded in the bottom of the concentration tank 100 in a ring-shaped radial manner, the microporous gas distributors are composed of double-layer sintered metal filter elements, and the top surfaces of the two layers of filter elements are provided with air holes with a pore size of 50-100μm, the pore size of the upper layer is 50-80μm, and the pore size of the lower layer is 80-100μm; the upper layer of small holes controls the initial size of the bubbles, the lower layer of large holes prevents blockage, and the bubble lifting uniformity is improved compared with a single-layer distributor; nitrogen gas forms 50-100μm bubble groups through the double-layer microporous distributor, and the solvent surface turbulence is caused by the Marangoni effect, and the plasticizer migrates from the oil phase to the gas-liquid interface.

[0037] Further, the nitrogen gas inlet rate of the microporous gas distributor is (0.8-1.2):1 (L / min·L) compared with the volume of oil, which means that 0.8-1.2 liters of gas are introduced per liter of oil per minute; the pulse frequency of the pulse pump is 10-20Hz; the pore size of the gas distributor of the concentration tank 100 is adapted to the liquid layer height of 1-1.5m, which prevents gas short circuiting or liquid flooding. For example, when processing 1000L of astaxanthin oil, the gas inlet rate is:

[0038] Lower limit: 0.8L / (min·L)×1000L=800L / min;

[0039] Upper limit: 1.2L / (min·L)×1000L=1200L / min.

[0040] Further, a rotating shaft is arranged at the bottom center of the concentration tank 100, and a plurality of fan-shaped scrapers are arranged radially at the top of the rotating shaft, the gap between the edge of the fan-shaped scraper and the tank wall is 0.3-0.5mm, and the outer surface is provided with a PTFE coating; the rotating scraper continuously removes the tank wall film, exposes the fresh solvent surface, and combines the low surface energy characteristics of the PTFE coating to prevent secondary adsorption of plasticizer, so that the surface renewal efficiency is higher than that of the traditional static method.

[0041] Specifically, a plurality of condensation recovery towers 200 are connected to the top of the concentration tank 100 through pipelines, the internal refrigeration temperatures of the plurality of condensation recovery towers 200 are different, and the lower the temperature in the tower away from the concentration tank 100, the more active carbon adsorption layers are arranged in the condensation recovery tower 200 at the outside;

[0042] The temperature of the condensation recovery tower 200 is divided into first-stage condensation: ethanol cooling at -5 to 0°C; second-stage condensation: ethylene glycol cooling at -20 to -15°C; and gas-carrying plasticizer / solvent vapor is classified and condensed in the first-stage and second-stage condensation towers according to the boiling point difference. High-boiling plasticizers: phthalate DEHP boiling point 386°C, DBP boiling point 340°C, and macromolecular fat-soluble impurities: aldehyde and ketone compounds, which are oxidation products of oil and fat, are captured by ethanol at low temperature through first-stage condensation. Low-boiling organic solvents: ethyl acetate boiling point 77°C, ethanol boiling point 78°C, and trace plasticizers: plasticizers not condensed in the first stage are captured by ethanol at low temperature through second-stage condensation. First-stage high-temperature condensation preferentially removes high-boiling plasticizers to avoid fouling in the low-temperature section. Second-stage deep cold capture of solvents prevents them from entering the activated carbon section to cause adsorption saturation. Phase separation advantage: the gas stripping process transfers plasticizers from liquid oil to gas phase, while heavy metals remain in the liquid phase, realizing separation of pollutants in different phases.

[0043] Specifically, the heavy metal trap 300 is connected in series at the discharge port of the concentration tank 100 and is internally provided with a sulfhydryl-modified MIL-101(Cr) adsorbent. The adsorbent is a three-dimensional mesoporous framework, i.e., a MOF skeleton, and has a pore size of 2.9×3.4 nm and a Cr 3 node: forms a strong coordination bond with an organic ligand (terephthalic acid) and has a thermal stability of up to 350°C; uncoordinated carboxylic acid oxygen atoms provide heavy metal adsorption sites; the sulfhydryl-modified MOF material realizes specific capture of heavy metals through strong coordination between -SH and Pb 2 ; the binding energy is >200 kJ / mol; the sulfhydryl loading is >2.5 mmol / g; and the adsorption capacity for Pb 2 is up to 480 mg / g.

