CN216727230U

CN216727230U - Separation and purification equipment

Info

Publication number: CN216727230U
Application number: CN202123151544.2U
Authority: CN
Inventors: 杨云; 朱波风; 杨雅舒
Original assignee: Zhejiang Mingyue Medical Technology Co ltd; Shanghai Mingyue Medical Technology Co ltd
Current assignee: Zhejiang Mingyue Medical Technology Co ltd; Shanghai Mingyue Medical Technology Co ltd
Priority date: 2021-12-15
Filing date: 2021-12-15
Publication date: 2022-06-14
Anticipated expiration: 2031-12-15

Abstract

The utility model relates to a separation and purification equipment. The separation and purification equipment comprises: a reaction vessel for containing a reaction solution; the first separation component is arranged at the liquid outlet end of the reaction container and is used for separating the reaction liquid; the liquid inlet end of the separation container is communicated with the liquid outlet end of the first separation component, and the separation container is used for layering the reaction liquid separated by the first separation component; an ultrasonic device connected with the separation container and used for promoting the reaction liquid in the separation container to be layered; the vacuum device is communicated with the separation container and is used for controlling the vacuum degree in the separation container; and the second separation component is arranged at the liquid outlet end of the separation container and is used for separating the layered reaction liquid. The separation and purification equipment optimizes the equipment structure, can obtain better separation and purification effects in a shorter time, and has the advantages of higher treatment effect and shorter time consumption.

Description

Separation and purification equipment

Technical Field

The utility model relates to an auxiliary reproduction technical field especially relates to a separation and purification equipment.

Background

During Assisted Reproduction (ART), the culture oil serves to prevent the evaporation of the medium by providing a barrier between the gamete or embryo culture medium and the air, ensuring that fluctuations in pH, osmotic pressure and temperature of the medium are minimized, and thus, the purity of the culture oil is critical to ensure that gametes or embryos develop and produce consistent results.

However, in actual production, some commercialized culture oil still damages gametes and embryos, and cannot reach more than 80% of blastocyst development rate, which is caused by insufficient purity of the culture oil and high content of heavy metals, impurities and hydrogen peroxide.

The existing purification method reduces heavy metal and peroxide value (POV) to qualified lines or even lower; however, these purification methods usually require tedious treatment procedures, and after the treatment, the time required for standing and layering is long, at least 3 to 5 days, which is time-consuming and inefficient.

SUMMERY OF THE UTILITY MODEL

Therefore, it is necessary to provide a separation and purification apparatus which is time-consuming and efficient.

The utility model discloses a realize through following technical scheme.

A separation and purification apparatus comprising: a reaction vessel for containing a reaction solution; the first separation component is arranged at the liquid outlet end of the reaction container and is used for separating the reaction liquid; the liquid inlet end of the separation container is communicated with the liquid outlet end of the first separation component, and the separation container is used for layering the reaction liquid separated by the first separation component; an ultrasonic device connected with the separation container and used for promoting the reaction liquid in the separation container to be layered; the vacuum device is communicated with the separation container and is used for controlling the vacuum degree in the separation container; and the second separation component is arranged at the liquid outlet end of the separation container and is used for separating the layered reaction liquid.

In some embodiments, the separation and purification apparatus further comprises:

the stirring device is arranged in the reaction container and comprises a plurality of stirring components, and each stirring component comprises a stirring rod and a plurality of stirring blades which are sequentially arranged on the stirring rod along the axial direction; and the stirring blades of the adjacent two stirring assemblies are arranged in a staggered manner.

In some embodiments, the stirring device further comprises a plurality of driving members respectively connected with the plurality of stirring assemblies for individually driving the stirring assemblies.

In some embodiments, the driving part is arranged at the bottom of the outer side of the reaction vessel, the stirring rod is arranged in the reaction vessel, the lower end of the stirring rod is connected with the driving part, and the upper end of the stirring rod is connected with or suspended from the top wall of the reaction vessel.

