CN216259212U

CN216259212U - Extracting tank

Info

Publication number: CN216259212U
Application number: CN202122392311.5U
Authority: CN
Inventors: 潘桀; 杨志刚; 杨东泽
Original assignee: Inner Mongolia Maiwei Biotechnology Co ltd
Current assignee: Inner Mongolia Maiwei Biotechnology Co ltd
Priority date: 2020-10-01
Filing date: 2021-09-30
Publication date: 2022-04-12
Anticipated expiration: 2031-09-30
Also published as: CN113861259A; CN216062109U

Abstract

The utility model discloses an extraction tank, which comprises a tank body, a stirring device, a flow baffle, a heat exchange system and a temperature control device, wherein the stirring device is arranged on the tank body; the extraction tank comprises a tank body, a feed inlet, a discharge outlet and a feed outlet, wherein the tank body comprises a cylindrical upper cylinder body and a conical lower cylinder body which are connected up and down; the stirring device is arranged in the center of the extraction tank, and a plurality of flow baffles are vertically arranged on the inner wall of the upper cylinder at intervals; the heat exchange system is fixedly arranged on the extraction tank, and the temperature control device controls the heat exchange system in a linkage manner. The method can realize saponification extraction of the protein substances of the fermentation mushroom dregs in one single equipment, simplifies the extraction process, and has the advantages of short extraction time, low energy consumption in the extraction process, low solvent loss and high product purity.

Description

Extracting tank

Technical Field

The utility model belongs to the field of extraction of medical intermediates, and particularly relates to an extraction tank for saponifying and extracting protein substances in fermentation fungus residues.

Background

Biological fermentation residues usually contain protein substances with high-valence lipids for special purposes, for example, ergosterol contained in certain fungi, starch fermentation products and antibiotic residues, and need to be extracted for preparing medical intermediates. In the prior art, a starch fermentation product is used as a raw material, equipment for extracting high-purity ergosterol is adopted, a plurality of devices for saponifying and extracting ergosterol are provided, the operation is complex, saponification and extraction are completed in different equipment, the raw material is subjected to saponification, filtration, extraction, decoloration, crystallization, recrystallization and other steps to obtain an ergosterol product, the process flow is long, the yield is low, and the energy consumption is high. In addition, when the ergosterol is extracted by a saponification extraction process, the loss of a solvent (namely a solvent and an extractant) is large, the production cost is high, and the volatilization of the solvent can cause serious problems of safety and environmental protection. Therefore, it is necessary to design an extraction apparatus with high efficiency and high extraction rate to meet the requirement of industrial production.

SUMMERY OF THE UTILITY MODEL

Aiming at the problems and the defects in the prior art, the utility model provides the extraction tank which can complete the saponification and the extraction reaction of the fermentation fungus residues in one device, simplifies the extraction process, shortens the extraction time, reduces the solvent consumption in the extraction process, improves the product quality and is very suitable for industrial mass production.

In order to achieve the purpose, the utility model provides a technical scheme that: an extraction tank comprises a tank body, a stirring device, a flow baffle, a heat exchange system and a temperature control device; wherein the content of the first and second substances,

the tank body comprises a cylindrical upper cylinder body and a conical lower cylinder body which are connected up and down, the tank top of the extraction tank is provided with a feed inlet, and the tank bottom of the extraction tank is provided with a discharge outlet;

the stirring device is arranged in the center of the extraction tank, and a plurality of flow baffles are vertically arranged on the inner wall of the upper cylinder at intervals;

the heat exchange system is fixedly arranged on the extraction tank, and the temperature control device controls the heat exchange system in a linkage manner.

Preferably, the stirring device comprises a stirring shaft, one end of the stirring shaft is connected with a stirring motor, the upper part of the stirring shaft positioned in the upper cylinder body is provided with at least one group of stirring blade sets, and the lower part of the stirring shaft positioned in the lower cylinder body is provided with at least one group of stirring blade sets.

Preferably, the upper part of the stirring shaft in the upper cylinder is sequentially provided with a first blade group, a second blade group and a third blade group from top to bottom, and the lower part of the stirring shaft in the lower cylinder is provided with a fourth blade group and a fifth blade group.

Preferably, the blade sets comprise two symmetrical blade-shaped blades, and the included angles between the blades of the two adjacent blade sets and the central axis of the stirring shaft form an anti-symmetric arrangement.

Preferably, the plurality of baffle plates are circumferentially arranged at equal angular intervals along the inner wall of the upper cylinder of the extraction tank.

Preferably, the heat exchange system comprises a first common heat exchange net arranged on the inner wall of the extraction tank and/or the outer wall of the upper cylinder body, and a first independent heat exchange net arranged outside the extraction tank and communicated with the first common heat exchange net; the heat exchange system is used for heating or cooling the materials in the extraction tank.

Preferably, the extraction tank uses a variable frequency speed regulating motor to control the stirring device.

Preferably, the extraction tank can be used for extracting protein substances of the fermentation mushroom dregs.

Preferably, the extraction tank can be used for saponification and extraction reaction of the fermentation mushroom dregs.

Preferably, the operation temperature of the saponification and extraction reaction of the extraction tank is 20-70 ℃.

Preferably, the top of the extraction tank is also provided with an air outlet and a reflux port, the reflux port is provided with a reflux device for condensing and refluxing the solvent and/or the extractant, and the top end of the reflux device is provided with an exhaust device.

Preferably, the extraction tank can be used for saponification extraction of ergosterol.

Compared with the prior extraction device, the extraction tank has the following beneficial technical effects:

1) the saponification extraction of the protein substances of the fermentation fungus residues is finished in a single equipment (extraction tank) by one step without intermediate steps of filtering, cooling, extracting and the like, thereby simplifying the extraction process flow; in addition, experiments show that 70-80% of protein extraction substances (ergosterol) in the fermentation mushroom residues can enter the light-phase extracting solution by standing and phase splitting in the extracting tank, and compared with the method that the extract is filtered and then subjected to phase splitting after extraction reaction, the method has the advantages that the volatilization loss of a solvent (a solvent) is small, the energy consumption is lower, the operating pressure of subsequent phase splitting can be reduced, and the phase splitting operating cost is reduced. In addition, the fermentation fungus dregs do not need to be pretreated before the solvent and the saponifier are added, and the extraction process is simplified.

2) After the saponification extraction reaction is completed, cooling water is introduced through a heat exchange system arranged on the extraction tank to cool, the material waste heat after the saponification and extraction reaction is removed, the volatilization loss of the solvent of the subsequent extracting solution in the filtering stage can be obviously reduced due to temperature reduction, the production cost is further reduced, and the operation environment and the safety are improved. The setting can also promote the dispersibility of saponifier in the material through heating under extracting jar toper on barrel inner wall and/or the second sharing heat transfer net on the outer wall, prevents on the one hand that the material cooling deposit that the saponifier dissolved from appearing at tank bottoms and pipeline, emergence jam, promotes the saponification reaction of saponifier better on the other hand.

3) The process flow of the utility model is short, the extraction rate (the quality of ergosterol products/the quality of mushroom dreg raw materials) is high, and the extraction rate is stabilized to be more than 0.1 percent and can reach 0.2 percent at most. The obtained ergosterol product has high purity which is not less than 98 wt%, and the product quality is superior to the product sold on the market at present.

4) Compared with the prior art, the extraction time can be greatly shortened, the time from feeding to obtaining the ergosterol crude product is shortened from 24-36 hours to 12-15 hours, and the production capacity is improved by 1 time.

5) The extraction tank is provided with a variable-frequency speed-regulating motor, the stirring intensity of the stirring device can be set at any time or adjusted as required, especially the stirring intensity is enhanced when saponification and extraction are synchronous, and saponification and extraction effects are greatly accelerated.

6) The vertical a plurality of fender flow boards that set up in interval on the cylindricality of drawing jar barrel inner wall, from the top down sets up multiunit paddle formula stirring vane on the (mixing) shaft, can change the stirring mode of drawing jar interior material, makes it all form the stirring in the axial of (mixing) shaft and radial, makes the saponification draw more abundant and the reaction of material contact more violent, and the saponification is drawed with higher speed, and is effectual.

7) The temperature control device is adopted to carry out temperature interlocking control on the heat exchange system in a DCS or PLC control mode, the operating conditions of saponification and extraction reaction can be accurately adjusted, the operation of optimal parameters is ensured, the reduction of saponification extraction rate caused by insufficient temperature or temperature runaway is avoided, the production cost is increased, and the reaction time is prolonged.

Drawings

FIG. 1 is a schematic view of the internal structure of an extraction tank according to the present invention;

FIG. 2 is a schematic view of a heating device of an extraction tank according to the present invention;

FIG. 3 is a schematic view of a process for extracting protein material from fermentation broth according to the present invention;

FIG. 4 is a schematic view of an extraction tank and heat exchange system and reflux apparatus arrangement of the present invention;

FIG. 5 is a schematic view of the temperature control device in the extraction tank.