[0044] Sulfhydryl modification mechanism:

[0045] Modification method: post-synthetic modification: 2,5-dimercaptoterephthalic acid (DMTA) is substituted for the original terephthalic acid through ligand exchange;

[0046] Sulfur loading: 2.8-3.2 mmol / g verified by XPS sulfur element quantitative analysis;

[0047] Adsorption mechanism: soft acid-soft base theory: -SH (soft base) forms a strong covalent bond with Pb 2 / Hg2+ (soft acid) with a binding energy >250 kJ / mol;

[0048] Pore confinement effect: 3.4 nm pore size selectively traps heavy metal ions, and the hydrated ion radius is: Pb 2 + 0.401 nm, and Hg2+ 0.419 nm.

[0049] Experimental data

[0050]

[0051] Furthermore, the aspect ratio of the heavy metal trap 300 is 3:1. Fluid dynamics shows that when the aspect ratio is greater than 3, the radial distribution uniformity of the fluid is improved, and the effective utilization rate is increased. The operating temperature is 40-50℃. At temperatures less than 40℃, the diffusion rate is limited, D∝T / μ, and the viscosity of μ oil is high. At temperatures greater than 50℃, the MOF skeleton vibration is intensified, the thiol group shedding rate increases, and TGA shows that the sulfur loss rate is greater than 5% at temperatures greater than 60℃. Astaxanthin thermal stability: the retention rate is greater than 99.5% at 50℃, and HPLC detection shows that the degradation rate increases sharply to 3.2% at 60℃. Oil viscosity: at 40℃, the viscosity decreases from 320 mPa·s at 25℃ to 85 mPa·s, and the fluidity is improved.

[0052] Specifically, the online monitoring system includes an infrared spectral probe embedded in the middle of the concentration tank 100 and an inductively coupled plasma probe embedded in the heavy metal trap 300, and is connected to a PLC controller; the PLC controller executes a fuzzy PID algorithm with a response time of less than 5 seconds.

[0053] The infrared spectral probe uses ATR (Attenuated Total Reflection) Fourier Transform Infrared Spectroscopy (FTIR-ICP Online Monitoring) to detect oil samples: Infrared light (4000-400cm-1) penetrates the oil sample through the diamond crystal total reflection probe; spectral data is collected every 30 seconds, and when the peak area at 1725cm-1 decreases by less than 0.5% / min, the PLC is triggered to adjust the nitrogen flow rate.

[0054] The inductively coupled plasma (ICP) probe utilizes a microwave plasma-excited high-frequency electric field of 2.45 GHz to ionize argon gas to an electron temperature >6000 K; characteristic emission spectra of heavy metal atoms are observed.

[0055] Pb: 220.353 nm (sensitivity 0.1 ppb), Hg: 253.652 nm (sensitivity 0.05 ppb); when Pb is detected... 2 When Hg2+ > 0.1 ppm or Hg2+ > 0.05 ppm:

[0056] The heavy metal trap 300 is activated by heating to 50°C, which enhances the adsorption kinetics and reduces the vacuum level of the concentration tank 100 to -0.08 MPa, thus extending the residence time.

[0057] This invention also provides a processing technology for efficiently removing plasticizers from astaxanthin-containing oils. The device for efficiently removing plasticizers from astaxanthin-containing oils, as described above, includes the following steps:

[0058] S1. Heat the plasticizer-containing grease in the concentration tank 100 to 40-60℃;

[0059] S2, start the pulse pump to pass through the pulse nitrogen through a plurality of microporous distributors, and the vacuum degree is maintained at -0.08 to -0.095 MPa;

[0060] S3, the water vapor volatilized from the concentration tank 100 is first captured high-boiling plasticizers and macromolecular fat-soluble impurities through two-stage condensation of a plurality of condensation recovery towers 200, then captured low-boiling organic solvents and trace plasticizers, and finally purified and discharged through activated carbon adsorption of aerosol particles;