In some of these embodiments, the ultrasound device comprises: an ultrasonic generator for providing an ultrasonic source; and the ultrasonic vibrator is arranged in the separation container, is connected with the ultrasonic generator and is used for interacting with the reaction liquid in the separation container.

In some embodiments, the ultrasonic vibrators are arranged in the separation container, the ultrasonic generator is arranged outside the separation container, and the plurality of ultrasonic vibrators penetrate through the bottom wall of the separation container and are connected with the ultrasonic generator.

In some of the embodiments, the number of the ultrasonic vibrators is multiple;

the ultrasonic vibrators are uniformly arranged in the circumferential direction of the inner side wall of the separation container; and/or the ultrasonic vibrators are arranged at different height positions of the inner side wall of the separation container.

In some of the embodiments, the first separation module and the second separation module are organic microporous filter membranes with the filter pore size of 0.1-0.8 μm.

In some embodiments, the separation and purification apparatus further comprises a liquid extraction device, wherein the liquid extraction device is communicated with the liquid outlet end of the separation container, and is used for extracting the reaction liquid separated from the second separation component.

In some embodiments, the separation and purification apparatus further comprises a control device for controlling the ultrasonic device, the vacuum device and the liquid pumping device.

The separation and purification equipment can be used for separating and purifying samples to be separated such as culture oil. Taking the culture oil as an example, the culture oil reacts with the additive agent in the reaction vessel to obtain a reaction solution; the reaction liquid is separated by the first separation component and then enters a separation container; the ultrasonic device provides ultrasonic cavitation to promote the reaction liquid in the separation container to eliminate bubbles and a small amount of liquid mixed in the culture oil, so that the quality of the culture oil is improved; further, the air pressure in the separation container is controlled by a vacuum device to be in a vacuum environment and the reaction liquid is layered, so that bubbles in the culture oil and Volatile Organic Compounds (VOCs) mixed with the bubbles are separated from the culture liquid, a good standing layering effect is obtained within a short time, and a separated and purified sample can be obtained through a second separation component. The separation and purification equipment optimizes the equipment structure, can obtain better separation and purification effects in a shorter time, and has the advantages of higher treatment effect and shorter time consumption.

Drawings

Fig. 1 is a schematic structural diagram of a separation and purification apparatus according to an embodiment of the present invention;

fig. 2 is a schematic structural diagram of a separation container, an ultrasonic device and a vacuum device of the separation and purification apparatus according to an embodiment of the present invention;

FIG. 3 is a graph comparing the standing and layering time of examples 1 to 3 and comparative examples 1 to 3 of the present invention;

description of the reference numerals:

10: separation and purification equipment; 110: a reaction vessel; 111: a feeding port; 112: a pH meter;

121: a first separation assembly; 122: a second separation assembly; 130: a separation vessel;

141: an ultrasonic generator; 142: an ultrasonic vibrator; 150: a vacuum device; 160: a stirring device;

162: a stirring assembly; 161: a stirring rod; 163: a stirring blade; 164: a drive member;

170: a liquid pumping device; 181: a first valve; 182: a second valve; 190: and a control device.

Detailed Description

In order to facilitate understanding of the present invention, the present invention will be described more fully hereinafter with reference to the accompanying drawings. The preferred embodiments of the present invention are shown in the drawings. The invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. It is to be understood that these embodiments are provided so that this disclosure will be thorough and complete.

In the description of the present invention, it is to be understood that the terms "upper", "lower", "top", "bottom", "inner", "outer", "axial", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.

In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

Referring to fig. 1, one embodiment of the present invention provides a separation and purification apparatus 10, which includes a reaction vessel 110, a first separation assembly 121, a separation vessel 130, an ultrasonic device, a vacuum device 150, and a second separation assembly 122.

The reaction container 110 is used for containing a reaction solution for the reaction between the sample to be separated and the additive agent to form the reaction solution.

The first separation assembly 121 is disposed at the liquid outlet end of the reaction vessel 110, and is used for separating the reaction liquid.

And a separation vessel 130, wherein the liquid inlet end of the separation vessel 130 is communicated with the liquid outlet end of the first separation assembly 121, so that the reaction liquid separated by the first separation assembly 121 is layered.