In the figure: 1-an extraction tank, 10-an upper cylinder body and 11-a lower cylinder body; 12-a stirring device, 13-a stirring motor, 14-a feeding hole, 15-a backflow hole, 16-an exhaust hole, 17-a flow baffle, 18-a first heating device, 19-a discharging hole and 30-a first common heat exchange network; 40-a first independent heat exchange network; 50-compressed air line; 51-a compressed air valve; 60-a second common heat exchange network; 70-a second independent heat exchange network; 80-a reflux unit; 81-gas phase line; 82-plate heat exchanger; 83-liquid phase line; 84-an exhaust; 120-stirring shaft, 121-first blade group, 122-second blade group, 123-third blade group, 124-fourth blade group, 125-fifth blade group, 126-bottom bearing, 127-connecting plate, 180-heating coil, 181-steam inlet pipe, 182-steam outlet pipe, 183-steam distribution plate, 184-condensate collecting plate, 401-first steam pipe network; 402-a first chilled water piping network; 4011-steam inlet pipe; 4012-steam admission valve; 4013-condensate valve; 4014-condensate pipe; 4021-cooling the water inlet pipe; 4022-a water inlet valve; 4023-a water return valve; 4024-Cooling the Return pipe.

Detailed Description

In order to better explain the context of the utility model, the utility model is further described below by means of specific examples, which should not be construed as limiting the scope of the utility model thereto, all features disclosed in the context of the utility model, or all steps of a method or process disclosed, may be combined in any way, except for mutually exclusive features and/or steps. Any feature disclosed in this application may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.

In describing embodiments of the present invention, the terms "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship that is based on the orientation or positional relationship shown in the associated drawings, which is for convenience and simplicity of description only, and does not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, the above-described terms should not be construed as limiting the present invention.

The utility model provides an extraction tank for extracting protein substances from fermentation mushroom dregs.

An extraction tank comprises a tank body, a stirring device, a flow baffle, a heat exchange system and a temperature control device; wherein the content of the first and second substances,

the heat exchange system is fixedly arranged on the extraction tank and connected with the temperature control device.

Preferably, agitating unit includes the (mixing) shaft, the one end of (mixing) shaft is connected with agitator motor, is located go up in the barrel (mixing) shaft upper portion is equipped with at least a set of stirring vane group, preferably is equipped with first blade group, second blade group and third blade group from top to bottom in proper order, is located in down in the barrel the lower part of (mixing) shaft is equipped with at least a set of stirring vane group, preferably is equipped with fourth blade group and fifth blade group, the blade group including two blade shape blades of symmetry, the blade of adjacent two sets of blade groups with the central axis contained angle of (mixing) shaft forms the antisymmetric arrangement.

Preferably, the plurality of flow baffles are circumferentially arranged along the inner wall of the upper cylinder of the extraction tank at equal intervals, more preferably, the lower ends of the plurality of flow baffles extend to the joint of the inner wall of the upper cylinder and the inner wall of the lower cylinder, more preferably, at least one flow guide hole is arranged at the position of the flow baffles close to the inner wall of the upper cylinder of the extraction tank, preferably, 3 to 6 flow guide holes are arranged at equal intervals along the length direction of the flow baffles at the upper part, the middle part and the lower part of the flow baffles, and the diameter of the flow guide hole is 50 to 100 mm.

Preferably, the top of the extraction tank is also provided with an air outlet and a reflux port, the center of the bottom of the extraction tank is provided with a discharge port, and the discharge port of the extraction tank is connected with a discharge pump; the exhaust port is connected with a tail gas collecting system for tail gas treatment.

Preferably, the bottom end of (mixing) shaft suit end bearing, the (mixing) shaft can rotate in the end bearing, end bearing fixed connection in draw the tank bottoms portion, more preferably end bearing pass through the fixed welding of connecting plate draw the tank bottoms portion, connecting plate one end is fixed end bearing's periphery, the other end is fixed draw the tank bottoms portion, more preferably end bearing through 3 connecting plate fixed welding for (mixing) shaft axis symmetric distribution draw the tank bottoms portion. Preferably, the extraction tank uses a variable frequency speed regulating motor to control a stirring shaft of the stirring device.

Preferably, an electric butterfly valve, a sight glass and an electric ball valve are sequentially arranged at a discharge port at the bottom of the extraction tank through pipelines, a light phase discharge pipeline and a cleaning pipeline are sequentially communicated on a pipeline between the electric butterfly valve and the sight glass, and the light phase discharge pipeline is connected with a light phase pump and used for conveying light phase extraction liquid; the cleaning pipeline is used for cleaning a discharge pipeline behind an electric butterfly valve at the bottom of the extraction tank, and preferably, the cleaning pipeline is connected with nitrogen purging and/or solvent cleaning.

Preferably, the first independent heat exchange network comprises a first steam pipe network and a first cooling water pipe network; the first steam pipe network comprises a steam inlet pipe, a steam inlet valve, a condensate valve and a condensate pipe, steam enters the first common heat exchange network from the steam inlet pipe through the steam inlet valve, and after materials in the extraction tank are heated, steam condensate flows out of the first common heat exchange network, returns to the first steam pipe network, passes through the condensate valve and flows into the condensate header pipe; the first cooling water pipe network comprises a cooling water inlet pipe, a water inlet valve, a water return valve and a cooling water return pipe, cooling water enters the first common heat exchange network from the cooling water inlet pipe through the water inlet valve, and after the materials in the extraction tank are cooled, cooling water flows out of the first common heat exchange network, returns to the first cooling water pipe network, passes through the water return valve and then flows into a cooling water return main pipe; more preferably, a compressed air line is arranged on a pipeline of the steam inlet valve of the first steam pipe network and/or the water inlet valve of the first cooling water pipe network communicated with the first common heat exchange network, and a compressed air valve is arranged on the compressed air line.

Preferably, the heat exchange system further comprises a second common heat exchange net arranged on the inner wall and/or the outer wall of the conical lower cylinder body of the extraction tank, and a second independent heat exchange net arranged outside the extraction tank and communicated with the second common heat exchange net; and the second common heat exchange net and the second independent heat exchange net are used for heating or cooling the materials in the conical lower cylinder body of the extraction tank.

Preferably, the second common heat exchange net and the second independent heat exchange net heat the material in the cylinder under the conical shape of the extraction tank through steam heat exchange or electric heating, and the second common heat exchange net and the second independent heat exchange net cool the material in the cylinder under the conical shape of the extraction tank through cooling water heat exchange.

Preferably, the temperature control device comprises a temperature detection module, a temperature conversion module and a temperature program control module; the temperature detection module detects a material temperature signal in the extraction tank, the material temperature signal is transmitted to the temperature program control module through the temperature conversion module, the temperature program control module judges the temperature signal and outputs a temperature control signal according to a judgment result to drive the heat exchange system to act.

Preferably, the temperature detection module comprises temperature detection points arranged at the upper part, the middle part and the lower part of the extraction tank body, and thermometers arranged at the temperature detection points, wherein the thermometers adopt platinum thermal resistors or temperature transmitters.

Preferably, the temperature conversion module may convert the temperature signal received from the temperature detection module into a standard meter signal.

Preferably, the temperature program control module outputs a temperature control signal to drive the heat exchange system to act by adopting a numerical comparison, logic judgment and digital quantity output function of a DCS or PLC control system; the action of the heat exchange system comprises inputting heat to the extraction tank, stopping inputting heat, withdrawing heat or stopping withdrawing heat by adjusting the steam flow and/or cooling water flow of the first independent heat exchange net and/or the second independent heat exchange net, and realizing accurate control of the temperature of the materials in the extraction tank.

Preferably, the temperature control device comprises two sets of independent DCS or PLC temperature control devices, and the two sets of independent DCS or PLC temperature control devices respectively control and adjust the steam flow and/or the cooling water flow of the first independent heat exchange network and the second independent heat exchange network.

Preferably, the first common heat exchange net is a first heating device arranged on the inner wall of the extraction tank and/or the outer wall of the upper cylinder body, the first heating device is a steam heating coil, and steam is introduced to heat the material in the extraction tank; more preferably, the first heating device comprises a heating coil arranged on the inner wall of the upper barrel body of the extraction tank, a steam distribution disc and a condensed water collection disc which are arranged on the outer wall of the upper barrel body of the extraction tank, and the steam distribution disc is communicated with the condensed water collection disc through the heating coil.

Preferably, the heating coil is arranged along the upper cylinder of the extraction tank in a longitudinally folded manner.

Preferably, draw and vertically set up 1 at least group heating coil on the barrel inner wall on the jar, more preferably along go up barrel inner wall circumference evenly sets up 4 ~ 8 groups heating coil at equal interval angle, heating coil's steam inlet pipe and steam outlet pipe set up draw on the jar barrel outer wall.