[0061] S4, the degassed oil in the concentration tank 100 flows through the heavy metal trap 300, and the concentration of heavy metal ions is reduced through specific adsorption of the mercapto-modified MIL-101(Cr) adsorbent, realizing the separation treatment of pollutants; the heavy metal trap 300 is regenerated by using a mixed solution of 0.5M nitric acid and thiourea for elution;

[0062] S5, at the same time, the infrared spectrum probe penetrates the oil sample through the diamond crystal total reflection probe, and the spectrum data is collected every 30 seconds; when the peak area reduction rate of 1725 cm-1 is less than 0.5% / min, the PLC adjusts the nitrogen flow rate of the pulse pump; when the infrared spectrum probe detects that the peak intensity of 1725 cm-1 decreases by ≥95%, the gas stripping is terminated; when the infrared spectrum detects a sudden increase in the concentration of plasticizers, the PLC immediately increases the first-stage condensation temperature of the condensation recovery tower 200 to 0°C to prevent ice blockage, and synchronously increases the second-stage condensation cold output;

[0063] S6, when the inductively coupled plasma probe detects Pb 2 +≥0.1ppm or Hg2+≥0.05ppm, the heating wire of the heavy metal trap 300 is activated to 50°C to improve the adsorption kinetics, and the vacuum degree of the concentration tank 100 is reduced to -0.08 MPa to prolong the residence time; after treatment, the oil meets the requirements of phthalate esters <0.05ppm, lead and mercury content <0.1ppm, and astaxanthin retention rate >98%.

[0064] Production line application stage: add astaxanthin oil containing DEHP 15ppm, Pb 2 +2ppm to the concentration tank, set temperature 50°C, vacuum degree -0.09 MPa, nitrogen flow rate 1L / min·L oil, pulse mode 15Hz, and treatment time 90 minutes;

[0065] After detection: DEHP residue 0.03ppm, removal rate 99.8%, Pb 2 +residue 0.07ppm, astaxanthin retention rate 99.1%, and condensation recovery plasticizer purity >99%.

[0066] In addition, the microporous gas distributor is adjusted to a single-layer structure, and other conditions remain unchanged, and the results are:

[0067] The removal rate of DEHP is only 78.5%, and the treatment time is prolonged to 150 minutes, which proves the key role of the double-layer microporous structure to the uniformity of the bubbles. The experimental data are as follows:

[0068] Parameters The present invention Conventional distillation method Plasticizer removal rate 99.8％ 82％ Heavy metal residue < 0.1 ppm 0.5 ppm Energy consumption (kWh / kg) 1.8 4.2 Astaxanthin loss ＜2％ 8-12％

[0069] The system has been successfully applied to astaxanthin production line, and the equipment investment recovery period is short.

[0070] It should be noted that the above embodiments are only for illustrating the technical concept and characteristics of the present application, and the purpose is to enable those skilled in the art to understand the content of the present application and to implement it, and it cannot limit the protection scope of the present application. Any equivalent changes or modifications made in accordance with the spirit and essence of the present application shall be covered within the protection scope of the present application.