And an ultrasonic device connected to the separation vessel 130 for providing ultrasonic cavitation to the reaction liquid in the separation vessel 130 for standing and layering, thereby layering the reaction liquid.

And a vacuum device 150, which is communicated with the separation container 130 and is used for controlling the vacuum degree of the reaction liquid in the separation container 130 for standing and layering, thereby promoting the reaction liquid to stand and layer.

And the second separation assembly 122 is arranged at the liquid outlet end of the separation container 130 and is used for separating the layered reaction liquid.

The separation and purification apparatus 10 can be used for separation and purification of a sample to be separated, such as culture oil. Taking the culture oil as an example, the culture oil reacts with the additive agent in the reaction vessel 110 to obtain a reaction solution; the reaction liquid enters the separation container 130 after being separated by the first separation assembly 121; the ultrasonic device provides ultrasonic cavitation to promote the reaction liquid in the separation container 130 to eliminate bubbles and a small amount of liquid mixed in the culture oil, so that the quality of the culture oil is improved; further, the air pressure in the separation container 130 is controlled by the vacuum device 150 in a vacuum environment to stratify the reaction liquid, so that bubbles and mixed Volatile Organic Compounds (VOCs) in the culture oil are separated from the culture liquid, a good standing and stratifying effect is obtained within a short time, and then a separated and purified sample can be obtained through the second separation component 122. The separation and purification equipment 10 optimizes the equipment structure, can obtain better separation and purification effects in a shorter time, and has the advantages of higher treatment effect and shorter time consumption.

It is understood that the reaction vessel 110 may be a straight cylinder type, but is not limited thereto. Further, the material of the reaction vessel 110 may be stainless steel. Further, the reaction vessel 110 may be provided with a feed port 111 and a sealing stopper for sealing the feed port 111. It will be appreciated that the number and location of the feed ports 111 on the reaction vessel 110 are not limited and may be set as desired. In one embodiment, the feed port 111 is provided at the top of the reaction vessel 110.

In some of these embodiments, the separation and purification apparatus 10 further comprises a stirring device 160. The stirring device 160 is disposed in the reaction vessel 110, the stirring device 160 includes at least one stirring assembly 162, and each stirring assembly 162 includes a stirring rod 161 and a plurality of stirring blades 163 sequentially disposed on the stirring rod 161 along the axial direction.

Further, the stirring assemblies 162 are multiple, and the stirring blades 163 of two adjacent stirring assemblies 162 are arranged in a staggered manner. The stirring device 160 with optimized structure is used for ensuring more sufficient stirring.

It is understood that the stirring process can mix a large number of bubbles in the reaction solution, but the separation and purification apparatus 10 can effectively remove bubbles mixed in the reaction solution by providing the ultrasonic device and the vacuum device 150.

Further, the stirring device 160 further includes a plurality of driving members 164, and the plurality of driving members 164 are respectively connected with the plurality of stirring assemblies 162 for individually driving the stirring assemblies 162. Specifically, the rotation speed and the rotation direction of each stirring assembly 162 can be independently controlled. For example, the direction of rotation of each agitator assembly 162 may be the same or opposite. It is appreciated that in other examples, multiple agitating assemblies 162 may be simultaneously driven by a single drive member 164.

Further, the driving member 164 is provided at the outer bottom of the reaction vessel 110. The stirring rod 161 is disposed in the reaction vessel 110, a lower end of the stirring rod 161 is connected to the driving member 164, and an upper end of the stirring rod 161 is connected to or suspended from a ceiling wall of the reaction vessel 110.

Still further, the driving part 164 may be a driving motor.

Further, the lower end of the stirring rod 161 penetrates the bottom wall of the reaction vessel 110 and is sealed with the bottom wall of the reaction vessel 110 by a sealing ring to prevent leakage or cross contamination. Specifically, the sealing ring is a high-density wear-resistant rubber sealing ring.

Further, the shape of the stirring blade 163 includes, but is not limited to, square, circular, and spiral.

