Refining device for medicinal ethyl oleate and use method therefor

Abstract

Disclosed in the present invention are a refining device for medicinal ethyl oleate and a use method therefor. The refining device comprises a preset negative pressure vacuum batching apparatus, a vacuum pump, a dynamically adjustable memory reaction kettle, a discharge three-way pipe, a plate-frame circulating filtration assembly, a bag-type filter, a preset negative pressure vacuum finished product storage tank, a second centrifugal pump, and a barrel-type cartridge filter. The preset negative pressure vacuum batching apparatus is in communication with the dynamically adjustable memory reaction kettle; the discharge three-way pipe is disposed at a lower end of the dynamically adjustable memory reaction kettle; an input end of the plate-frame circulating filtration assembly and an input end of the bag-type filter are respectively in communication with and arranged at the other two ends of the discharge three-way pipe; the preset negative pressure vacuum finished product storage tank is in communication with and arranged at an output end of the bag-type filter. The present invention pertains to the field of ethyl oleate production, and specifically provides a refining device for medicinal ethyl oleate and a use method therefor, which overcomes the inability of existing ethyl oleate refining devices to control the peroxide value physicochemical index of the product, and facilitates more uniform and thorough stirring and mixing of materials.

Description

[Corrected according to Rule 26 17.07.2024] A method for using a refining device for medicinal ethyl oleate TECHNICAL FIELD

[0001] The present application belongs to the field of ethyl oleate production, specifically refers to a kind of medicinal ethyl oleate refining device and its using method. BACKGROUND

[0002] Ethyl oleate is a suitable solvent for steroids and other lipophilic drugs, its properties are similar to almond oil and peanut oil, however, compared with fatty oil, ethyl oleate has small viscosity and is easily absorbed by body components, and ethyl oleate can also be used as a solvent for subcutaneous injection drugs.

[0003] At present, the main refining method for ethyl oleate is to use conventional high vacuum distillation method or activated carbon decolorization to remove color, the maximum effect of the two conventional refining methods is to control the refining of ethyl oleate color and residue, but it cannot change the peroxide value of the product, and ethyl oleate needs to be replaced by ammonia gas during preparation to replace oxide to ensure the peroxide value of ethyl oleate, but the existing technology of ethyl oleate cannot ensure the maximum contact of ammonia gas and ethyl oleate, and it is difficult to solve the contradiction that ammonia gas should be gathered and dispersed to ensure the maximum contact area of liquid medicine and ammonia gas, and the contradiction that liquid medicine should be gathered and dispersed.

[0004] SUMMARY

[0005] To solve the above-mentioned existing problems, the present application provides a kind of pre-acting principle to the pre-vacuum negative pressure treatment of batching tank and finished product tank, so that there is no oxide in the batching tank and finished product tank, avoid ethyl oleate oxidation, introduce the same principle and self membrane principle, according to the asymmetric principle, pump a small amount of liquid ammonia through a plurality of misaligned holes of different sizes, form splashing liquid ammonia microbeads, the splashing and shaking of liquid ammonia in unstable state makes the mixing of liquid ammonia and ammonia gas more uniform, realizes the mixing of ammonia gas itself, solves the contradiction that ammonia gas and liquid medicine should be gathered and separated, through the self-mixing of liquid ammonia, the mixing mechanism and separation mechanism are cut off, there is no separation and mixing mechanism, but a better mixing effect is achieved, 360° all-round mixing is realized, the purity of liquid medicine is higher, the existing ethyl oleate refining device cannot control the peroxide value of the product, the rigid inactive object is changed into movable object with self-adaptability, elastic ball is added in the reaction kettle body, mechanical vibration is generated by using composite material, elastic ball rotates with stirring rod to continuously elastically adapt to material, so as to intensify the mixing of material, the mixing of material is more uniform and thorough, elastic memory spring is convenient for elastic ball to deform under heat, and the medicinal ethyl oleate refining device and its using method are convenient for elastic ball to take.

[0006] The technical scheme adopted by the present application is as follows: the present application is a refining device for medicinal ethyl oleate and a use method thereof, comprising a preset negative pressure vacuum batching device, a vacuum pump, a dynamic adjustment type memory reaction kettle, a discharge tee, a plate and frame circulating filter assembly, a bag filter, a preset negative pressure vacuum finished product storage tank, a second centrifugal pump and a barrel type filter core filter, the preset negative pressure vacuum batching device is arranged on one side of the dynamic adjustment type memory reaction kettle, the preset negative pressure vacuum batching device is communicated with the dynamic adjustment type memory reaction kettle, the discharge tee is arranged at the lower end of the dynamic adjustment type memory reaction kettle, the input ends of the plate and frame circulating filter assembly and the bag filter are respectively communicated with the other two ends of the discharge tee, the preset negative pressure vacuum finished product storage tank is communicated with the output end of the bag filter, the second centrifugal pump is arranged between the preset negative pressure vacuum finished product storage tank and the bag filter, the second centrifugal pump is convenient for pumping the material discharged from the dynamic adjustment type memory reaction kettle into the bag filter for filtration and then pumping to the preset negative pressure vacuum finished product storage tank, the input end of the barrel type filter core filter is communicated with the bottom wall of the preset negative pressure vacuum finished product storage tank, the vacuum pump is respectively communicated with the preset negative pressure vacuum finished product storage tank and the preset negative pressure vacuum batching device, the vacuum pump pumps out the air in the preset negative pressure vacuum batching device and the preset negative pressure vacuum finished product storage tank to make them in a vacuum state, so that the ethyl oleate is prevented from being oxidized by contacting with oxidants; the preset negative pressure vacuum batching device comprises a batching tank one, a batching tank two, a feeding tee, a feeding hose, a fixing block, an elastic rubber sleeve, a sealing air bag, an air inlet pipe, a one-way air inlet valve, a pressing air bag, a batching vacuum pipe and a batching vacuum valve, the upper wall of the dynamic adjustment type memory reaction kettle is communicated with a feeding port, the feeding tee is arranged in a Y shape, the lower end of the feeding tee is communicated with the feeding port, the batching tank one and the batching tank two are arranged above the dynamic adjustment type memory reaction kettle, the two ports of the upper end of the feeding tee are respectively communicated with the bottom wall of the batching tank one and the bottom wall of the batching tank two, a first discharging valve is arranged between the feeding tee and the batching tank one, a second discharging valve is arranged between the feeding tee and the batching tank two, the first discharging valve is convenient for controlling the communication between the feeding tee and the batching tank one, so as to control the discharging of the material in the batching tank one into the dynamic adjustment type memory reaction kettle, the second discharging valve is convenient for controlling the communication between the feeding tee and the batching tank two, so as to control the discharging of the material in the batching tank two into the dynamic adjustment type memory reaction kettle, the batching vacuum pipe is communicated between the air pumping end of the vacuum pump and the batching tank one, the batching vacuum valve is arranged on the batching vacuum pipe, the batching vacuum valve is convenient for controlling the communication of the batching vacuum pipe, so as to control the vacuum pumping treatment of the batching tank one by the vacuum pump, the feeding hose is communicated with the upper wall of the batching tank one, the feeding hose is provided with a first feeding valve, the fixing block is sleeved on the outer sidewall of the end of the feeding hose away from the batching tank one, the elastic rubber sleeve is fixedly connected to the fixing block, the elastic rubber sleeve is convenient for elastically sleeving and fixing the fixing block at the tank opening or bottle opening of the material tank, the elastically arranged elastic rubber sleeve is convenient for sealing the tank opening or bottle opening of the material tank,The sealing air bag is arranged in a ring shape, the sealing air bag is fixedly sleeved outside the feeding hose, the sealing air bag is arranged on the side of the fixing block far from the ingredient tank one, the air inlet pipe is arranged in communication on the side wall of the sealing air bag and penetrates the fixing block, the pressing air bag is arranged in communication on the end of the air inlet pipe far from the sealing air bag, the one-way air inlet valve is arranged on the air inlet pipe, the one-way air inlet valve ensures that the gas in the pressing air bag can only flow into the sealing air bag through the air inlet pipe, and the gas in the sealing air bag cannot flow back into the pressing air bag through the air inlet pipe, the side wall of the pressing air bag is provided with a one-way valve, the one-way valve facilitates air inlet of the pressing air bag, the side wall of the sealing air bag is provided with an air outlet pipe, the air outlet pipe penetrates the fixing block, the air outlet pipe is provided with an air outlet valve, the air outlet valve facilitates air outlet of the gas in the sealing air bag, the elastic rubber sleeve is elastically sleeved on the tank opening or bottle opening of the material tank, and the sealing air bag is placed at the tank opening or bottle opening, at this time, the elastic rubber sleeve preliminarily elastically seals the tank opening or bottle opening of the material tank, the pressing air bag is pressed, the gas in the pressing air bag is pressed into the sealing air bag, the sealing air bag is inflated to block the tank opening or bottle opening of the material tank, the one-way air inlet valve avoids backflow of the gas in the sealing air bag into the pressing air bag, the pressing air bag is inflated again by suction through the one-way valve to restore deformation, when the sealing air bag needs to be removed from the tank opening or bottle opening of the material tank, the air outlet valve is opened, so that the gas in the sealing air bag is discharged through the air outlet pipe, and then the sealing air bag and the elastic rubber sleeve can be removed, the sealing of the material tank during extraction of the material is facilitated, the possibility of oxidation of ethyl oleate due to entry of oxidants into the material tank is reduced, the vacuum pump draws the inside of the ingredient tank one into a vacuum negative pressure state through the ingredient vacuum pipe, and the oxidants in the ingredient tank one are drawn out, when the feeding hose is inserted into the material tank and the rubber protective sleeve and the sealing air bag seal the tank opening or bottle opening of the material tank, due to the pressure difference, the material in the material tank is automatically drawn into the ingredient tank one, and due to the negative pressure vacuum state in the ingredient tank one, oxidation of ethyl oleate is effectively avoided.