Preferably, the steam inlet pipe of the heating coil penetrates through the upper cylinder wall of the extraction tank and is communicated to a ring-shaped steam distribution disc sleeved on the extraction tank body, the steam outlet pipe of the heating coil penetrates through the upper cylinder wall of the extraction tank and is communicated to a ring-shaped condensed water collection disc sleeved on the extraction tank body, and the ring-shaped condensed water collection disc is positioned below the ring-shaped steam distribution disc; the steam enters from the annular steam distribution disc and flows through the heating coil and the annular condensed water collection disc in sequence to complete heating of the extraction tank.

The steam pressure of the heating coil is 0.3-0.8 MPa, the temperature is 160-180 ℃, and the flow rate is 2-3 tons/hour.

Preferably, the first common heat exchange net is a first cooling device arranged on the inner wall of the extraction tank and/or the outer wall of the upper cylinder body, and the first cooling device utilizes the first heating device to introduce cooling water for cooling the materials in the extraction tank; the temperature of the cooling water is 14-25 ℃, preferably 14-17 ℃, the pressure is 0.2-0.3 Mpa, and the flow is 30-40 cubic/hour.

Preferably, the water outlet pipe and the cover of cooling water are established draw the annular steam distribution dish intercommunication on the jar body, the water inlet pipe and the cover of cooling water are established draw the annular comdenstion water catch tray intercommunication on the jar body, the cooling water is followed the water inlet pipe gets into annular comdenstion water catch tray flows through in proper order heating coil follow behind the annular steam distribution dish the water outlet pipe flows out, and the completion is right draw the cooling of jar.

Preferably, the extraction tank top is further provided with: a manhole for maintenance, a lamp hole for illumination and a sight glass hole for observation.

Preferably, a backflow device for condensing and refluxing the solvent and/or the extracting agent is arranged at the backflow port on the top of the extraction tank, and an exhaust device is installed at the top end of the backflow device.

Preferably, reflux unit is the backward flow condenser pipe, preferentially is cooling water backward flow condenser pipe, follows it gets into to draw volatile solvent of jar tank deck and/or extractant the cooling water backward flow condenser pipe after by the cooling, the condensation be the liquid phase reflux again extremely draw the jar, exhaust apparatus is installed on the top of backward flow condenser pipe.

Preferably, the reflux device is a reflux condensation system comprising a gas phase pipeline, a plate heat exchanger and a liquid phase pipeline, the solvent and/or extractant volatilized from the top of the extraction tank enters the plate heat exchanger positioned above the extraction tank through the gas phase pipeline, is cooled and condensed into a liquid phase through heat exchange of the plate heat exchanger, and then flows back to the extraction tank through the liquid phase pipeline, and an exhaust device is installed on the liquid phase pipeline; the plate heat exchanger adopts cooling water for heat exchange. The reflux device can reduce the solvent loss and realize the recycling of the solvent in the saponification extraction process.

Preferably, the cylinder body and the interface of the extraction tank are made of high-temperature-resistant and high-pressure-resistant 304 stainless steel; the extraction tank is provided with a temperature detection point, a pressure detection point and a sampling point; the operation temperature of saponification and extraction reaction of the extraction tank is 20-70 ℃, and more preferably 50-58 ℃.

Preferably, the extraction tank can be used for extracting protein substances of the fermentation mushroom dregs, the extraction tank can be used for saponification and extraction reaction of the fermentation mushroom dregs, and the extraction tank can be used for saponification extraction of ergosterol.

The present invention is described in detail below with reference to the drawings and the specific embodiments, which are not repeated herein, but the embodiments of the present invention are not limited to the following embodiments.

Extracting pot

FIG. 1 is a schematic view of the internal structure of an extraction tank according to the present invention; FIG. 2 is a schematic view of a heating device of an extraction tank according to the present invention; fig. 4 is a schematic diagram of an extraction tank and heat exchange system and reflux device arrangement of the present invention.

As shown in fig. 1, the extracting tank 1 includes a cylindrical upper cylinder 10 and a conical lower cylinder 11 connected up and down, and the lower cylinder 11 may be provided in other shapes, such as an elliptical shape or a hemispherical shape. The central stirring device 12 is arranged at the center of the extraction tank 1, the flow baffle plate 17 is arranged on the inner wall of the extraction tank 1, the feed inlet 14, the return port 15 and the exhaust port 16 are arranged at the top of the extraction tank 1, and the discharge outlet 19 is arranged at the center of the bottom of the extraction tank 1. Reaction materials such as fermentation mushroom dregs, a solvent, a saponifier, an extractant and the like can be added into the extraction tank 1 through the feed inlet 14. The exhaust port 16 is used for discharging reaction tail gas, and the exhaust port 16 is connected with a tail gas collecting system for treating the tail gas; the reflux port 15 is used for condensing and refluxing the solvent vapor generated in the extraction reaction.

As shown in fig. 1, the stirring device 12 includes a stirring shaft 120, one end of the stirring shaft 120 is connected with a stirring motor 13, the upper portion of the stirring shaft 120 located in the upper cylinder 10 is sequentially provided with a first blade group 121, a second blade group 122 and a third blade group 123 from top to bottom, the lower portion of the stirring shaft 120 located in the lower cylinder 11 is provided with a fourth blade group 124 and a fifth blade group 125, all the blade groups include two blades symmetrically arranged along the central axis of the stirring shaft 120, preferably blade-shaped blades, the blade planes of the two adjacent blade groups are arranged in a reverse direction with the central axis of the stirring shaft 120, the included angle is measured by observing the extraction tank 1 from the tank top to the tank bottom, for example, the included angle between the blades of the first blade group 121 and the central axis of the stirring shaft 120 is 60 degrees, the included angle between the blades of the second blade group 122 and the central axis of the stirring shaft 120 is 120 degrees, and the sum of the included angles is 180 degrees. The paddle-shaped blade arrangement is beneficial to forcibly stirring the materials in the extraction tank and enhancing the reaction among the solvent, the saponifier and the fermentation mushroom dregs.

The upper cylinder 10 of the extraction tank 1 is vertically provided with a plurality of baffle plates 17 at intervals, preferably, the baffle plates 17 are arranged along the inner wall of the upper cylinder 10 of the extraction tank 1 at equal intervals in circumferential direction, for example, 4 baffle plates 17 are arranged along the inner wall of the upper cylinder 10 of the extraction tank 1 at equal intervals in circumferential direction symmetrically, that is, the baffle plates are arranged along the inner wall of the upper cylinder 10 of the extraction tank 1 at equal intervals in circumferential direction by 90 degrees, and for enhancing the baffle turbulent flow effect, the lower end of the baffle plate 17 is extended to the joint between the inner wall of the upper cylinder 10 and the inner wall of the lower cylinder 11. Due to the arrangement of the flow baffle plate 17, when the stirring shaft 120 rotates to stir materials, the materials are blocked when centrifugal force generated by the rotation of the cylinder wall touches the flow baffle plate 17 on the inner wall of the upper cylinder 10, so that the materials are forced to move upwards along the surface of the flow baffle plate 17 to form an axial stirring effect, and then the materials and the radial movement of the materials generated by the rotation of the stirring shaft are overlapped to form turbulent flow, thereby accelerating the mixing degree of the materials and increasing the extraction effect in the stirring process. In order to avoid the influence on material mixing caused by dead angles during stirring, 3 flow guide holes (not shown in the figure) with the diameter of 50mm are arranged at the position, close to the inner wall of the upper cylinder body of the extraction tank 1, of the flow baffle plate 17 at equal intervals along the upper part, the middle part and the lower part of the flow baffle plate 17 in the length direction, and the flow guide holes can guide material fluid at the positions of the flow baffle plate and the inner wall of the upper cylinder body of the extraction tank to pass through at an accelerated speed, so that the material at the position is driven to be blended into turbulence formed by superposition of axial and radial movement of the material generated by rotation of the stirring shaft, and the material mixing effect is enhanced.