Further, a pH meter 112 is further included, and the pH meter 112 is disposed in the reaction vessel 110 and is used for detecting the pH value of the solution in the reaction vessel 110.

Further, a first valve 181 is disposed on a connection line between the reaction vessel 110 and the separation vessel 130, for controlling the opening and closing of the flow of the reaction solution in the reaction vessel 110 to the separation vessel 130. Specifically, the first valve 181 is disposed between the first separation assembly 121 and the separation vessel 130.

Further, the separation vessel 130 may be a transparent vessel, or may be provided with a transparent observation window, so as to observe the layering of the reaction solution such as the culture oil in the separation vessel 130. In one embodiment, the material of the separation container 130 may be one of polymethyl methacrylate (PMMA), polyethylene terephthalate-1, 4-cyclohexanedimethanol (PEGT), and polyethylene terephthalate (PET).

In some of the embodiments, the ultrasonic device includes an ultrasonic generator 141 and an ultrasonic vibrator 142.

The ultrasonic generator 141 is used to provide a source of ultrasonic waves. The ultrasonic vibrator 142 is provided in the separation vessel 130 and connected to the ultrasonic generator 141 for interacting with the reaction liquid in the separation vessel 130.

Further, the ultrasonic vibrator 142 is provided inside the separation vessel 130, and the ultrasonic generator 141 is provided outside the separation vessel 130.

Further, the number of the ultrasonic transducers 142 is plural.

As shown in fig. 1, in some embodiments, the plurality of ultrasonic vibrators 142 are uniformly arranged in the circumferential direction of the inner side wall of the separation vessel 130. Further, the plurality of ultrasonic transducers 142 are disposed at different height positions on the inner side wall of the separation vessel 130.

In other embodiments, as shown in fig. 2, a plurality of ultrasonic vibrators 142 extend through the bottom wall of the separation vessel 130 and are connected to the ultrasonic generator 141.

In some embodiments, the ultrasonic generator 141 can provide ultrasonic waves with a resonant impedance of not more than 20 Ω and a resonant frequency of 25 to 30 kHz.

In some of these embodiments, the first separation module 121 and the second separation module 122 are organic microporous filtration membranes with a filtration pore size of 0.1 μm to 0.8. mu.m. In a specific example, the filtration pore size of the organic microfiltration membrane is 0.22 μm.

Further, each of the first separation module 121 and the second separation module 122 is independently selected from one of a polytetrafluoroethylene microfiltration membrane and a polyethersulfone microfiltration membrane.

In some embodiments, the separation and purification apparatus 10 further comprises a vacuum device for detecting the air pressure of the separation container 130. Further, a vacuum device is provided at the top of the separation vessel 130. Further, the vacuum device 150 may be a vacuum pump.

With continued reference to fig. 1, in some embodiments, the separation and purification apparatus 10 further includes a liquid pumping device 170. The liquid extraction device 170 is communicated with the liquid outlet end of the separation container 130 for extracting the reaction liquid separated from the second separation assembly 122.

Further, the fluid drawing device 170 may be a peristaltic pump. Further, the device also comprises a discharge pipe which is communicated with the discharge end of the liquid pumping device 170 so as to further perform sub-packaging, sealing and sealing on the product obtained by separation and purification. It will be appreciated that a storage means may be included in communication with the discharge end of the extraction means 170 for storing the product from the separation and purification.

Further, a second valve 182 is further included, and the second valve 182 is disposed on a connection pipeline between the separation container 130 and the liquid pumping device 170, for controlling the opening and closing of the reaction liquid in the separation container 130 to the liquid pumping device 170. Specifically, the second valve 182 is disposed between the second separating assembly 122 and the pumping device 170.

In some embodiments, the separation and purification apparatus 10 further comprises a control device 190, wherein the control device 190 is connected to each of the ultrasonic device, the vacuum device 150 and the liquid-extracting device 170 for independently controlling the ultrasonic device, the vacuum device 150 and the liquid-extracting device 170.