[0007] Further, the dynamic adjustment type memory reaction kettle comprises a reaction kettle body, a stirring motor, a stirring shaft, an insulated dynamic adjustment type elastic memory ball, a ball inlet pipe, a ball outlet pipe, a heat inlet pipe, a heat preservation reflux cavity and a heat outlet pipe. The reaction kettle body is a hollow cavity. The stirring motor is arranged on the upper wall of the reaction kettle body. The stirring shaft is rotatably arranged in the reaction kettle body. The output shaft of the stirring motor penetrates the upper wall of the reaction kettle body and is coaxially connected with the stirring shaft. The stirring shaft is provided with stirring blades. The stirring motor drives the stirring shaft to rotate. The stirring shaft drives the stirring blades to rotate to stir the materials in the reaction kettle body. The insulated dynamic adjustment type elastic memory ball is arranged in the reaction kettle body. The ball inlet pipe is communicated with the upper wall of the reaction kettle body. The ball outlet pipe is communicated with the lower wall of the reaction kettle body. The ball inlet pipe facilitates the placement of the insulated dynamic adjustment type elastic memory ball in the reaction kettle body. The ball outlet pipe facilitates the removal of the insulated dynamic adjustment type elastic memory ball from the reaction kettle body. The free end ports of the ball inlet pipe and the ball outlet pipe are respectively threadedly connected with sealing covers. The sealing covers facilitate the plugging of the free ends of the ball inlet pipe and the ball outlet pipe. The heat preservation reflux cavity is wrapped outside the reaction kettle body. The heat inlet pipe penetrates the heat preservation reflux cavity and is communicated with the reaction kettle body. The heat outlet pipe is communicated with the bottom wall of the heat preservation reflux cavity. The heat inlet pipe and the heat outlet pipe are externally connected with a heating device. The heating device generates hot gas which is sent into the reaction kettle body through the heat inlet pipe to heat the materials in the reaction kettle body. A transition pipe is arranged between the heat preservation reflux cavity and the reaction kettle body. The hot gas in the reaction kettle body is discharged into the heat preservation reflux pipe through the transition pipe to continuously heat the reaction kettle body and then is discharged through the heat outlet pipe, so that the pressure in the reaction kettle body is normal.

[0008] Further, the reaction kettle body is provided with a pressure sensor, a liquid level sensor and a temperature sensor. One side of the reaction kettle body is provided with a controller. The controller is electrically connected with the pressure sensor, the liquid level sensor and the temperature sensor.

[0009] Further, the insulated dynamic adjustment type elastic memory ball comprises a high-temperature-resistant rubber ball and shape memory alloy springs. The shape memory alloy springs are uniformly arranged on the surface of the high-temperature-resistant rubber ball. The shape memory alloy springs are elongated after being heated, so as to dynamically move in the reaction kettle body along with the rotation of the stirring shaft and the stirring blades. When the shape memory alloy springs collide with the reaction kettle body or the stirring shaft and the stirring blades, the mixing of the materials is intensified under the spring elastic force, so that the materials are more quickly and uniformly mixed together. The shaking degree of the insulated dynamic adjustment type elastic memory ball is dynamically adjusted according to the volume of the materials and the stirring speed of the stirring shaft. When the materials are discharged, the reaction kettle body is no longer heated to restore normal temperature. The shape memory alloy springs restore the deformation and shrink, so that the volume of the insulated dynamic adjustment type elastic memory ball is reduced. The insulated dynamic adjustment type elastic memory ball is conveniently discharged from the ball outlet pipe for cleaning. An insulating silica gel layer is wrapped outside the insulated dynamic adjustment type elastic memory ball, so as to effectively insulate and avoid the generation of sparks due to friction.

[0010] Further, the reactor body lower wall is provided with a discharge port, the plate and frame circulating filter assembly comprises a first centrifugal pump, a circulating liquid delivery pipe, a plate and frame filter and a backflow pipe, the discharge tee pipe is arranged in an inverted Y shape, the upper end of the discharge tee pipe is in communication with the discharge port, the input end of the first centrifugal pump and the input end of the bag filter are respectively in communication with two ports at the lower end of the discharge tee pipe, a liquid discharge valve is in communication between the discharge tee pipe and the bag filter, a circulating valve is in communication between the discharge tee pipe and the first centrifugal pump, the circulating liquid delivery pipe is in communication between the output end of the first centrifugal pump and the input end of the plate and frame filter, one end of the backflow pipe is in communication with the output end of the plate and frame filter, and the other end of the backflow pipe penetrates through the heat preservation backflow cavity and is in communication with the reactor body; when the circulating valve is turned on and the liquid discharge valve is closed, the first centrifugal pump pumps the liquid in the reactor body out and to the plate and frame filter through the circulating liquid delivery pipe for filtration, and the plate and frame filter returns the filtered liquid to the reactor body through the backflow pipe, so that the liquid is thoroughly filtered through multiple cycles of filtration.