As shown in fig. 1, 2 and 4, in order to accelerate the saponification and the extraction reaction, the extraction tank 1 is provided with a first common heat exchange network 30 which is arranged in the extraction tank 1 in the heat exchange component part, and a first independent heat exchange network 40 which is communicated with the first common heat exchange network 30 is arranged outside the extraction tank 1, wherein the first independent heat exchange network 40 comprises a first steam pipe network 401 and a first cooling water pipe network 402, and the first common heat exchange network 30 has dual functions of heating and cooling. When the extraction tank 1 is used for saponifying and extracting protein substances (such as ergosterol) from the fermentation mushroom dreg material, the first common heat exchange net 30 is the first heating device 18 which plays a role in heating the material; after the materials in the extraction tank 1 are saponified and extracted, the first common heat exchange net 30 is the first cooling device which cools the reaction materials by using cooling water before the subsequent filtering process is required. The first heating device and the first cooling device share the equipment and the pipeline of the first common heat exchange network 30, and the heating or cooling of the materials in the extraction tank 1 is switched and completed according to the reaction requirement. By switching the first steam pipe network 401 and the first cooling water pipe network 402, the first common heat exchange network 30 changes the heat medium to heat or cool the material in the extraction tank 1. The first steam pipe network 401 comprises a steam inlet pipe 4011, a condensed water pipe 4014, a steam inlet valve 4012 arranged between the steam inlet pipe 4011 and the first common heat exchange network 30, and a condensed water valve 4013 arranged between the condensed water pipe 4014 and the first common heat exchange network 30. The first cooling water network 402 includes a cooling water inlet pipe 4021, a cooling water return pipe 4024, a water inlet valve 4022 provided between the cooling water inlet pipe 4021 and the first common heat exchange network 30, and a water return valve 4023 provided between the cooling water return pipe 4024 and the first common heat exchange network 30.

The first heating means 18 comprises a heating coil 180 vertically disposed on the inner wall of the upper cylinder 10 of the extraction tank 1, a steam distribution plate 183 and a condensed water collection plate 184 mounted on the outer wall of the upper cylinder 10 of the extraction tank 1. In the present embodiment, as needed, a plurality of sets of heating coils 180 may be installed and arranged at equal intervals in the circumferential direction along the inner wall of the upper cylinder 10 of the extraction tank 1, for example, 8 sets of heating coils 180 may be installed and arranged at 45 degrees in the circumferential direction along the inner wall of the upper cylinder 10 of the extraction tank 1. Because the heating coil 180 is vertically arranged on the inner wall of the upper barrel 10 of the extraction tank 1, the similar stirring and flow blocking effect of the flow blocking plate 17 can be achieved, so that the material mixing degree is accelerated, and the extraction effect in the stirring process is increased.

The solvent and the extractant generate gas in the heating reaction process of the extraction tank 1 due to heating and volatilization, the pressure in the extraction tank 1 can be increased, the saponification and extraction effects can be reduced on one hand, and the potential safety hazard can be generated on the other hand. In order to ensure the safe and stable operation of the extraction tank and the saponification and extraction effects, a backflow port 15 is arranged at the top of the extraction tank 1, and a backflow device 80 with a heat exchange condenser is arranged in an upward extending manner from the backflow port 15. As shown in fig. 4, the reflux apparatus 80 includes a gas phase pipe 81, a plate heat exchanger 82, and a liquid phase pipe 83. The reflux unit 80 may be a cooling water reflux condenser tube. When the gas phase of the solvent or the extracting agent after volatilization enters the reflux device 80 from the reflux port 15 through the gas phase pipeline 81, the gas phase is cooled by cooling water in the plate heat exchanger 82 and condensed and then flows back to the extraction tank 1 through the liquid phase pipeline 83, so that the safety problem and loss of the solvent and the extracting agent caused by heating and volatilization can be eliminated, and the normal operation of the extraction reaction is also ensured. In order to ensure the safety of production and maintenance, an exhaust device 84 is also arranged on the liquid phase pipeline 83. In addition, the reflux device 80 may be a cooling water reflux condenser tube, and the gas phase after the solvent or the extractant is volatilized is directly condensed and refluxed to the extraction tank 1.

As shown in fig. 2 and 4, when the extraction tank 1 is used for saponification extraction, the first heating device 18 is a steam heating coil, the heating coil 180 penetrates through the wall of the upper cylinder 10 of the extraction tank 1 and is communicated with a steam distribution disc 183 through a steam inlet pipe 181, heat is provided for saponification and extraction reaction of materials in the extraction tank 1 by inputting hot steam, and the heating coil 180 penetrates through the wall of the upper cylinder 10 of the extraction tank 1 and is communicated with a condensed water collection disc 184 through a steam outlet pipe 182. Hot steam from the steam inlet pipe 4011 exchanges heat with materials in the extraction tank 1 through the heating coil 180 through the steam inlet valve 4012, condensed water formed by cooling and condensation flows into a condensed water collecting disc 184 through a steam outlet pipe 182, finally enters a condensed water pipe 4014 through a condensed water valve 4013, and the condensed water enters a sewer to be directly discharged or is collected into a hot water tank to provide waste heat for equipment needing hot bath or water heating equipment in a factory.

As shown in fig. 4, after the fermentation residue material in the extraction tank 1 is saponified and extracted, the first common heat exchange network 30 is switched to the first cooling device to cool the reacted material. Cooling water from a cooling water inlet pipe 4021 of a first cooling water pipe network 402 enters the heating coil 180 through a water inlet valve 4022 through a condensed water collecting disc 184 to perform heat exchange with materials in the extraction tank 1 to reduce the temperature of the materials in the extraction tank 1, heated hot water flows into a steam distribution disc 183 through a steam outlet pipe 182 and enters a cooling water return pipe 4024 through a water return valve 4023, and the hot water enters a cold water return header pipe or is collected to enter a hot water tank to provide waste heat for equipment needing hot bath or water heating equipment in a plant area.

In order to accelerate the saponification and extraction reaction of the materials and accelerate the heat exchange of the materials, the temperature of the materials in the extraction tank 1 is uniform, the reaction time is shortened, the temperature rise or the temperature reduction of the materials is accelerated, and the extraction tank 1 controls the rotating speed of the stirring shaft 120 by using the variable-frequency speed-regulating motor 13. In order to clean water in the pipeline in maintenance and convenient to disassemble and assemble or weld, and in heating and cooling switching, steam and water in the pipeline are cleaned, a compressed air pipeline 50 is arranged on the pipeline between the first steam pipe network 401, the first cooling water pipe network 402 and the first common heat exchange network 30, and a compressed air valve 51 is arranged on the compressed air pipeline 50.

Through the extraction tank of above-mentioned design, the saponification of protein material in the fermentation fungus sediment and extraction reaction speed obviously obtain promoting by a wide margin, need not carry out secondary saponification, secondary extraction to the fermentation fungus sediment moreover, and primary saponification, extraction reaction just can realize fully extracting protein material (for example ergosterol) in the fermentation fungus sediment, have promoted extraction production efficiency greatly. In addition, through forcing the cooling to the extract in the extraction tank, not only can the waste heat be retrieved and energy-conserving, can reduce the loss of menstruum in the production moreover, reduce cost improves the operational safety.

(II) saponification extraction process of protein substances in fermentation fungus residues

FIG. 3 is a schematic view of a process for extracting protein material from fermentation broth according to the present invention; FIG. 5 is a schematic view of the temperature control device in the extraction tank.

As shown in FIG. 3, the fermented residue from penicillin is directly added into an extraction tank, a metered solvent is added, a first heating device of the extraction tank is started, the fermented residue and the solvent are heated, and stirring is carried out. After the temperature is raised to the preset saponification temperature, the measured saponifying agent is added, and the mixture is continuously stirred to generate saponification reaction. Adding extractant, and heating and stirring to obtain extract containing ergosterol.

In an extraction tank, stopping stirring, maintaining the temperature of extraction reaction, standing the extracted reactants, naturally layering the reactants, wherein the lower layer is a heavy phase, the upper layer is a light phase, the heavy phase is mainly a mixture of methanol, water, protein, hypha, cell wall residues after saponification wall breaking and the like, the light phase is an n-heptane solution dissolved with ergosterol and a small amount of protein, and the light phase also contains a small amount of macromolecular solid particles.

Because the control of the reaction temperature for the saponification extraction of ergosterol from the fermentation strain residues has a great influence on the efficiency of the saponification and extraction reaction and the yield of the product, the reaction temperature for the saponification extraction of ergosterol needs to be timely regulated.

As shown in fig. 5, a temperature control device is used to control the material reaction temperature of the extraction tank 1. The temperature control device comprises a temperature detection module, a temperature conversion module and a temperature program control module, wherein the temperature detection module detects material temperature value signals in the extraction tank 1, temperature detection points can be arranged at the upper part, the middle part and the lower part of the extraction tank body, a platinum thermal resistance thermometer is adopted for measurement, the temperature conversion module converts the received temperature signals into standard instrument signals and transmits the standard instrument signals to the temperature program control module, and the temperature program control module judges the signals. In one embodiment of the utility model, a DCS temperature control device is adopted, and a temperature program control module adopts the functions of numerical comparison, logic judgment and digital quantity output of a DCS system and outputs a temperature control signal to a heat exchange system for heat exchange operation; the heat exchange system inputs heat to the extraction tank, stops inputting heat, withdraws heat or stops withdrawing heat by adjusting the steam flow and/or the cooling water flow of the first independent heat exchange net and/or the second independent heat exchange net, and realizes temperature control of materials in the extraction tank.