Further, control device 190 may also be connected to pH meter 112 for obtaining data of pH meter 112.

Further, the control device 190 is used for controlling the operations of the ultrasonic device, the vacuum device 150 and the liquid pumping device 170, such as turning on, turning off and turning off.

Further, the control device 190 may include a display device that can display the operation states and parameters of the ultrasonic device, the vacuum device 150, and the fluid pumping device 170.

Further, the control device 190 may further include a control interface, which may be a touch screen and may facilitate operation by an operator. Furthermore, the control interface can be provided with a password protection mode, so that the existing parameters are prevented from being maliciously changed or mistakenly changed in the working state.

Another embodiment of the present invention provides a method for separating and purifying culture oil, which can be performed by using any one of the above separation and purification apparatuses 10.

The method for separating and purifying the culture oil comprises the following steps S10-S40.

Step S10: mixing the culture oil to be separated and purified with an additive agent to obtain a reaction solution. The additive agent includes a first reducing agent.

In some embodiments, the culture oil to be separated and purified is light liquid paraffin oil, the relative density of the culture oil is 0.830-0.860, and the kinematic viscosity of the culture oil is 12 cs-30 cs.

In some embodiments, step S10 may be performed in the reaction vessel 110 of the separation and purification apparatus 10.

Further, the additive agent also comprises a second reducing agent and a nonionic amphoteric buffer solution. Further, the first reducing agent is an oil-soluble reducing agent, and the second reducing agent is a water-soluble or water-oil-soluble reducing agent. Therefore, the problems of peroxide value, heavy metal and other impurities in the culture oil are solved at the same time, the treatment procedure of the traditional method is avoided to be complicated, and the problem of peroxide value or heavy metal is solved singly.

In one embodiment, the culture oil to be separated and purified is mixed with a first reducing agent, then mixed with a second reducing agent, and then mixed with a nonionic amphoteric buffer. The first reducing agent, the second reducing agent and the nonionic amphoteric buffer are sequentially added through the feed port 111, and a stirring process is performed after each feed to be sufficiently mixed.

In some embodiments thereof, the first reducing agent may be at least one of Butylated Hydroxyanisole (BHA), Butylated Hydroxytoluene (BHT), Propyl Gallate (PG), and vitamin E.

Further, the first reducing agent is added in the form of a solution. The solvent of the first reducing agent solution may be water for injection. Further, the concentration of the first reducing agent solution is 20 g/L-60 g/L; further, the volume ratio of the first reducing agent solution to the culture oil to be separated and purified is (2-3): 1. further, after the first reducing agent is added, stirring is carried out for 10min to 25min at the rotating speed of 1000r/min to 1500r/min, so as to reduce the content of peroxide value in the culture oil.

In some of these embodiments, the second reducing agent may be at least one of vitamin C, tea polyphenols, ascorbic acid, palmitate, and phytic acid. Further, the second reducing agent is added in the form of a solution. The solvent of the second reducing agent solution may be water for injection. Further, the concentration of the second reducing agent solution is 10 g/L-40 g/L; further, the volume ratio of the second reducing agent solution to the culture oil to be separated and purified is (1-2): 1. further, after the second reducing agent is added, stirring is carried out for 15-30 min at the rotating speed of 1000-1500 r/min, so as to remove harmful heavy metals, water-soluble Volatile Organic Compounds (VOCs) and other impurities in the culture oil raw material.

In some of these embodiments, the non-ionic ampholytic buffer is a 0.9% sodium chloride solution containing HEPES at a concentration of 10mmol/L to 25 mmol/L. Further, the volume ratio of the nonionic amphoteric buffer solution to the culture oil is (1-2): 1. further, after the nonionic amphoteric buffer solution is added, stirring is carried out for 15-30 min at the rotating speed of 1000-1500 r/min, so as to remove harmful heavy metals, water-soluble Volatile Organic Compounds (VOCs) and other impurities in the culture oil raw material.

Step S20: and filtering and separating the reaction solution to obtain separated reaction solution.