[0011] Further, the preset negative pressure vacuum finished product storage tank is arranged in a hollow cavity, a finished product vacuum pipe is in communication between the preset negative pressure vacuum finished product storage pipe and the air suction end of the vacuum pump, a finished product vacuum valve is arranged on the finished product vacuum pipe, the finished product vacuum valve facilitates the on-off control of the finished product vacuum pipe, the preset negative pressure vacuum finished product storage tank is in communication with the barrel type filter element filter through a discharge pipe, a discharge valve is arranged on the discharge pipe, the discharge valve facilitates the discharge of the liquid in the preset negative pressure vacuum finished product storage tank, and the output end of the barrel type filter element filter is in communication with a filling pipe, so that the liquid can be filled.

[0012] Further, the second upper wall of the batching tank is in communication with a feed pipe, and the feed pipe is provided with a second feed valve.

[0013] Further, the reaction kettle body is provided with an asymmetric micro-splashing self-adaptive oxygen removal device, which comprises a liquid ammonia tank, a micro-flow pump, a liquid ammonia pump-in pipe, an inclined buffer cavity, a one-way valve shell, a micro-bead one-way valve and a micro-bead forming layer. The liquid ammonia tank and the micro-flow pump are arranged on one side of the reaction kettle body. The input end of the micro-flow pump is communicated with the liquid ammonia tank. The liquid ammonia pump-in pipe is communicated with the output end of the micro-flow pump. The one-way valve shell is arranged on the inner side wall of the reaction kettle body. The one-way valve shell is in a hemispherical shape. The micro-bead one-way valve is communicated with the side wall of the one-way valve shell. A plurality of micro-bead one-way valves with different sizes are arranged on the one-way valve shell. The micro-bead forming layer is wrapped outside the one-way valve shell. The micro-bead forming layer is in a hemispherical shape with the same center as the one-way valve shell. A one-way valve micro-bead generating cavity is arranged between the micro-bead forming layer and the one-way valve shell. The one-way valve micro-bead generating cavity facilitates the formation of micro-beads from the micro-bead one-way valve. A plurality of micro-bead holes with different sizes are arranged on the micro-bead forming layer. The inclined buffer cavity is communicated with one end of the liquid ammonia pump-in pipe away from the micro-flow pump. The other end of the inclined buffer cavity is communicated with the upper end of the one-way valve shell in an inclined manner. The asymmetrically arranged micro-bead holes and the micro-bead one-way valves correspond to each other, which facilitates the formation of micro-beads. The one-way valve shell is wrapped with a liquid ammonia cooling channel. The liquid ammonia cooling channel is communicated with the one-way valve shell through a through hole. The liquid ammonia cooling channel facilitates the low temperature of the one-way valve shell and the stable formation of micro-beads. The inclined buffer cavity facilitates the pumping of liquid ammonia from the upper end of the one-way valve shell. The micro-flow pump pumps the liquid ammonia in the liquid ammonia tank to the one-way valve shell through the micro-bead one-way valve. The liquid ammonia flowing out of the micro-bead one-way valve forms splashing micro-beads after passing through the asymmetrically arranged micro-bead one-way valves with different sizes. The splashing micro-beads flow out of the upper end of the micro-bead forming layer first. With the increase of the number of micro-beads, the micro-beads diffuse from the lower end of the micro-bead forming layer to the reaction kettle body under the action of gravity, forming unstable splashing and shaking, which makes the mixing more uniform. The melting point of ethyl oleate is -32℃, and the melting point of liquid ammonia is -33.5℃. Part of the liquid ammonia flowing into the reaction kettle body vaporizes, and the temperature decreases after absorbing heat, forming liquid ammonia micro-beads in a gas-liquid mixed state. The low temperature of liquid nitrogen can make ethyl oleate solidify instantly. Ethyl oleate is wrapped outside the liquid ammonia micro-beads, making the reaction more comprehensive and uniform. Through the principle of homogeneity and the mixing of liquid ammonia itself, the ethyl oleate and liquid ammonia are mixed uniformly in 360°, replacing the oxidant in the reaction kettle. This effectively solves the contradiction that ammonia gas needs to be gathered together to facilitate ammonia replacement of oxidants and needs to be separated to ensure that the contact area between ammonia gas and the liquid is uniform and maximized. It overcomes the technical difficulties of gathering and dispersing the liquid and mixing and dispersing the elastic ball. By cutting off the mixing mechanism and the separation mechanism from the device, the liquid and ammonia gas are better mixed and separated in the absence of a separation mechanism and a cutting mechanism. The micro-splashing self-adaptive oxygen removal device better controls the technical effect of the peroxide value of the product, making the purity of the liquid very high.

[0014] Further, the side walls of the first and second ingredient tanks are respectively provided with scales, which facilitate accurate reading of the liquid levels of the first and second ingredient tanks and accurate control of the material proportion; the dynamic adjustment type memory reaction kettle is provided with a support frame, and the first and second ingredient tanks are arranged on the support frame, which supports and fixes the first and second ingredient tanks.

[0015] A method for using a pharmaceutical ethyl oleate refining device, comprising the following steps:

[0016] 1) Vacuumizing: opening the ingredient vacuum valve and closing the product vacuum valve, the vacuum pump draws the first ingredient tank into a vacuum negative pressure state through the ingredient vacuum pipe, and the oxides in the first ingredient tank are drawn out, the ingredient vacuum valve is closed and the product vacuum valve is opened, and the vacuum pump draws the preset negative pressure vacuum product storage tank into a vacuum negative pressure state through the product vacuum pipe, and the oxides in the preset negative pressure vacuum product storage tank are drawn out;

[0017] 2) Activated carbon preparation: granular activated carbon is added to a NaOH solution with a concentration of 0.5 mol / L at a weight ratio of 0.1%, stirred at 100 rpm for 40 minutes at 50°C, and then filtered, washed with deionized water to pH 7 after water removal, and then modified activated carbon is obtained;

[0018] 3) Ingredient preparation: the elastic rubber sleeve is elastically sleeved at the bottle opening of the material tank, and the sealing air bag is placed at the tank opening or bottle opening, the gas in the pressing air bag is pressed into the sealing air bag by pressing the pressing air bag, the sealing air bag is inflated to seal the bottle opening of the material tank, the feeding valve one is opened, the feeding hose is inserted into the material tank, and the crude ethyl oleate in the material tank is pressed into the first ingredient tank under the action of pressure difference, the feeding valve two is opened, the modified activated carbon is sent into the second ingredient tank through the feeding pipe, and the ethyl oleate and modified activated carbon are weighed and prepared according to the feeding ratio;

[0019] 4) Discharging: closing the liquid discharge valve and the circulating valve, opening the first discharging valve to pour the crude ethyl oleate in the first ingredient tank into the reaction kettle body, waiting for the temperature in the reaction kettle body to drop to 70-80°C, opening the second discharging valve to pour the modified activated carbon in the second ingredient tank into the reaction kettle body, rotating the stirring shaft and stirring blade driven by the stirring motor and driving the insulated dynamic adjustment type elastic memory ball to stir, adsorb and decolorize for 30 minutes, closing the liquid discharge valve and opening the circulating valve, and controlling the first centrifugal pump to pump the reaction kettle body to the plate and frame filter for circulation filtration while hot;

[0020] 5) oxide replacement: when the liquid medicine is clear, close the circulating valve, raise its temperature to 140-150 DEG C, open the micro-flow pump to the reaction kettle body to micro-flow liquid ammonia, oxide replacement is completed, its temperature is cooled to below 45 DEG C, open the drain valve to filter through the bag filter to get the initial filtration filtrate;

[0021] 6) mixing: the initial filtration filtrate of step 5) is pumped into the pre-set negative pressure vacuum finished product storage tank with the second centrifugal pump for 30 min, and the initial product of the liquid medicine is obtained after passing the inspection;

[0022] 7) filling: opening the discharge valve, the initial product of the liquid medicine of step 6) is filtered through the barrel filter to be packaged in polyethylene barrels according to the specifications of 500g-10000g / barrel, and the ethyl oleate for medicine is obtained.