In an embodiment of the present invention, when the material is added into the extraction tank to perform a saponification extraction reaction, and the temperature detection module detects that the temperature of the material in the extraction tank 1 is lower than a preset temperature value a (for example, 20 to 50 ℃), the temperature control device starts the temperature program control module to drive the heat exchange system to input heat to the extraction tank, at this time, the first cooling water pipe network 402 is closed, the first steam pipe network 401 opens the steam inlet valve 4012 of the steam inlet pipe 4011 to the extraction tank 1, and the hot steam enters the first common heat exchange network 30 to heat the saponification extraction material in the extraction tank 1; when the temperature of the material in the extraction tank 1 rises to be close to a preset temperature value A, the opening of the steam inlet valve 4012 is reduced until the steam inlet valve is closed, so that the heat input of the heat exchange system to the extraction tank 1 is reduced; if the temperature of the material in the extraction tank 1 exceeds a preset temperature value B (for example, 58-70 ℃), the temperature program control module outputs a temperature control signal to drive the heat exchange system to withdraw heat from the extraction tank, at this time, the first steam pipe network 401 is closed, the first cooling water pipe network 402 can be started, and cooling water (for example, cold water at 14-17 ℃) is injected into the heat exchange system to cool the material.

After the extraction tank 1 is filled with materials to complete saponification extraction reaction, in order to reduce the loss of solvents in the subsequent filtration process, reduce cost and improve operation safety, and meanwhile, the extraction solution in the extraction tank can be forcibly cooled by recycling waste heat. When the temperature detection module detects that the temperature of the material in the extraction tank 1 is higher than a preset temperature value C (for example, 30-40 ℃), the temperature control device starts the temperature program control module to drive the heat exchange system to withdraw heat from the extraction tank 1; at this time, the first steam pipe network 401 is closed, the first cooling water pipe network 402 starts a water inlet valve 4022 of a cooling water inlet pipe 4021 to input cooling water to the first common heat exchange network 30 for cooling; when the temperature of the material in the extraction tank 1 approaches the preset temperature value C, the opening of the water inlet valve 4022 is reduced until it is closed to reduce the heat withdrawal to the extraction tank 1.

The temperature control device also can comprise two sets of independent DCS or PLC temperature control devices, the steam flow and/or the cooling water flow of the first independent heat exchange net and the second independent heat exchange net are respectively controlled and adjusted, and materials in the upper barrel body and the conical lower barrel body of the extraction tank are simultaneously regulated and controlled so as to accelerate the material mixing uniformity of saponification extraction reaction and realize the rapid temperature uniformity of the materials.

As shown in fig. 3, a discharge valve at the bottom of the extraction tank is opened, the heavy phase in the extraction tank is discharged into a heavy phase collection device through a heavy phase discharge pipeline, the heavy phase is firstly filtered by a pump, residues of cell walls after saponification and wall breaking and heavy phase filtrate are separated, and the heavy phase filtrate enters a subsequent phase separation tank for phase separation; when the heavy phase in the extraction tank is completely discharged, switching to a light phase pipeline, discharging the light phase in the extraction tank into a light phase collection device through the light phase pipeline, filtering the light phase, separating large particle impurities in the light phase and light phase filtrate, and feeding the light phase filtrate into a subsequent phase splitting tank for phase splitting.

The heavy phase filtrate and the light phase filtrate can be fed into a subsequent phase separation tank together for phase separation and standing delamination, or can be fed into different phase separation tanks separately for phase separation, and in actual production, the heavy phase filtrate and the light phase filtrate are preferably fed into different phase separation tanks separately for phase separation and standing delamination. Wherein, the solvent and the water (i.e. heavy phase) are separated from the lower layer of the phase separation tank and are continuously recovered and recycled to the extraction unit for use, and the upper layer liquid (i.e. light phase) containing the ergosterol and the extractant is separated from the upper layer of the phase separation tank and enters the crystallization unit for preparing the ergosterol.

As shown in fig. 3, the light phase enters a decoloring tank for decoloring, a decoloring agent (preferably activated carbon) is added, heating is carried out, decoloring is carried out under stirring, hot filtration is carried out, filtrate is collected, the collected filtrate is heated and distilled under negative pressure, and the condensing and recycling extractant is recycled to an extraction unit for use. And continuously cooling the concentrated solution, and filtering to obtain a solid ergosterol crude product. The hot filtering in the decolorization aims to avoid that part of the product is crystallized and separated out and a decolorizer is filtered together after the temperature of the filtrate is reduced, so that the extraction rate is influenced.

And adding the ergosterol crude product into a recrystallization container, adding a recrystallization solvent, heating until the crude product is completely dissolved, then cooling and crystallizing according to a program, filtering and drying to obtain the ergosterol product.

The saponification and extraction reactions for extracting protein substances (such as ergosterol) from the fermentation fungus residues are carried out in the same reaction kettle, namely the extraction tank, so that the complex process operations of setting the saponification and extraction reactions in different reaction kettles, filtering, cooling and re-heating in the middle are reduced in the prior art, the production process flow is simplified, and the production energy consumption can be reduced. In addition, the standing and layering treatment in the extraction tank can achieve the effect of primary phase separation, so that the extraction efficiency of protein substances (such as ergosterol) can be improved, the whole extraction time is greatly shortened, intermediate operation links are reduced, the loss in the extraction of the protein substances (such as ergosterol) can be reduced, and the purity of crude products of the protein substances (such as ergosterol) is also improved to a certain extent.

The utility model can be used for extracting the ergosterol by using the ergosterol contained in the penicillin fermentation mushroom dregs, and can also be used for extracting the ergosterol by using mushroom dregs produced by other similar antibiotics, but the ergosterol content is greatly different due to different strains and fermentation processes.

Method for detecting ergot product

1. Appearance detection

And detecting the appearance crystal form and color by naked eyes, and comparing with a standard substance.

2. Purity detection

A detection instrument: high Performance Liquid Chromatography (HPLC) with ultraviolet detector.

The detection method comprises the following steps: 100% methanol in fluidity; an appropriate amount of ergosterol was dissolved in methanol solvent without using ultrasonic waves. Extracting a proper amount of sample to be detected by using a microsyringe, injecting the sample to be detected into HPLC, detecting the wavelength of 281 nanometers, and detecting a column: conventional C18 column.

(IV) examples

In the following, the ergosterol is extracted from the penicillin fermentation residues as an example, and the structure and the function of the extraction tank are further described, so that the embodiments 1 to 9 are completed. By way of comparison, example 10 is completed with reference to CN 201810432608. The extraction raw material is penicillin fermentation bacteria residue with the water content of 70 percent.

Description of the experimental conditions: in each of examples 1 to 10, crystallization was carried out using a 100L glass reactor, a 50L separatory funnel, a mini centrifuge (for heavy phase filtration), a 25L rotary evaporator (for concentration), and a 20L crystallization vessel. The relevant results are illustrated below.

Example 1

(1) Saponification extraction: weighing 1kg of penicillin fermentation residues, adding the penicillin fermentation residues into an extraction tank, adding 1.2kg of methanol, heating by steam at 160 ℃ and under the pressure of 0.3-0.4 Mpa to maintain the temperature at 55 ℃, adding 70g of solid sodium hydroxide, stirring for 6 hours, then adding 1.2kg of petroleum ether to maintain the temperature at 50 ℃, stirring for 3 hours, completing saponification and extraction, and standing and layering in the extraction tank.

(2) Filtering and phase separation: and (2) standing and phase splitting the material extracted and reacted in the step (1), filtering the light phase, filtering the heavy phase, performing vacuum suction filtration, collecting filtrate, pumping the filtrate into a phase splitting tank, standing and layering, collecting upper-layer light-phase liquid, and recovering a lower-layer solvent. Simultaneously, 0.5kg of filter cake is collected.

(3) Decoloring and crystallizing: and (3) adding the upper-layer liquid collected in the filtering and phase-splitting in the step (2) into a decoloring tank with a stirring device, maintaining the temperature at 50 ℃, adding 1g of activated carbon, stirring for 2 hours, filtering while hot, collecting filtrate, heating and distilling the collected filtrate under negative pressure, and condensing to recover petroleum ether. And cooling the concentrated solution to 10 ℃, and filtering to obtain 0.7g of white solid, namely the ergosterol crude product. The time required for concentration and crystallization was 2 hours.

The ergosterol extraction was 0.07% and the purity was analyzed to be 87%. The extraction time is greatly shortened, and the time from feeding to obtaining the crude product of the ergosterol is shortened to 13 hours, wherein the time for obtaining the ergosterol extract is 9 hours. The ergosterol product is observed to be white powder in appearance and slightly poor in crystal form.