In some embodiments, the filtering and separating step of step S20 can be performed by the first separating component 121 of the separation and purification apparatus 10.

It can be understood that the step S20 removes the precipitated impurities such as harmful heavy metals in the culture oil raw material by filtration separation.

Step S30: and carrying out ultrasonic treatment on the separated reaction liquid, and then carrying out vacuum standing treatment to allow the reaction liquid to stand for layering.

It can be understood that the ultrasonic treatment of step S30 is beneficial to eliminating air bubbles and a small amount of liquid mixed in the culture oil after the reaction in the reaction vessel, and improving the quality of the culture oil; further, the culture oil is controlled to carry out vacuum standing treatment to realize standing layering, so that bubbles and mixed Volatile Organic Compounds (VOCs) in the culture oil can be promoted to be separated from the culture solution, and a good standing layering effect is obtained in a short time. After standing and layering, the upper layer is the oil phase of the reduced culture oil, and the lower layer is the water phase, and the purpose of separating the culture oil can be achieved through filtering. Therefore, the problems of long overall time consumption and low efficiency caused by long standing and layering time after the completion of each treatment in the conventional separation method which needs at least 4-5 times of washing treatment are solved.

In some embodiments, step S30 can be performed in the separation vessel 130 of the separation and purification apparatus 10. Specifically, after the reaction liquid in the reaction vessel 110 enters the separation vessel 130 by opening the first valve 181, the first valve 181 is closed. Starting an ultrasonic device to carry out ultrasonic treatment on the separated reaction liquid; then, the ultrasonic device is turned off, the vacuum device 150 is turned on, the air pressure in the separation vessel 130 is controlled to be vacuum pressure, and standing layering is performed.

Furthermore, the resonance impedance of the ultrasonic wave in the ultrasonic wave treatment is not more than 20 omega, and the resonance frequency is 25-30 kHz. Further, the time of ultrasonic treatment is 30-60 min, such as 30min, 35min, 40min, 45min, 50min, 55min, 60 min.

Further, the pressure of the standing layer is controlled to be 10 to 30kPa, for example, 10kPa, 12kPa, 14kPa, 16kPa, 18kPa, 20kPa, 22kPa, 24kPa, 26kPa, 28kPa, 30 kPa. Further, the time of the vacuum standing treatment is 48-64 h, such as 48h, 50h, 52h, 54h, 56h, 58h, 60h, 62h and 64 h.

Step S40: and (4) separating the reaction liquid after standing and layering.

In some embodiments, the separation step of step S40 can be performed by the second separation assembly 122 of the separation and purification apparatus 10 described above.

It can be understood that the method for separating and purifying culture oil of the present invention may further include: and (4) extracting and storing the reaction liquid separated in the step (S40). In addition, the separation and purification method may include other steps mentioned in the above separation and purification apparatus 10, and will not be described herein again.

The method for separating and purifying the culture oil has the advantages that the process is simplified, only the agents are added into the reaction container, and the subsequent standing layering is carried out by separating, combining ultrasonic treatment and vacuum standing treatment, so that a good separation and purification effect can be obtained in a short time, and the method has the advantages of high treatment effect and short time consumption.

In order to make the objects, technical solutions and advantages of the present invention more concise and clear, the present invention is described with the following specific embodiments, but the present invention is by no means limited to these embodiments. The following description of the preferred embodiments is merely exemplary in nature and is in no way intended to limit the scope of the invention. It should be understood that any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

In order to better explain the present invention, the following description is given with reference to the embodiments. The following are specific examples.

Utilize the utility model provides an above-mentioned separation and purification equipment handles 3 different brands' medicinal grade light liquid paraffin oil. The 3 different brands are brand a (Jilin Jihua), brand B (Hunan Erkang) and brand c (sigma), respectively.

Example 1

The brand A is light liquid paraffin oil, the relative density of the light liquid paraffin oil is 0.830-0.860, and the kinematic viscosity of the light liquid paraffin oil is 12-30 cs; the separation and purification method of the culture oil of brand A comprises the following steps:

(1) preparing a reducing agent solution 1: 3g of Butylated Hydroxyanisole (BHA) was weighed accurately, poured into a beaker with a capacity of 100mL, 100mL of water for injection was added, and the mixture was stirred with a glass rod until the solid was completely dissolved.