[0023] The beneficial effects obtained by the above structure are as follows: the ethyl oleate for medicine refining device and the use method thereof are designed reasonably, easy to operate, the pre-acting principle is used to pre-vacuum the material tank and the finished product tank, so that there is no oxide in the material tank and the finished product tank, avoiding the oxidation of ethyl oleate, the material tank and the finished product tank under negative pressure are convenient for the liquid medicine to be pressed in, the same principle and the mixing of liquid ammonia are used to mix the ethyl oleate and liquid ammonia in 360°, which is convenient for the oxide replacement in the reaction kettle, effectively solves the contradiction that ammonia gas should be gathered together to replace the oxide and separated to ensure that the contact area between ammonia gas and liquid medicine is uniform and maximized, overcomes the technical difficulties that the liquid medicine should be gathered and dispersed, and the elastic ball should be mixed and dispersed, the mixing mechanism and the separation mechanism are cut from the device, in the case of no separation mechanism and cutting mechanism, the liquid medicine and ammonia gas are better mixed and separated, the technical effect of self-adaptive oxygen removal is better realized, the technical effect of controlling the peroxide value of the product is realized, the purity of the liquid medicine is very high, the existing ethyl oleate refining device cannot control the peroxide value of the product, the principle of changing the rigid inactive object into movable object with self-adaptability is used, the insulated dynamic adjustment type elastic memory ball is added in the reaction kettle body, the insulated dynamic adjustment type elastic memory ball constantly shakes with the rotation of the stirring rod, so as to intensify the mixing of the material, so that the material mixing is more uniform and complete, the shape memory alloy spring is convenient for the insulated dynamic adjustment type elastic memory ball to be deformed by heat, and the insulated dynamic adjustment type elastic memory ball is convenient to take. BRIEF DESCRIPTION OF DRAWINGS

[0024] Fig. 1 is a schematic diagram of the ethyl oleate for medicine refining device structure;

[0025] Fig. 2 is a schematic diagram of the pre-set negative pressure vacuum material device structure of the ethyl oleate for medicine refining device;

[0026] Figure 3 is a partial enlarged view of part A of Figure 2;

[0027] Figure 4 is a schematic diagram of the internal structure of a dynamic adjustment type memory reactor of a refining device for ethyl oleate for pharmaceutical use according to the present application;

[0028] Figure 5 is a schematic diagram of an insulation dynamic adjustment type elastic memory ball structure of a refining device for ethyl oleate for pharmaceutical use according to the present application;

[0029] Figure 6 is a sectional view of an asymmetric micro-splashing type self-adaptive oxygen removal device of a refining device for ethyl oleate for pharmaceutical use according to the present application.

[0030] The accompanying drawings are included to provide a further understanding of the present application, and constitute a part of the specification, illustrate the present application together with the embodiments thereof, and explain the present application, but do not limit the present application. In the drawings: 1, preset negative pressure vacuum batching device, 2, vacuum pump, 3, dynamic adjustment type memory reactor, 4, discharge tee, 5, plate and frame circulation filter assembly, 6, bag filter, 7, preset negative pressure vacuum finished product storage tank, 8, second centrifugal pump, 9, barrel type filter element filter, 10, batching tank one, 11, batching tank two, 12, feed tee, 13, feed hose, 14, fixed block, 15, elastic rubber sleeve, 16, sealing air bag, 17, air inlet pipe, 18, one-way air inlet valve, 19, feed valve one, 20, pressing air bag, 21, batching vacuum pipe, 22, batching vacuum valve, 23, feed inlet, 24, discharge valve one, 25, support frame, 26, discharge valve two, 27, one-way valve, 28, exhaust pipe, 29, exhaust valve, 30, reactor body, 31, stirring motor, 32, stirring shaft, 33, insulation dynamic adjustment type elastic memory ball, 34, ball inlet pipe, 35, ball outlet pipe, 36, heat inlet pipe, 37, heat preservation reflux cavity, 38, heat outlet pipe, 39, stirring blade, 40, sealing cover, 41, transition pipe, 42, pressure sensor, 43, liquid level sensor, 44, temperature sensor, 45, controller, 46, high-temperature-resistant rubber ball, 47, shape memory alloy spring, 48, discharge outlet, 49, first centrifugal pump, 50, circulation liquid delivery pipe, 51, plate and frame filter, 52, reflux pipe, 53, liquid discharge valve, 54, circulation valve, 55, finished product vacuum pipe, 56, finished product vacuum valve, 57, discharge pipe, 58, discharge valve, 59, filling pipe, 60, feed pipe, 61, feed valve two, 62, micro-flow pump, 63, scale, 64, asymmetric micro-splashing type self-adaptive oxygen removal device, 65, liquid ammonia tank, 66, micro-bead hole, 67, liquid ammonia pump inlet pipe, 68, oblique buffer cavity, 69, one-way valve housing, 70, one-way valve, 71, liquid ammonia cooling channel, 72, micro-bead formation layer, 73, one-way valve micro-bead generation cavity. DETAILED DESCRIPTION

[0031] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments of the present application; based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative labor fall within the protection scope of the present application.