Example 2

(1) Saponification extraction: weighing 1kg of penicillin fermentation fungus residues, adding the penicillin fermentation fungus residues into an extraction tank, adding 1.2kg of methanol, heating by steam at 160 ℃ and under the pressure of 0.3-0.4 Mpa to maintain the temperature at 55 ℃, adding 70g of solid sodium hydroxide, stirring for 6 hours, then adding 1.2kg of petroleum ether, maintaining the temperature at 50 ℃, stirring for 3 hours to complete saponification and extraction, cooling the saponified and extracted materials to 30-40 ℃ by 17 ℃ cooling water, and standing and layering for 10 minutes in the extraction tank.

(3) 2 times of extraction of filter cakes: adding 0.6kg of petroleum ether into the extraction tank, and then adding 0.5kg of filter cake generated after filtering and phase separation in the step (2); heating to 50 deg.C, stirring, and extracting at the same temperature for 2 hr.

(4) Filtering and phase separation: and (4) performing vacuum filtration on the material obtained after the 2-time extraction reaction of the filter cake in the step (3), collecting filtrate, pumping the filtrate into a phase separation tank, standing for layering, collecting upper-layer light-phase liquid, and recovering a lower-layer solvent.

(5) Decoloring and crystallizing: and (3) mixing the upper layer light phase liquid collected in the steps (2) and (4), adding the mixture into a decoloring tank with a stirring device, maintaining the temperature at 50 ℃, adding 1.5g of activated carbon, stirring for 2 hours, filtering while the mixture is hot, collecting filtrate, heating and distilling the collected filtrate under negative pressure, and condensing to recover petroleum ether. And cooling the concentrated solution to 10 ℃, and filtering to obtain 0.75g of white solid, namely the ergosterol crude product. The time required for concentration and crystallization was 2 hours.

The ergosterol extraction was 0.075% with an analytical purity of 87%. The extraction time is shortened, and the time from feeding to obtaining the ergosterol crude product is shortened to 15 hours, wherein the time for obtaining the ergosterol extract is 11 hours. The ergosterol product is observed to be white powder in appearance and slightly poor in crystal form.

However, compared with example 1, the loss of the solvent (solvent and extractant) in the subsequent filtration stage is obviously reduced due to the addition of the 17 ℃ cooling water for cooling the saponified and extracted material to 40 ℃ and standing for layering. Saponification extraction is carried out according to 40-50 cubic materials, waste heat of the materials is recovered without cooling, standing and layering are directly carried out, subsequent filtration is carried out, the loss of a solvent is about 2-3 cubic, and filtration is carried out after the waste heat of the materials is recovered by cooling, and the loss of the solvent can be reduced to below 1 cubic.

Example 3

(1) Saponification extraction: weighing 1kg of penicillin fermentation residues, adding the penicillin fermentation residues into an extraction tank, adding 1.2kg of chloroform, heating by steam at 180 ℃ and 0.3-0.4 Mpa to maintain the temperature at 57 ℃, adding 50g of sodium hydroxide, and stirring for 4 hours. 1.2kg of n-heptane was added thereto, and the mixture was stirred for 3 hours while maintaining the temperature at 50 ℃. Saponification and extraction were completed and the layers were allowed to stand for 10 minutes.

(2) Filtering and phase separation: and (2) standing and phase splitting the material extracted and reacted in the step (1), filtering the light phase, filtering the heavy phase, performing vacuum suction filtration, collecting filtrate, pumping the filtrate into a phase splitting tank, standing and layering, collecting upper-layer light-phase liquid, and recovering a lower-layer solvent.

(3) Decoloring and crystallizing: and (3) adding the upper layer light phase liquid collected in the filtering and phase splitting in the step (2) into a decoloring tank with a stirring device, heating to 60 ℃, adding 1g of activated carbon, stirring for 2 hours, carrying out vacuum filtration while the liquid is hot, collecting filtrate, heating and distilling under negative pressure, and condensing and recovering n-heptane. And cooling the concentrated solution to-10 ℃, and performing suction filtration to obtain 1.1g of white solid, namely the ergosterol crude product. The time taken for concentration and crystallization was 4 hours.

The ergosterol extraction was 0.11% and the purity was analyzed to be 88%. The extraction time is greatly shortened, and the time from feeding to obtaining the crude product of the ergosterol is shortened to 7 hours, wherein the time for obtaining the ergosterol extract is 13 hours. The ergosterol product is observed to be white powder in appearance and slightly poor in crystal form.

Example 4

(1) Saponification extraction: weighing 1kg of penicillin fermentation residues, adding the penicillin fermentation residues into an extraction tank, adding 1.2kg of ethanol, heating by using steam at 180 ℃ and under the pressure of 0.3-0.4 Mpa to maintain the temperature at 58 ℃, adding 50g of sodium hydroxide, and stirring for 4 hours. 1.2kg of n-heptane was added thereto, and the mixture was stirred for 3 hours while maintaining the temperature at 50 ℃. Saponification and extraction were completed and the layers were allowed to stand for 10 minutes.

The ergosterol extraction was 0.11% and the purity was analyzed to be 85%. The extraction time is greatly shortened, and the time from feeding to obtaining the crude product of the ergosterol is shortened to 13 hours, wherein the time for obtaining the ergosterol extract is 7 hours. The ergosterol product is observed to be white powder in appearance and slightly poor in crystal form.

Example 5

(1) Saponification extraction: weighing 1kg of penicillin fermentation fungus residue, adding 1.2kg of methanol into an extraction tank, introducing steam with the temperature of 180 ℃ and the pressure of 0.3-0.4 Mpa, heating to maintain the temperature at 58 ℃, adding 50g of sodium hydroxide, condensing, refluxing and stirring in a gas phase for 4 hours. 1.2kg of n-heptane was added, and the mixture was refluxed and stirred for 3 hours while maintaining the temperature at 50 ℃. And (4) finishing saponification extraction, and standing for layering for 10 min.

(3) Decoloring and crystallizing: and (3) adding the upper layer light phase liquid collected in the filtering and phase splitting in the step (2) into a decoloring tank with a stirring device, heating to 60 ℃, adding 1g of activated carbon, stirring for 2 hours, carrying out vacuum filtration while the liquid is hot, collecting filtrate, heating and distilling under negative pressure, and condensing and recovering n-heptane. And cooling the concentrated solution to-10 ℃, and performing suction filtration to obtain 1.2g of white solid, namely the ergosterol crude product. The time taken for concentration and crystallization was 4 hours.

The extraction rate of ergosterol is 0.12%, and the purity is 90%. The extraction time is greatly shortened, and the time from feeding to obtaining the crude product of the ergosterol is shortened to 13 hours, wherein the time for obtaining the ergosterol extract is 7 hours. The ergosterol product is observed to be white powder in appearance and slightly poor in crystal form.

It was found that if no gas phase reflux condensation is performed during the saponification extraction, the solvent loss increases and the extraction rate and purity of ergosterol decrease. The gas phase condensation reflux can reduce solvent loss by 68%, increase extraction rate by 15.8% and improve purity by 3.6%. Therefore, the reflux is carried out in the saponification and extraction processes, which is beneficial for the solvent to play a role in promoting the saponification and extraction.

Example 6

(1) Saponification extraction: weighing 10kg of penicillin fermentation residues, adding the penicillin fermentation residues into an extraction tank, adding 12kg of methanol, introducing steam of 180 ℃ and 0.3-0.4 Mpa, heating to maintain the temperature at 60 ℃, adding 200g of sodium hydroxide, and stirring for 3 hours. 8kg of n-heptane was added thereto, and the mixture was stirred for 2 hours while maintaining the temperature at 55 ℃. Saponification and extraction were completed and the layers were allowed to stand for 10 minutes.

(3) Decoloring and crystallizing: and (3) adding the upper layer light phase liquid collected in the filtering and phase splitting of the step (2) into a decoloring tank with a stirring device, heating to 65 ℃, adding 1g of activated carbon, and stirring for 2 hours. Vacuum filtering, collecting filtrate, distilling the collected filtrate under negative pressure, and condensing to recover n-heptane. Cooling the concentrated solution to 10 ℃ at the cooling speed of 0.5 ℃/min, and performing suction filtration to obtain 10.5g of white solid, namely the ergosterol crude product. The time required for concentration and crystallization was 2 hours.

(4) And (3) recrystallization: and (3) adding the crude product obtained in the step (3) into a recrystallization container with 800g of recrystallization solvent, heating the recrystallization solvent to 50 ℃ until the crude product is completely dissolved, cooling to-10 ℃ at a cooling speed of 1 ℃/min, carrying out suction filtration to obtain white solid, and carrying out vacuum drying to obtain 9.4g of product, namely the ergosterol product. Recrystallization took 4 hours.

The extraction rate of ergosterol is 0.094%, and the purity of the product analyzed is 98%. The extraction time is greatly shortened, and the time from feeding to obtaining the crude product of the ergosterol is shortened to 13 hours, wherein the time for obtaining the ergosterol extract is 5 hours. The ergosterol product is observed to have bright appearance and good crystal form.