(2) Preparing a reducing agent solution 2: 2g of vitamin C was accurately weighed, poured into a beaker with a capacity of 100mL, and 100mL of water for injection was added, and the mixture was stirred with a glass rod until the solid was completely dissolved.

(3) Preparing a nonionic amphoteric buffer solution 3: 47.6mg of HEPES was accurately weighed, poured into a 100mL beaker, and 100mL of physiological saline was added thereto, and the mixture was stirred with a glass rod until the solid was completely dissolved.

(4) Taking a certain volume of culture oil raw material, loading the culture oil raw material into a reaction container from a feeding port, and then adding a reducing agent solution 1: the volume ratio of the culture oil raw materials is 2: 1, filling the reducing agent solution 1 into a reaction vessel, starting the stirring function of the reaction vessel, and stirring at the rotating speed of 1200r/min for 20 min.

(5) According to the reducing agent solution 2: the volume ratio of the culture oil raw materials is 1: and 1, adding a reducing agent solution 2 into the mixed solution in the step (4), and stirring at the rotating speed of 1200r/min for 10 min.

(6) Following a non-ionic amphoteric buffer 3: the volume ratio of the culture oil raw materials is 1: and 1, adding a nonionic amphoteric buffer solution 3 into the mixed solution obtained in the step (5), and stirring at the rotating speed of 1200r/min for 20 min.

(7) And (4) closing the second valve, opening the first valve, and filtering the mixed liquor obtained in the step (6) into a separation container through the first separation assembly.

(8) Closing the first valve, opening the ultrasonic device, adjusting the resonant frequency of the ultrasonic generator to 30kHz, allowing the culture oil mixed solution in the separation container to act for 45min, and closing the ultrasonic generator after the ultrasonic treatment is completed; and then starting a vacuum pump, and keeping the vacuum pressure at 22kPa for suction until the culture oil is completely settled and layered.

(9) And closing the vacuum pump, opening the second valve, simultaneously opening the peristaltic pump, filtering the well-standing culture oil through the second separation assembly, subpackaging, sealing and storing in a refrigerator or a cold storage for a long time.

Example 2

The method for separating and purifying the culture oil of brand B is basically the same as the step of the example 1, and is characterized in that: step (4) according to the reducing agent solution 1: the volume ratio of the culture oil raw materials is 3: 1, filling the reducing agent solution 1 into a reaction container, starting the stirring function of the reaction container, and stirring at the rotating speed of 1000r/min for 20 min.

Example 3

The separation and purification method of brand C culture oil is basically the same as the step of example 1, except that: preparing a nonionic amphoteric buffer solution 3: 238mg of HEPES was accurately weighed, poured into a 100mL beaker, and 100mL of physiological saline was added thereto, followed by continuous stirring with a glass rod until the solid was completely dissolved.

The culture oils of examples 1 to 3 were tested for PV value and heavy metal content before and after separation and purification according to the fat PV value test method and heavy metal test method in the Chinese pharmacopoeia (fourth part), and the test results are shown in Table 1 below.

TABLE 1

As can be seen from Table 1, the PV value and the heavy metal content of the culture oil after the separation and purification treatment of the present invention are reduced compared to those before the treatment, indicating that the separation and purification treatment method is effective for the culture oil.

Comparative example 1

Comparative example 1 is essentially the same as example 1 except that: and (4) adopting conventional standing for layering in the standing and layering step in the step (8). The method comprises the following specific steps: and (4) closing the second valve, opening the first valve, filtering the mixed liquor obtained in the step (6) through the first separation component, allowing the filtered mixed liquor to enter a separation container, closing the first valve, and naturally standing and layering at room temperature without opening an ultrasonic device and a vacuum device.