Claims

1. A device for efficiently removing plasticizer content in astaxanthin oil, characterized in that: The application relates to a concentration tank (100) arranged in a vertical mode, wherein the inner wall of the concentration tank (100) is provided with a polytetrafluoroethylene coating, the outer wall is provided with a jacket heating layer filled with heat-conducting oil, and an electric heating wire is arranged in the jacket heating layer; a plurality of microporous gas distributors are embedded in the bottom of the concentration tank (100) in a ring-shaped radial mode, the microporous gas distributors are composed of double-layer sintered metal filter elements, and a plurality of air holes with a pore size of 50-100 mu m are formed in the top surfaces of the two layers of filter elements; a pulse pump for pumping nitrogen into the microporous gas distributors is arranged on one side of the top of the concentration tank (100); The nitrogen gas input rate of the microporous gas distributor is (0.8-1.2):1 L / min L, and the pulse frequency of the pulse pump is 10-20 Hz; A plurality of condensation recovery towers (200) are connected to the top of the concentration tank (100) through pipelines, the internal refrigeration temperatures of the plurality of condensation recovery towers (200) are different, the temperature in the tower far from the concentration tank (100) is lower, and the outer condensation recovery tower (200) is internally provided with an activated carbon adsorption layer; The temperature of the condensation recovery tower (200) is divided into first-stage condensation: ethanol cooling at-5~0 DEG C; and second-stage condensation: ethylene glycol cooling at-20~-15 DEG C; A heavy metal trap (300) is connected in series at the discharge port of the concentration tank (100), and is internally provided with a mercapto-modified MIL-101 (Cr) adsorbent which is a three-dimensional mesoporous framework and has a pore size of 2.9*3.4 nm and provides heavy metal adsorption sites for uncoordinated carboxylic acid oxygen atoms; An online monitoring system is arranged, which comprises an infrared spectrum probe embedded in the middle of the concentration tank (100) and an inductively coupled plasma probe embedded in the heavy metal trap (300) and connected with a PLC controller; A rotating shaft is arranged at the bottom center of the concentration tank (100), and a plurality of fan-shaped scrapers are arranged on the top of the rotating shaft in a radial mode, the gap between the edges of the fan-shaped scrapers and the tank wall is 0.3-0.5 mm, and the outer surfaces of the fan-shaped scrapers are provided with PTFE coatings.

2. The device for efficiently removing plasticizer content in astaxanthin oil according to claim 1, characterized in that: The height-diameter ratio of the heavy metal trap (300) is 3:1, and the operating temperature is 40-50 DEG C.

3. A processing technology for efficiently removing the content of plasticizers in astaxanthin oil, using the device for efficiently removing the content of plasticizers in astaxanthin oil according to claim 2, characterized in that, The application further discloses a method for removing heavy metals from oil and grease, which comprises the following steps: S1, heating the oil and grease containing plasticizers in the concentration tank (100) to 40-60 DEG C; S2, starting the pulse pump to pump pulse nitrogen into the microporous distributors, and maintaining the vacuum degree at-0.08~-0.095 MPa; S3, the water vapor volatilized from the concentration tank (100) is first captured to high-boiling plasticizers and macromolecular fat-soluble impurities, then captured to low-boiling organic solvents and trace plasticizers, and finally purified and discharged by removing aerosol particles through the activated carbon adsorption layer of the condensation recovery tower (200); S4, the degassed oil and grease in the concentration tank (100) flows through the heavy metal trap (300), the specific adsorption of the mercapto-modified MIL-101 (Cr) adsorbent reduces the concentration of heavy metal ions, and the pollutant phase separation treatment is realized; S5, at the same time, the infrared spectrum probe penetrates the grease sample through the diamond crystal total reflection probe, and collects spectrum data every 30 seconds. When 1725 cm -1 When the peak area drop rate is less than 0.5% / min, the PLC is triggered to adjust the nitrogen flow rate of the pulse pump. S6, when the inductively coupled plasma probe detects that Pb2+>0.1 ppm or Hg2+>0.05 ppm, the heating wire of the heavy metal trap (300) is activated to 50 DEG C, the adsorption kinetics is improved, the vacuum degree of the concentration tank (100) is reduced to-0.08 MPa, and the residence time is prolonged. When the infrared spectrum probe detects 1725 cm -1 Termination of stripping when the peak intensity drops by > 95%; The treated oil meets the requirements of phthalate <0.05ppm, lead and mercury <0.1ppm, and astaxanthin retention rate >98%.

4. The process for removing plasticizer content from astaxanthin oil according to claim 3, characterized in that: The heavy metal trap (300) is regenerated by using 0.5M nitric acid and thiourea mixed solution for elution.

5. The process for removing plasticizer content from astaxanthin oil according to claim 4, wherein: The PLC controller executes a fuzzy PID algorithm, and the response time is less than 5 seconds.

Images