Example 7

(1) Saponification extraction: weighing 15kg of penicillin fermentation residues, adding into an extraction tank, adding 900g of solid sodium hydroxide, adding 20kg of methanol, heating by steam at 170 ℃ to maintain the temperature at 55 ℃, and stirring for 3 hours. Adding 18kg of n-heptane, heating and maintaining the temperature at 55-60 ℃, and stirring for 3 hours. Saponification and extraction were completed and the layers were allowed to stand for 10 minutes.

(3) Decoloring and crystallizing: and (3) adding the upper layer light phase liquid collected in the filtering and phase splitting of the step (2) into a decoloring tank with a stirring device, heating to 65 ℃, adding 8g of active carbon, and stirring for 1 hour. Vacuum filtering, collecting filtrate, distilling the collected filtrate under negative pressure, and condensing to recover n-heptane. The concentrate produced by distillation was collected. Cooling the concentrated solution to 5 ℃ at the cooling rate of 1 ℃/min, and filtering to obtain 30.5g of white solid, namely the ergosterol crude product. The time required for concentration and crystallization was 3 hours.

(4) And (3) recrystallization: and (3) adding the crude product obtained in the step (3) into a recrystallization container with 800g of recrystallization solvent, heating the recrystallization solvent to 60 ℃ until the crude product is completely dissolved, cooling to-10 ℃ at a cooling speed of 0.5 ℃/min, performing suction filtration to obtain a white solid, and performing vacuum drying to obtain 14.5g of product, namely the ergosterol product. Recrystallization took 4 hours.

The extraction rate of ergosterol is 0.097%, and the purity of the product analyzed is 98.5%. The extraction time is greatly shortened, and the time from feeding to obtaining the crude product of the ergosterol is shortened to 14 hours, wherein the time for obtaining the ergosterol extract is 6 hours. The ergosterol product is observed to have bright appearance and good crystal form.

Example 8

(1) Saponification extraction: weighing 15kg of penicillin fermentation residues, adding into an extraction tank, adding 900g of solid sodium hydroxide, adding 20kg of methanol, heating by steam at 170 ℃ to maintain the temperature at 58 ℃, and stirring for 3 hours. 15kg of n-heptane was added, and the mixture was heated to maintain the temperature at 55 to 60 ℃ and stirred for 3 hours. Saponification and extraction were completed and the layers were allowed to stand for 10 minutes.

(3) Decoloring and crystallizing: and (3) adding the upper layer light phase liquid collected in the filtering and phase splitting of the step (2) into a decoloring tank with a stirring device, heating to 70 ℃, adding 8g of active carbon, and stirring for 1 hour. Vacuum filtering, collecting filtrate, distilling the collected filtrate under negative pressure, and condensing to recover n-heptane. The concentrate produced by distillation was collected. And cooling the concentrated solution to 5 ℃ at the cooling speed of 1 ℃/min, and performing suction filtration to obtain 33.2g of white solid, namely the ergosterol crude product. The time required for concentration and crystallization was 3 hours.

(4) And (3) recrystallization: and (3) adding the crude product obtained in the step (3) into a recrystallization container with 800g of recrystallization solvent, heating the recrystallization solvent to 60 ℃ until the crude product is completely dissolved, cooling to-20 ℃ at a cooling speed of 0.5 ℃/min, performing suction filtration to obtain white solid, and performing vacuum drying to obtain 27.5g of product, namely the ergosterol product. Recrystallization took 5 hours.

The extraction rate of ergosterol is 0.183%, and the purity of the product analyzed is 99%. The extraction time is greatly shortened, and the time from feeding to obtaining the crude ergosterol product is shortened to 15 hours, wherein the time for obtaining the ergosterol extract is 6 hours. The ergosterol product is observed to have bright appearance and good crystal form.

Example 9

(1) Saponification extraction: weighing 10kg of penicillin fermentation residues, adding the penicillin fermentation residues into an extraction tank, adding 12kg of methanol, heating by steam at 170 ℃ to maintain the temperature at 55 ℃, adding 700g of solid sodium hydroxide, stirring for 4 hours, then adding 12kg of n-heptane, heating to maintain the temperature at 55-60 ℃, and stirring for 3 hours. Saponification and extraction were completed and the layers were allowed to stand for 10 minutes.

(3) Decoloring and crystallizing: and (3) adding the upper layer light phase liquid collected in the filtering and phase splitting of the step (2) into a decoloring tank with a stirring device, maintaining the temperature at 50 ℃, adding 10g of activated carbon, stirring for 1 hour, filtering while hot, collecting filtrate, heating and distilling the collected filtrate under negative pressure, and condensing to recover n-heptane. And cooling the concentrated solution to-10 ℃, and filtering to obtain 20g of white solid, namely the ergosterol crude product. The time required for concentration and crystallization was 3 hours.

(4) And (3) recrystallization: and (3) adding the crude product obtained in the step (3) into a recrystallization container with 800g of recrystallization solvent, heating the recrystallization solvent to 65 ℃ until the crude product is completely dissolved, cooling to-10 ℃ at a cooling speed of 0.5 ℃/min, performing suction filtration to obtain white solid, and performing vacuum drying to obtain 12.5g of product, namely the ergosterol product. Recrystallization took 4 hours.

The extraction rate of ergosterol is 0.125%, and the purity of the product analyzed is 98.5%. The extraction time is greatly shortened, and the time from feeding to obtaining the crude ergosterol product is shortened to 15 hours, wherein the time for obtaining the ergosterol extract is 7 hours. The ergosterol product is observed to have bright appearance and good crystal form.

Example 10 (comparative example to example 5)

According to the process steps and reaction equipment disclosed in the prior art CN201810432608, by referring to example 3, penicillin fermentation mushroom residue is used as a raw material, and a crude ergosterol product is prepared under the conditions of selecting the same raw material formula, the same solvent and extraction agent, heating and other operation parameters of patent example 5, so as to verify the improvement effect of the process.

(1) Saponification: weighing 1kg of penicillin fermentation residues, adding the penicillin fermentation residues into a saponification reaction vessel, adding 1.2kg of methanol, heating the mixture by steam at 180 ℃ to maintain the temperature at 58 ℃, adding 50g of sodium hydroxide, and stirring the mixture for 18 hours. And then cooled to room temperature.

(2) Filtering I: carrying out vacuum filtration on the material in the step (1), and collecting 0.5kg of filter cake; recovering the filtrate.

(3) Extraction: adding 0.5kg of the filter cake in the step (2) into a container with stirring, adding 1.2kg of n-heptane, then adding, and heating to maintain the temperature at 50 ℃ for extraction for 18 hours.

(4) And (4) filtering II: and (4) carrying out vacuum filtration on the material in the step (3), and collecting filtrate.

(5) And (3) distillation: and (4) heating and distilling the filtrate collected in the step (4) at normal pressure, and condensing to recover n-heptane. The residue was cooled to room temperature and filtered to give crude ergosterol product.

(6) And (3) decoloring: and (3) adding the crude product obtained in the step (5) into a closed container, adding 600g of trichloromethane, heating to 50 ℃, stirring until the trichloromethane is completely dissolved, adding 1g of activated carbon, and stirring for 2 hours.

(7) And (3) crystallization: and (4) filtering the mixture obtained in the step (6) while the mixture is hot, collecting filtrate, cooling the filtrate to-10 ℃ at the cooling speed of 0.5 ℃/min, and performing suction filtration to obtain 1.0g of white solid, namely the ergosterol crude product. The time taken for concentration and crystallization was 4 hours.

The ergosterol extraction was 0.10% and the purity was analyzed to be 87%. From the feeding to the obtaining of the ergosterol crude product for 40 hours, the time for obtaining the ergosterol extract is 36 hours. The ergosterol product is observed to be white powder in appearance and slightly poor in crystal form.

Example 11

In order to examine the extraction effect of different extractants, the applicant selects ergosterol with the purity of 98.5%, and respectively dissolves in three solvents of n-heptane, petroleum ether and n-hexane, and observes the solubility experiment of the ergosterol dissolved in the 3 solvents at different temperatures by controlling the temperature, and the research results are shown in table 1, table 2 and table 3.