[0032] As shown in Figures 1-6, the present application for refining ethyl oleate and its use method, including a preset negative pressure vacuum batching device 1, a vacuum pump 2, a dynamic adjustment type memory reactor 3, a discharge tee 4, a plate and frame circulating filter assembly 5, a bag filter 6, a preset negative pressure vacuum finished product storage tank 7, a second centrifugal pump 8 and a barrel filter 9, the preset negative pressure vacuum batching device 1 is arranged on one side of the dynamic adjustment type memory reactor 3, the preset negative pressure vacuum batching device 1 is communicated with the dynamic adjustment type memory reactor 3, the discharge tee 4 is arranged at the lower end of the dynamic adjustment type memory reactor 3, the input ends of the plate and frame circulating filter assembly 5 and the bag filter 6 are respectively communicated with the other two ends of the discharge tee 4, the preset negative pressure vacuum finished product storage tank 7 is communicated with the output end of the bag filter 6, the second centrifugal pump 8 is arranged between the preset negative pressure vacuum finished product storage tank 7 and the bag filter 6, the input end of the barrel filter 9 is communicated with the bottom wall of the preset negative pressure vacuum finished product storage tank 7, the vacuum pump 2 is respectively communicated with the preset negative pressure vacuum finished product storage tank 7 and the preset negative pressure vacuum batching device 1; the preset negative pressure vacuum batching device 1 includes a batching tank one 10, a batching tank two 11, a feeding tee 12, a feeding hose 13, a fixed block 14, an elastic rubber sleeve 15, a sealing air bag 16, an air inlet pipe 17, a one-way air inlet valve 18, a pressing air bag 20, a batching vacuum pipe 21 and a batching vacuum valve 22, the upper wall of the dynamic adjustment type memory reactor 3 is communicated with a feeding port 23, the feeding tee 12 is arranged in Y shape, the lower end of the feeding tee 12 is communicated with the feeding port 23, the batching tank one 10 and the batching tank two 11 are arranged above the dynamic adjustment type memory reactor 3, two ports of the upper end of the feeding tee 12 are respectively communicated with the bottom wall of the batching tank one 10 and the bottom wall of the batching tank two 11, a first discharging valve 24 is arranged between the feeding tee 12 and the batching tank one 10, a second discharging valve 26 is arranged between the feeding tee 12 and the batching tank two 11, the batching vacuum pipe 21 is communicated between the air suction end of the vacuum pump 2 and the batching tank one 10, the batching vacuum valve 22 is arranged on the batching vacuum pipe 21, the feeding hose 13 is communicated with the upper wall of the batching tank one 10, a first feeding valve 19 is arranged on the feeding hose 13, the fixed block 14 is sleeved on the outer sidewall of the end of the feeding hose 13 away from the batching tank one 10, the elastic rubber sleeve 15 is fixedly connected to the fixed block 14, the sealing air bag 16 is arranged in a ring shape, the sealing air bag 16 is fixedly sleeved on the outer side of the feeding hose 13, the sealing air bag 16 is arranged on the side of the fixed block 14 away from the batching tank one 10, the air inlet pipe 17 penetrates through the fixed block 14 and is communicated with the sidewall of the sealing air bag 16, the pressing air bag 20 is communicated with the end of the air inlet pipe 17 away from the sealing air bag 16, the one-way air inlet valve 18 is arranged on the air inlet pipe 17, the sidewall of the pressing air bag 20 is provided with a one-way valve 27, the sidewall of the sealing air bag 16 is provided with an exhaust pipe 28, the exhaust pipe 28 penetrates through the fixed block 14, and the exhaust pipe 28 is provided with an exhaust valve 29.

[0033] The dynamic adjustment type memory reactor 3 comprises a reactor body 30, a stirring motor 31, a stirring shaft 32, an insulated dynamic adjustment type elastic memory ball 33, an inlet ball pipe 34, an outlet ball pipe 35, an inlet heat pipe 36, a heat preservation reflux cavity 37 and an outlet heat pipe 38. The reactor body 30 is a hollow cavity. The stirring motor 31 is arranged on the upper wall of the reactor body 30. The stirring shaft 32 is rotatably arranged in the reactor body 30. The output shaft of the stirring motor 31 penetrates the upper wall of the reactor body 30 and is coaxially connected with the stirring shaft 32. The stirring shaft 32 is provided with stirring blades 39. The insulated dynamic adjustment type elastic memory ball 33 is arranged in the reactor body 30. The inlet ball pipe 34 is communicated with the upper wall of the reactor body 30. The outlet ball pipe 35 is communicated with the lower wall of the reactor body 30. The free end ports of the inlet ball pipe 34 and the outlet ball pipe 35 are respectively threadedly connected with sealing covers 40. The heat preservation reflux cavity 37 is wrapped outside the reactor body 30. The inlet heat pipe 36 penetrates the heat preservation reflux cavity 37 and is communicated with the reactor body 30. The outlet heat pipe 38 is communicated with the bottom wall of the heat preservation reflux cavity 37. The inlet heat pipe 36 and the outlet heat pipe 38 are connected with a heating device. The heat preservation reflux cavity 37 and the reactor body 30 are communicated with a transition pipe 41.

[0034] The reactor body 30 is provided with a pressure sensor 42, a liquid level sensor 43 and a temperature sensor 44. One side of the reactor body 30 is provided with a controller 45. The controller 45 is electrically connected with the pressure sensor 42, the liquid level sensor 43 and the temperature sensor 44.

[0035] The insulated dynamic adjustment type elastic memory ball 33 comprises a high-temperature-resistant rubber ball 46 and shape memory alloy springs 47. The shape memory alloy springs 47 are uniformly arranged on the surface of the high-temperature-resistant rubber ball 46.

[0036] The lower wall of the reactor body 30 is provided with a discharge port 48. The plate and frame circulating filtration assembly 5 comprises a first centrifugal pump 49, a circulating liquid conveying pipe 50, a plate and frame filter 51 and a reflux pipe 52. The discharge tee pipe 4 is arranged in an inverted Y shape. The upper end of the discharge tee pipe 4 is communicated with the discharge port 48. The input end of the first centrifugal pump 49 and the input end of the bag filter 6 are respectively communicated with two ports of the lower end of the discharge tee pipe 4. The discharge tee pipe 4 and the bag filter 6 are communicated with a liquid discharge valve 53. The discharge tee pipe 4 and the first centrifugal pump 49 are communicated with a circulating valve 54. The circulating liquid conveying pipe 50 is communicated between the output end of the first centrifugal pump 49 and the input end of the plate and frame filter 51. One end of the reflux pipe 52 is communicated with the output end of the plate and frame filter 51. The other end of the reflux pipe 52 penetrates the heat preservation reflux cavity 37 and is communicated with the reactor body 30.

[0037] The preset negative pressure vacuum finished product storage tank 7 is provided as a hollow cavity, a finished product vacuum pipe 55 is arranged in communication between the preset negative pressure vacuum finished product storage pipe and the air suction end of the vacuum pump 2, a finished product vacuum valve 56 is arranged on the finished product vacuum pipe 55, a discharge pipe 57 is arranged in communication between the preset negative pressure vacuum finished product storage tank 7 and the barrel type filter core filter 9, a discharge valve 58 is arranged on the discharge pipe 57, and a filling pipe 59 is arranged in communication at the output end of the barrel type filter core filter 9.

[0038] A feeding pipe 60 is arranged in communication on the upper wall of the ingredient tank two 11, and a second feeding valve 61 is arranged on the feeding pipe 60.

[0039] The reaction kettle body 30 is provided with an asymmetric micro-splashing self-adaptive deoxidizing device 64, which includes a liquid ammonia tank 65, a micro-flow pump 62, a liquid ammonia pump-in pipe 67, an inclined buffer cavity 68, a one-way valve housing 69, a micro-bead one-way valve 70 and a micro-bead forming layer 72. The liquid ammonia tank 65 and the micro-flow pump 62 are arranged on one side of the reaction kettle body 30, the input end of the micro-flow pump 62 is in communication with the liquid ammonia tank 65, the liquid ammonia pump-in pipe 67 is arranged in communication at the output end of the micro-flow pump 62, the one-way valve housing 69 is arranged on the inner side wall of the reaction kettle body 30, the one-way valve housing 69 is provided in a hemispherical shape, the micro-bead one-way valve 70 is arranged in communication on the side wall of the one-way valve housing 69, a plurality of groups of micro-bead one-way valves 70 of different sizes are arranged in a staggered manner on the one-way valve housing 69, the micro-bead forming layer 72 is arranged in a wrapped manner on the outer side of the one-way valve housing 69, the micro-bead forming layer 72 is provided in a hemispherical shape with the same spherical center as the one-way valve housing 69, a one-way valve micro-bead generating cavity 73 is arranged between the micro-bead forming layer 72 and the one-way valve housing 69, a plurality of groups of micro-bead holes 66 of different sizes are arranged in a staggered manner on the micro-bead forming layer 72, the inclined buffer cavity 68 is arranged in communication at the end of the liquid ammonia pump-in pipe 67 away from the micro-flow pump 62, the other end of the inclined buffer cavity 68 is in communication with the upper end of the one-way valve housing 69 in an inclined manner, and a liquid ammonia cooling channel 71 is arranged in a wrapped manner on the outer wall of the one-way valve housing 69.