Comparative example 2

Comparative example 2 is essentially the same as example 2, except that: and (4) adopting conventional standing for layering in the standing and layering step in the step (8). The method comprises the following specific steps: and (4) closing the second valve, opening the first valve, filtering the mixed liquor obtained in the step (6) through the first separation component, allowing the filtered mixed liquor to enter a separation container, closing the first valve, and naturally standing and layering at room temperature without opening an ultrasonic device and a vacuum device.

Comparative example 3

Comparative example 3 is essentially the same as example 3, except that: and (4) adopting conventional standing for layering in the standing and layering step in the step (8). The method comprises the following specific steps: and (3) closing the second valve, opening the first valve, filtering the mixed liquor obtained in the step (6) through the first separation component, feeding the filtered mixed liquor into a separation container, then closing the first valve, and naturally standing and layering at room temperature without opening an ultrasonic device and a vacuum device.

The time for the standing and layering in step (8) of examples 1 to 3 and comparative examples 1 to 3 was counted, and the results are shown in fig. 3. As can be seen from FIG. 3, comparing examples 1-3 with the conventional standing layering of comparative examples 1-3, the time for treating the standing layering of the embodiment of the present invention is significantly shortened, and about 30% of the time is saved.

All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.

The above-mentioned embodiments only represent some embodiments of the present invention, and the description thereof is specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several variations and modifications can be made, which are within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims, and the description and drawings can be used to interpret the contents of the claims.

Claims

1. A separation and purification apparatus, comprising:

a reaction vessel for containing a reaction liquid;

the first separation component is arranged at the liquid outlet end of the reaction container and is used for separating the reaction liquid;

the liquid inlet end of the separation container is communicated with the liquid outlet end of the first separation component, and the separation container is used for layering the reaction liquid separated by the first separation component;

an ultrasonic device connected with the separation container and used for promoting the reaction liquid in the separation container to be layered;

a vacuum device communicated with the separation container and used for controlling the vacuum degree in the separation container; and

and the second separation component is arranged at the liquid outlet end of the separation container and is used for separating the layered reaction liquid.

2. The separation and purification apparatus of claim 1, further comprising:

3. The separation and purification apparatus of claim 2, wherein the stirring device further comprises a plurality of driving members respectively connected to the plurality of stirring assemblies for individually driving the stirring assemblies.

4. The separation and purification apparatus according to claim 3, wherein the driving member is disposed at the bottom of the outer side of the reaction vessel, the stirring rod is disposed in the reaction vessel, the lower end of the stirring rod is connected to the driving member, and the upper end of the stirring rod is connected to or suspended from the top wall of the reaction vessel.

5. The separation and purification apparatus of any one of claims 1 to 4, wherein the ultrasonic device comprises:

an ultrasonic generator for providing an ultrasonic source; and

and the ultrasonic vibrator is arranged in the separation container, is connected with the ultrasonic generator and is used for interacting with the reaction liquid in the separation container.

6. The separation and purification apparatus according to claim 5, wherein the ultrasonic vibrators are disposed in the separation container, the ultrasonic generator is disposed outside the separation container, and the plurality of ultrasonic vibrators penetrate through a bottom wall of the separation container and are connected to the ultrasonic generator.

7. The separation and purification apparatus according to claim 5, wherein the number of the ultrasonic vibrators is plural;

the ultrasonic vibrators are uniformly arranged in the circumferential direction of the inner side wall of the separation container, and/or the ultrasonic vibrators are arranged at different height positions of the inner side wall of the separation container.

8. The separation and purification apparatus of any one of claims 1 to 4 and 6 to 7, wherein the first separation module and the second separation module are organic microporous filtration membranes having a filtration pore size of 0.1 μm to 0.8 μm.

9. The separation and purification apparatus according to any one of claims 1 to 4 and 6 to 7, further comprising a liquid extraction device, wherein the liquid extraction device is communicated with the liquid outlet end of the separation container and is used for extracting the reaction liquid separated from the second separation component.

10. The separation and purification apparatus according to claim 9, further comprising a control device for controlling the ultrasonic device, the vacuum device and the liquid pumping device.