TABLE 1 solubility of ergosterol in Petroleum Ether

Serial number	Temperature of	Solute (ergosterol)	Solvent (Petroleum ether)	Solubility in water
					1	21℃	86.0mg	100.0g	0.860×10^-3
2	29℃	195.5mg	100.0g	1.955×10^-3
					3	41℃	298.7mg	100.0g	2.987×10^-3
4	45℃	357.3mg	100.0g	3.573×10^-3
					5	50℃	618.4mg	100.0g	6.184×10^-3
6	57℃	771.0mg	100.0g	7.710×10^-3

TABLE 2 solubility of ergosterol in n-heptane

Serial number	Temperature of	Solute (ergosterol)	Solvent (n-heptane)	Solubility in water
					1	21℃	0.100.1g	100.0g	1.01×10^-3
2	29℃	0.205.0g	100.0g	2.05×10^-3
					3	41℃	0.324.3g	100.0g	3.24×10^-3
4	45℃	0.445.3g	100.0g	4.45×10^-3
					5	50℃	0.762.3g	100.0g	7.32×10^-3
6	60℃	1.0163g	100.0g	10.16×10^-3

TABLE 3 solubility of ergosterol in n-hexane

Serial number	Temperature of	Solute (ergosterol)	Solvent (n-hexane)	Solubility in water
					1	21℃	62.2mg	100.0g	0.62×10^-3
2	29℃	167.2mg	100.0g	1.67×10^-3
					3	41℃	265.9mg	100.0g	2.65×10^-3
4	45℃	340.2mg	100.0g	3.40×10^-3
					5	50℃	565.2mg	100.0g	5.65×10^-3

Applicants have found that multiple factors need to be considered in selecting an extractant: the extractant not only has extraction, but also has double functions of dissolution and extraction. The selection standard is 1) good solubility to ergosterol and small solubility to high protein and other impurities; 2) can be layered with solvent water solution, and is convenient for recovering the extractant. The applicant has found, through comparative studies, that the best results are obtained by selecting n-heptane as the extractant.

As can be seen from the solubility data in table 1, table 2, table 3: the ergosterol has the greatest solubility in n-heptane at the same temperature, so the extractant is chosen to be n-heptane. Meanwhile, 50 ℃ was selected as the optimum extraction operation temperature, considering that in this patent, saponification and extraction were performed in the same reaction vessel, and the boiling point of methanol, which is a solvent in the saponification reaction, was 64.7 ℃ while the boiling point of n-heptane, which is an extractant, was 98 ℃, in order to reduce energy consumption and prevent boiling of methanol during the reaction. Therefore, the n-heptane extraction is comprehensively considered and selected, the extraction temperature is 50 ℃, the extraction effect is considered, the power cost and the solvent loss are considered, and the method is more economical and cost-effective.

EXAMPLES 1-10 comparative analysis of extraction results

The results of the ergosterol extraction tests of examples 1-10 are summarized and made in Table 4 to analyze the effect of different extraction processes on the extraction yield and purity of the product.

(1) The one-step extraction feasibility of the utility model is as follows: the extraction results of the comparative example 1 and the example 2 in the table 4 show that the ergosterol extracted by the fermentation mushroom residue for the second time is very limited, the extraction rate is increased from 0.07% to 0.075%, and the increase of the extraction rate is very little, which indicates that the ergosterol extracted by the fermentation mushroom residue process and the extraction tank provided by the patent has a good one-step extraction effect, can fully complete the extraction of the ergosterol in the fermentation mushroom residue, the secondary extraction affects the industrial production efficiency, the raw material consumption is increased, the energy consumption is also increased, and the industrial production is uneconomical. In addition, the secondary extraction is added, and the quality and the purity of the crude ergosterol are not contributed. Therefore, the ergosterol is extracted by the one-step method by adopting the process and the extraction tank of the patent with good effect.

TABLE 4 examples 1-10 comparison of results of ergosterol extraction studies

(2) Selecting a solvent: from the comparison of the extraction results of examples 3, 4 and 5 in table 4, it was found that chloroform, ethanol and methanol can be used as the solvent for the saponification reaction of extracting ergosterol from fermentation broth, and methanol is selected as the solvent, so that the extraction rate of ergosterol is 0.12% at the highest, and the product purity is 90%, and the best effect is obtained. The solvent has two functions, namely, the solvent can dissolve part of protein and polysaccharide and reduce the amount of the protein and polysaccharide counted in an extracting agent so as to improve the purity of the ergosterol product, and the solvent plays a wall breaking role so as to enhance the saponification effect and be beneficial to extracting the ergosterol. The effect of methanol in both aspects is better when n-heptane is selected as the extractant.

In addition, from the comparison of the extraction reaction time data of 1-9 in table 4, it is found that the preparation time of the ergosterol crude product is greatly reduced by adopting the process and the extraction tank equipment of the patent under the condition of selecting n-heptane as the extractant, and the preparation time can be basically shortened to 9 hours by selecting the combination of methanol as the solvent and n-heptane as the extractant, which indicates that the extraction efficiency of the product is higher by adopting the technology of the patent.

(3) And (3) selecting a recrystallization solvent: compared with the refining and purifying effects of 4 solvents of toluene, ethanol, ethyl acetate, ethanol and toluene mixed solution, the extraction data of the embodiment 6-9 in the table 4 show that the two components of the ethanol and toluene mixed solution are selected for the recrystallization of the ergosterol, the effect is the best, the extraction rate of the ergosterol is up to 0.183%, and the product purity is up to 99%.

(4) This patent contrasts with the prior art (CN201810432608 process). From the comparison of the extraction result data of example 5 and example 10 in table 4, it is found that, not only is the extraction rate of ergosterol product high (0.12% in example 5) and the product purity high (90% in example 5) by using the process and extraction tank of the present invention in one step, but also the extraction time of ergosterol is greatly shortened (the preparation time of crude ergosterol product is 9 hours in example 5 and 36 hours in example 10), which indicates that the effect of ergosterol extraction by using the process and extraction tank of the present invention in one step is improved obviously, and for industrial production, not only the production efficiency is improved, but also the energy consumption can be reduced, the product cost can be reduced, and the market competitiveness of the product can be improved. The extraction tank capable of simultaneously completing saponification and extraction is designed, filtration is not needed before extraction, the process flow is simplified, the energy consumption is reduced, the reaction time is greatly shortened, and meanwhile, the loss possibly caused by filtration in the prior art is avoided, so that the extraction rate and the purity of the product can be improved. And the DCS or PLC temperature control device is adopted to carry out linkage control on the saponification extraction temperature, so that the saponification and extraction reaction temperature can be accurately adjusted, the operation of optimal parameters is ensured, the increase of production cost and the extension of reaction time caused by insufficient temperature or temperature runaway reduction of the saponification extraction rate are avoided. Reflux reduces solvent loss.

In addition, the utility model also finds that after the saponification extraction reaction is finished, the temperature is reduced, and the material waste heat after the saponification and extraction reaction is recovered, so that the energy is saved, the solvent volatilization loss of the subsequent extracting solution in the filtering stage can be obviously reduced, the production cost is further reduced, and the operating environment and the safety are improved.

The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims

1. An extraction tank is characterized by comprising a tank body, a stirring device, a flow baffle, a heat exchange system and a temperature control device; wherein the content of the first and second substances,

2. The extraction tank as claimed in claim 1, wherein the stirring device comprises a stirring shaft, one end of the stirring shaft is connected with a stirring motor, at least one stirring blade set is arranged at the upper part of the stirring shaft in the upper cylinder, and at least one stirring blade set is arranged at the lower part of the stirring shaft in the lower cylinder.

3. The extraction tank as claimed in claim 2, wherein the upper part of the stirring shaft in the upper cylinder is provided with a first blade set, a second blade set and a third blade set from top to bottom, and the lower part of the stirring shaft in the lower cylinder is provided with a fourth blade set and a fifth blade set.

4. The extraction tank as claimed in claim 3, wherein the blade sets comprise two symmetrical blade-shaped blades, and the blades of the two adjacent blade sets form an anti-symmetrical arrangement with the central axis of the stirring shaft.

5. The extraction tank as claimed in claim 1, wherein the plurality of baffles are arranged at circumferentially equally spaced angles along an inner wall of the upper body of the extraction tank.

6. The extraction tank as claimed in any one of claims 1 to 5, wherein the heat exchange system comprises a first common heat exchange network arranged on the inner wall of the extraction tank and/or the outer wall of the upper cylinder body, and a first independent heat exchange network arranged outside the extraction tank and communicated with the first common heat exchange network; the heat exchange system is used for heating or cooling the materials in the extraction tank.

7. The extraction tank as claimed in any one of claims 1 to 5, wherein the temperature control device comprises a temperature detection module, a temperature conversion module, a temperature program control module; the temperature detection module detects a material temperature signal in the extraction tank, the material temperature signal is transmitted to the temperature program control module through the temperature conversion module, the temperature program control module judges the temperature signal and outputs a temperature control signal according to a judgment result to drive the heat exchange system to act.

8. The extraction tank as claimed in any one of claims 1 to 5, wherein the top of the extraction tank is further provided with an exhaust port and a reflux port, the reflux port is provided with a reflux device for condensation and reflux of the solvent and/or the extractant, and the top end of the reflux device is provided with an exhaust device.

9. The extraction tank of claim 8, wherein the reflux device is a reflux condenser tube or a reflux condensing system comprising a gas phase pipeline, a plate heat exchanger and a liquid phase pipeline.