[0040] The side walls of the ingredient tank one 10 and the ingredient tank two 11 are respectively provided with a scale 63, the side wall of the dynamic adjustment type memory reaction kettle 3 is provided with a support frame 25, and the ingredient tank one 10 and the ingredient tank two 11 are arranged on the support frame 25.

[0041] A method for using a device for refining oleic acid ethyl ester for pharmaceutical use, comprising the following steps:

[0042] 1) Vacuumizing: open the ingredient vacuum valve 22 and close the product vacuum valve 56, the vacuum pump 2 draws the inside of the ingredient tank 10 into a vacuum negative pressure state through the ingredient vacuum pipe 21, and the oxides in the ingredient tank 10 are drawn out, close the ingredient vacuum valve 22 and open the product vacuum valve 56, the vacuum pump 2 draws the inside of the preset negative pressure vacuum product storage tank 7 into a vacuum negative pressure state through the product vacuum pipe 55, and the oxides in the preset negative pressure vacuum product storage tank 7 are drawn out;

[0043] 2) Activated carbon preparation: granular activated carbon is added into a NaOH solution with a concentration of 0.5 mol / L at a weight ratio of 0.1%, stirred at 100 rpm for 40 minutes at 50°C, filtered, washed with deionized water to pH 7 after removing water, and then modified activated carbon is obtained;

[0044] 3) Ingredient preparation: the elastic rubber sleeve 15 is elastically sleeved at the bottle opening of the material tank, and the sealing air bag 16 is placed at the tank opening or bottle opening, the gas in the pressing air bag 20 is pressed into the sealing air bag 16 by pressing the pressing air bag 20, the sealing air bag 16 is inflated to seal the bottle opening of the material tank, the feeding hose 13 is inserted into the material tank, the feeding valve one 19 is opened, the crude ethyl oleate in the material tank is pressed into the ingredient tank one 10 under the action of pressure difference, the feeding valve two 61 is opened, the modified activated carbon is sent into the ingredient tank two 11 through the feeding pipe 60, and the ethyl oleate and the modified activated carbon are weighed and prepared according to the feeding ratio;

[0045] 4) Discharging: close the liquid discharge valve 53 and the circulating valve 54, open the discharging valve one 24 to pour the crude ethyl oleate in the ingredient tank one 10 into the reaction kettle body 30, wait for the temperature in the reaction kettle body 30 to drop to 70-80°C, open the discharging valve two 26 to pour the modified activated carbon in the ingredient tank two 11 into the reaction kettle body 30, the stirring motor 31 drives the stirring shaft 32 and the stirring blade 39 to rotate and drive the insulated dynamic adjustment type elastic memory ball 33 to stir and adsorb decolorization for 30 minutes, close the liquid discharge valve 53 and open the circulating valve 54, control the first centrifugal pump 49 to pump the liquid in the reaction kettle body 30 to the plate and frame filter 51 for circulation filtration while hot,

[0046] 5) Oxide replacement: when the liquid is clarified, close the circulating valve 54, raise the temperature of the liquid to 140-150°C, open the micro-flow pump 62 to introduce liquid ammonia at a low flow rate, and perform oxide replacement, after the oxide replacement is completed, cool the liquid to below 45°C, open the liquid discharge valve 53, filter the liquid through the bag filter 6 to obtain an initial filtration filtrate;

[0047] 6) Mixing: the initial filtration filtrate obtained in step 5) is pumped into the preset negative pressure vacuum product storage tank 7 under vacuum by the second centrifugal pump 8 for 30 minutes, and a liquid primary product is obtained after inspection;

[0048] 7) Filling: The pharmaceutical liquid primary product of step 6) is filtered through the bucket filter 9, and then packaged in a 500g-10000g / bucket specification to obtain the pharmaceutical ethyl oleate.

[0049] In use, the ingredient vacuum valve 22 is opened and the finished product vacuum valve 56 is closed, the vacuum pump 2 draws the inside of the ingredient tank 10 into a vacuum negative pressure state through the ingredient vacuum pipe 21, and the oxide in the ingredient tank 10 is drawn out. The ingredient vacuum valve 22 is closed and the finished product vacuum valve 56 is opened, and the inside of the preset negative pressure vacuum finished product storage tank 7 is drawn into a vacuum negative pressure state by the vacuum pump 2 through the finished product vacuum pipe 55, and the oxide in the preset negative pressure vacuum finished product storage tank 7 is drawn out. After the vacuum is drawn, the ingredient vacuum valve 22 is closed and the finished product vacuum valve 56 is closed, the heat inlet pipe 36 and the heat outlet pipe 38 are connected to the heating device, the heating device generates hot gas which is sent into the reaction kettle body 30 through the heat inlet pipe 36 to heat the material in the reaction kettle body 30. The hot gas in the reaction kettle body 30 is discharged into the heat preservation reflux pipe 52 through the transition pipe 41 to continuously heat the reaction kettle body 30 and then discharged through the heat outlet pipe 38, ensuring that the pressure in the reaction kettle body 30 is normal. The elastic rubber sleeve 15 is elastically sleeved on the bottle opening of the material tank, and the sealing air bag 16 is placed at the tank opening or bottle opening. The pressing air bag 20 is pressed to press the gas in the pressing air bag 20 into the sealing air bag 16, and the sealing air bag 16 is inflated to seal the bottle opening of the material tank. The one-way air inlet valve 18 ensures that the gas in the pressing air bag 20 can only flow into the sealing air bag 16 through the air inlet pipe 17, and the gas in the sealing air bag 16 cannot flow back to the pressing air bag 20 from the air inlet pipe 17. The pressing air bag 20 is inflated again by drawing air through the one-way valve 27 to restore the deformation. The feeding valve 19 is opened, the feeding hose 13 is inserted into the material tank, and the crude ethyl oleate in the material tank is pressed into the ingredient tank 10 under the action of the pressure difference. When the sealing air bag 16 needs to be removed from the tank opening or bottle opening of the material tank, the exhaust valve 29 is opened to discharge the gas in the sealing air bag 16 through the exhaust pipe 28, and then the sealing air bag 16 and the elastic rubber sleeve 15 can be removed. This ensures the sealing of the material tank when the material is extracted, reduces the possibility of oxide entering the material tank to oxidize the ethyl oleate, opens the feeding valve 61, and sends the modified activated carbon into the ingredient tank 11 through the feeding pipe 60. The ethyl oleate and the modified activated carbon are weighed and mixed according to the mixing ratio. The liquid discharge valve 53 and the circulating valve 54 are closed, the crude ethyl oleate in the ingredient tank 10 is poured into the reaction kettle body 30 through the discharge valve 24, and when the temperature in the reaction kettle body 30 drops to 70-80℃, the modified activated carbon in the ingredient tank 11 is poured into the reaction kettle body 30 through the discharge valve 26. After the material is poured, the discharge valve 24 and the discharge valve 26 are closed. The stirring motor 31 drives the stirring shaft 32 and the stirring blade 39 to rotate and drive the insulated dynamic adjustment type elastic memory ball 33 to stir and absorb decolorization for 30 minutes. The shape memory alloy spring 47 becomes longer after being heated, which facilitates dynamic movement in the reaction kettle body 30 with the rotation of the stirring shaft 32 and the stirring blade 39. When the shape memory alloy spring 47 collides with the reaction kettle body 30 or the stirring shaft 32 and the stirring blade 39, the spring force is intensified to mix the materials, so that the materials are mixed more quickly and uniformly.The shaking degree of the insulating dynamic adjustment type elastic memory ball 33 is dynamically adjusted according to the volume of the material and the stirring speed of the stirring shaft 32. When the material is discharged, the reaction kettle body 30 is no longer heated to restore normal temperature, the shape memory alloy spring 47 restores the deformation shrinkage, so that the volume of the insulating dynamic adjustment type elastic memory ball 33 becomes smaller, the insulating dynamic adjustment type elastic memory ball 33 is conveniently discharged from the ball discharge pipe 35 for cleaning, the liquid discharge valve 53 is closed and the circulating valve 54 is opened, the first centrifugal pump 49 is used to control the hot control to discharge the liquid medicine in the reaction kettle body 30 through the discharge tee pipe 4 and then send it into the plate and frame filter 51 through the circulating liquid pipe 50, and then return it to the reaction kettle body 30 through the backflow pipe 52, the first centrifugal pump 49 repeatedly circulates and filters the liquid medicine in the reaction kettle body 30 through the plate and frame filter 51, when the liquid medicine is clarified, the circulating valve 54 is closed, the temperature is increased to 140-150℃, the micro-flow pump 62 is opened to micro-flow into liquid ammonia into the reaction kettle body 30, and oxide replacement is carried out, the inclined buffer cavity 68 pumps the liquid ammonia out from the upper end of the one-way valve shell 69, the micro-flow pump 62 pumps the liquid ammonia in the liquid ammonia tank 65 out to the one-way valve shell 69, and then flows out through the micro-bead one-way valve 70, the liquid ammonia flowing out from the micro-bead one-way valve 70 forms a splashing type micro-bead after passing through the asymmetrically positioned micro-bead one-way valves 70 with different sizes, the splashing type micro-bead first flows out from the upper end of the micro-bead forming layer 72, and as the number of micro-beads increases, the micro-beads diffuse from the lower end of the micro-bead forming layer 72 to the reaction kettle body 30 under the action of gravity to form unstable splashing and shaking, so that the mixing is more complete and uniform, a part of the liquid ammonia flowing into the reaction kettle body 30 is gasified, the temperature is lowered after heat absorption, and a gas-liquid mixed state of liquid ammonia micro-bead is formed, the low temperature of the liquid nitrogen can make the ethyl oleate solidify instantaneously, the ethyl oleate is wrapped outside the liquid ammonia micro-bead, the reaction is more complete and uniform, and through the homogeneous principle and the mixing of the liquid ammonia itself, the ethyl oleate and the liquid ammonia are mixed and replaced in 360° full range to replace the oxides in the reaction kettle body 30, effectively solving the contradiction that the ammonia gas needs to be gathered together to facilitate ammonia replacement of oxides and needs to be separated to ensure that the contact area between the ammonia gas and the liquid medicine is uniform and maximized, overcoming the technical difficulties that the liquid medicine needs to be gathered and dispersed and the insulating dynamic adjustment type elastic memory ball 33 needs to be mixed and dispersed, cutting off the mixing mechanism and the separation mechanism from the device, and in the case of no separation mechanism and cutting mechanism, the liquid medicine and the ammonia gas are better mixed and separated, and the technical effect of self-mixing and separation is achieved, the micro-splashing type self-adaptive deoxidization better realizes the technical effect of controlling the peroxide value of the product, the purity of the liquid medicine is very high, after the oxide replacement is completed, the discharge valve two 26 and the ammonia pump 62 are closed, the temperature of the liquid medicine in the reaction kettle body 30 is cooled to below 45℃, the liquid discharge valve 53 is opened, the liquid medicine is filtered through the bag filter 6 to obtain the primary filtered filtrate, the primary filtered filtrate is pumped into the pre-set negative pressure vacuum finished product storage tank 7 by the second centrifugal pump 8 for mixing for 30 min, and the liquid medicine primary product is obtained after inspection, when filling is needed, the discharge valve 58 is opened,The initial product of the liquid medicine in the preset negative pressure vacuum finished product storage tank 7 flows to the barrel filter 9 through the discharge pipe 57, is filtered, and is discharged through the filling pipe 59 to be filled.

[0050] It should be noted that the relational terms herein, such as first and second, and the like, are used solely to distinguish one from another entity or action without necessarily requiring or implying any actual relationship or order between such entities or actions. Moreover, the terms "comprises", "comprising", or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but can also include other elements not expressly listed or inherent to such process, method, article, or apparatus.

[0051] While embodiments of the application have been shown and described, it is to be understood that the application is not limited to the details of the embodiments described, since numerous modifications, changes, substitutions, and equivalents will occur to those skilled in the art without departing from the spirit and scope of the present application, which is defined by the following claims and their equivalents.

Claims

1. An apparatus for refining ethyl oleate for pharmaceutical use, characterized by: The utility model provides a kind of negative pressure vacuum batching device, vacuum pump, dynamic adjustment type memory reaction kettle, discharge tee, plate frame circulating filter component, bag filter, preset negative pressure vacuum finished product storage tank, second centrifugal pump and bucket filter, the preset negative pressure vacuum batching device is located dynamic adjustment type memory reaction kettle side, preset negative pressure vacuum batching device is communicated with dynamic adjustment type memory reaction kettle, the discharge tee is located the lower end of dynamic adjustment type memory reaction kettle, the input end of plate frame circulating filter component and bag filter is respectively communicated and located the other two ends of discharge tee, the preset negative pressure vacuum finished product storage tank is communicated and located the output end of bag filter, the second centrifugal pump is located between preset negative pressure vacuum finished product storage tank and bag filter, the input end of bucket filter is communicated and located the bottom wall of preset negative pressure vacuum finished product storage tank, the vacuum pump is communicated with preset negative pressure vacuum finished product storage tank, preset negative pressure vacuum batching device respectively;The preset negative pressure vacuum batching device includes batching tank one, batching tank two, feed tee, feed hose, fixed block, elastic rubber sleeve, sealing air bag, air inlet pipe, one-way air inlet valve, pressing air bag, batching vacuum pipe and batching vacuum valve, the upper wall of dynamic adjustment type memory reaction kettle is communicated and located feed inlet, the feed tee is arranged in Y shape, the lower end of feed tee is communicated and located feed inlet, batching tank one and batching tank two are located above dynamic adjustment type memory reaction kettle, the two ports of feed tee upper end are communicated with the bottom wall of batching tank one and the bottom wall of batching tank two respectively, one-way valve one is arranged between feed tee and batching tank one, one-way valve two is arranged between feed tee and batching tank two, the batching vacuum pipe is communicated between the air extraction end of vacuum pump and batching tank one, the batching vacuum valve is arranged on batching vacuum pipe, the feed hose is communicated on the upper wall of batching tank one, and one-way valve one is arranged on the feed hose, the fixed block is sleeved on the outer wall of the end of feed hose away from batching tank one, the elastic rubber sleeve is fixedly connected on the fixed block, the sealing air bag is arranged in ring shape, the sealing air bag is fixedly sleeved on the outer side of feed hose, and the sealing air bag is located on the side of fixed block away from batching tank one, the air inlet pipe is communicated on the side wall of sealing air bag, the pressing air bag is communicated on the end of air inlet pipe away from sealing air bag, the one-way air inlet valve is arranged on air inlet pipe, one-way valve is arranged on the side wall of pressing air bag, the side wall of sealing air bag is provided with air outlet pipe, air outlet pipe penetrates fixed block, and air outlet valve is arranged on air outlet pipe.

2. A device for refining ethyl oleate for pharmaceutical use according to claim 1, characterized in that: The dynamic adjustment type memory reaction kettle comprises a reaction kettle body, a stirring motor, a stirring shaft, an insulating dynamic adjustment type elastic memory ball, a ball inlet pipe, a ball outlet pipe, a heat inlet pipe, a heat preservation reflux cavity and a heat outlet pipe, the reaction kettle body is a hollow cavity, the stirring motor is arranged on the upper wall of the reaction kettle body, the stirring shaft is rotatably arranged in the reaction kettle body, the output shaft of the stirring motor is coaxially connected with the stirring shaft through the upper wall of the reaction kettle body, stirring blades are arranged on the stirring shaft, the insulating dynamic adjustment type elastic memory ball is arranged in the reaction kettle body, the ball inlet pipe is communicated and arranged on the upper wall of the reaction kettle body, the ball outlet pipe is communicated and arranged on the lower wall of the reaction kettle body, the free end ports of the ball inlet pipe and the ball outlet pipe are respectively threadedly connected with sealing covers, the heat preservation reflux cavity is wrapped outside the reaction kettle body, the heat inlet pipe is communicated through the heat preservation reflux cavity and the reaction kettle body, the heat outlet pipe is communicated and arranged on the bottom wall of the heat preservation reflux cavity, and the transition pipe is arranged between the heat preservation reflux cavity and the reaction kettle body.

3. A device for refining ethyl oleate for pharmaceutical use according to claim 2, characterized in that: The pressure sensor, the liquid level sensor and the temperature sensor are arranged in the reaction kettle body, and the controller is arranged on one side of the reaction kettle body and electrically connected with the pressure sensor, the liquid level sensor and the temperature sensor.

4. A device for refining ethyl oleate for pharmaceutical use according to claim 2, characterized in that: The insulating dynamic adjustment type elastic memory ball comprises a high-temperature-resistant rubber ball and shape memory alloy springs, and the shape memory alloy springs are uniformly arranged on the surface of the high-temperature-resistant rubber ball.

5. A device for refining ethyl oleate for pharmaceutical use according to claim 2, characterized in that: The lower wall of the reaction kettle body is provided with a discharge port, the plate and frame circulating filter assembly comprises a first centrifugal pump, a circulating liquid conveying pipe, a plate and frame filter and a reflux pipe, the discharge tee pipe is arranged in an inverted Y shape, the upper end of the discharge tee pipe is communicated and arranged at the discharge port, the input end of the first centrifugal pump and the input end of the bag type filter are respectively communicated and arranged on two ports of the lower end of the discharge tee pipe, the discharge tee pipe and the bag type filter are communicated through the liquid discharge valve, the discharge tee pipe and the first centrifugal pump are communicated through the circulating valve, the circulating liquid conveying pipe is communicated between the output end of the first centrifugal pump and the input end of the plate and frame filter, one end of the reflux pipe is communicated with the output end of the plate and frame filter, and the other end of the reflux pipe penetrates through the heat preservation reflux cavity and is communicated with the reaction kettle body.

6. A device for refining ethyl oleate for pharmaceutical use according to claim 1, characterized in that: The preset negative pressure vacuum finished product storage tank is arranged in a hollow cavity, the finished product vacuum pipe is communicated between the preset negative pressure vacuum finished product storage pipe and the air suction end of the vacuum pump, the finished product vacuum valve is arranged on the finished product vacuum pipe, the discharge pipe is communicated between the preset negative pressure vacuum finished product storage tank and the barrel type filter element filter, the discharge valve is arranged on the discharge pipe, and the filling pipe is communicated with the output end of the barrel type filter element filter.

7. A device for refining ethyl oleate for pharmaceutical use according to claim 1, characterized in that: The second feeding pipe is communicated with the second upper wall of the feeding tank, and the second feeding valve is arranged on the second feeding pipe.

8. A device for refining ethyl oleate for pharmaceutical use according to claim 2, characterized in that: The asymmetric micro-splashing self-adaptive oxygen removal device is arranged on the reactor body, and comprises a liquid ammonia tank, a micro-flow pump, a liquid ammonia pump-in pipe, an inclined buffer cavity, a one-way valve shell, a one-way valve, a liquid ammonia cooling channel and a micro-bead forming layer.

9. A device for refining ethyl oleate for pharmaceutical use according to claim 1, characterized in that: The side walls of the first and second ingredient tanks are respectively provided with scale rulers; the side wall of the dynamic adjustment type memory reactor is provided with a support frame, and the first and second ingredient tanks are arranged on the support frame.

10. A method of using a pharmaceutical oleic acid ethyl ester refining device, comprising the following steps: 1) Vacuumizing: opening the ingredient vacuum valve and closing the finished product vacuum valve, the vacuum pump draws the inside of the first ingredient tank into a vacuum negative pressure state through the ingredient vacuum pipe, and the oxides in the first ingredient tank are drawn out, the ingredient vacuum valve is closed and the finished product vacuum valve is opened, the vacuum pump draws the inside of the preset negative pressure vacuum finished product storage tank into a vacuum negative pressure state through the finished product vacuum pipe, and the oxides in the preset negative pressure vacuum finished product storage tank are drawn out; 3) Ingredient: the elastic rubber sleeve is elastically sleeved at the bottle opening of the material tank, and the sealing air bag is placed at the tank opening or bottle opening, the gas in the pressing air bag is pressed into the sealing air bag by pressing the pressing air bag, the sealing air bag is inflated to seal the bottle opening of the material tank, the inlet valve one is opened, the inlet hose is inserted into the material tank, the crude oleic acid ethyl ester in the material tank is pressed into the first ingredient tank under the action of pressure difference, the inlet valve two is opened, the modified activated carbon is sent into the second ingredient tank through the feeding pipe, and the oleic acid ethyl ester and the modified activated carbon are weighed and mixed according to the feeding ratio; 4) Discharging: closing the liquid discharge valve and the circulating valve, opening the first discharging valve, and putting the crude oleic acid ethyl ester in the first ingredient tank into the reactor body, ​ The modified activated carbon in the second ingredient tank is put into the reaction kettle body, the stirring motor drives the stirring shaft and stirring blade to rotate and drives the insulating dynamic adjustment type elastic memory ball to stir and adsorb decolorization for 30 minutes, the drain valve is closed and the circulating valve is opened, the first centrifugal pump is controlled to draw the liquid in the reaction kettle body to the plate and frame filter for circulation filtration while hot, 5) Oxide replacement: when the liquid is clarified, the circulating valve is closed, the temperature is raised to 140-150℃, the micro-flow pump is opened to micro-flow into liquid ammonia in the reaction kettle body, oxide replacement is carried out, the temperature is cooled to below 45℃ after oxide replacement is completed, the drain valve is opened, the liquid is filtered through the bag filter to obtain the primary filtration filtrate; 6) Mixing: the primary filtration filtrate in step 5) is pumped into a vacuum pre-set negative pressure vacuum finished product storage tank by the second centrifugal pump for 30 minutes, and the pharmaceutical liquid primary product is obtained after inspection; 7) Filling: the pharmaceutical liquid primary product in step 6) is filtered through the barrel type filter cartridge filter, and then packaged in polyethylene barrels according to the specifications of 500g-10000g / barrel to obtain the pharmaceutical ethyl oleate.

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