CN111704958A - Method and device for refining medicinal ethyl oleate - Google Patents
Method and device for refining medicinal ethyl oleate Download PDFInfo
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- CN111704958A CN111704958A CN202010622798.9A CN202010622798A CN111704958A CN 111704958 A CN111704958 A CN 111704958A CN 202010622798 A CN202010622798 A CN 202010622798A CN 111704958 A CN111704958 A CN 111704958A
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- ethyl oleate
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/02—Refining fats or fatty oils by chemical reaction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
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- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method and a device for refining medicinal ethyl oleate, wherein a refining device for medicinal ethyl oleate is adopted to refine the medicinal ethyl oleate to obtain a high-purity medicinal ethyl oleate product, and the production method comprises the following steps: preparing materials, feeding materials, adsorbing and concentrating, mixing and filling; a refining device for medicinal ethyl oleate comprises a stainless steel reaction kettle, a plate-frame filter, a bag filter, a barrel-type filter element filter and a stainless steel storage tank. The process is connected together, continuous production can be realized, the working efficiency is high, and the method can be matched with the method for refining the medicinal ethyl oleate to refine the medicinal ethyl oleate to obtain a high-purity medicinal ethyl oleate product.
Description
Technical Field
The invention relates to the field of production of ethyl oleate, and particularly relates to a method and a device for refining medicinal ethyl oleate.
Background
Ethyl oleate is a suitable solvent for steroids and other lipophilic drugs, and has properties similar to almond oil and peanut oil, however, ethyl oleate is less viscous and is readily absorbed by body components than fatty oils, and ethyl oleate is also used as a solvent for drugs for subcutaneous injection.
At present, a conventional high vacuum distillation method or a refining method for decoloring and removing color by activated carbon is mainly adopted for a refining method of ethyl oleate, and the two conventional refining methods have the greatest effect of refining and controlling the color and residue of the ethyl oleate, but cannot change the physicochemical index of the peroxide value of a product.
Disclosure of Invention
The invention aims to provide a method and a device for refining medicinal ethyl oleate.
The invention is realized by the following technical scheme.
A refining method of medicinal ethyl oleate comprises the following steps: preparing materials, feeding materials, adsorbing and concentrating, mixing and filling;
step A, batching: weighing and mixing ethyl oleate and active carbon according to the feeding proportion;
step B, feeding: adding 1000Kg of ethyl oleate into a reaction kettle;
step C, adsorption concentration: adding 0.1% of activated carbon, cooling to 70-80 ℃, stirring, adsorbing and decoloring for 30 minutes, circularly filtering with a plate frame while the solution is hot, cooling the solution to below 45 ℃ after the solution is clarified, and filtering by a bag filter;
step D, mixing: pumping the filtrate into a stainless steel storage tank by a pump, mixing for 30min, inspecting, fine filtering, and packaging;
step E, filling: packing the feed liquid with a polyethylene barrel according to the specification of 20 Kg/barrel;
the adsorption concentration comprises the following steps: after the liquid medicine is clarified, the temperature is raised to 140-150 ℃, nitrogen is introduced for oxide replacement, a vacuum valve is opened, the vacuum degree is adjusted to-0.03 pa, pressure is reduced for replacement for 2 hours, the temperature is cooled to below 45 ℃, and bag filtration is carried out.
The further technical scheme is that the mixture ratio of the materials in the step A is ethyl oleate: activated carbon 100: 0.1.
the further technical proposal is that the adsorption stirring speed in the step c is 30-60 r/min, and the nitrogen replaces the stirring speed in the adsorption concentration to be 30-60 r/min.
A refining device for medicinal ethyl oleate comprises a stainless steel reaction kettle, a plate frame filter, a bag filter, a barrel type filter element filter and a stainless steel storage tank, wherein a discharge port at the lower end of the stainless steel reaction kettle is connected with a conveying pipeline with a first control valve and a first centrifugal pump through a tee joint, the rear end of the conveying pipeline is communicated with the plate frame filter, a liquid outlet of the plate frame filter is connected with a circulating material port at the upper end of the stainless steel reaction kettle through a pipeline, a discharge port at the lower end of the stainless steel reaction kettle is connected with the bag filter through a tee joint and a pipeline with a second control valve, a discharge port of the bag filter is connected with the stainless steel storage tank through a pipeline with a second centrifugal pump, a discharge port of the stainless steel storage tank is connected with the barrel type filter element filter, the stainless steel reaction kettle comprises a kettle body, a heat preservation cavity, and the side of the upper part of the heat preservation cavity is provided with a heating inlet of the communication, the bottom of the heat preservation cavity is provided with a heating outlet of the communication, the center of the bottom of the kettle body is provided with a discharge hole, the middle part of the top cover of the heat preservation cavity is provided with a stirring motor, the output port of the stirring motor is communicated with the stirring paddle blade arranged in the kettle body, the top cover of the kettle body on the left side of the stirring motor is provided with an observation hole, and the top cover of the kettle body on.
Preferably, all install the control valve on the pipeline that stainless steel reation kettle, stainless steel storage tank and the discharge gate of plate and frame filter lower extreme are connected to all install the control valve on the feed inlet of bag filter and the feed inlet of plate and frame filter.
Preferably, the stainless steel reaction kettle adopts a carbon steel jacket lining enamel reaction kettle, and the upper end of the stainless steel reaction kettle is provided with an observation hole made of transparent glass, a temperature sensor mounting hole, a feeding hole, a pressure sensor mounting hole, a liquid level meter mounting hole, a vacuum valve mounting hole and an air inlet.
Preferably, the heat preservation chamber shell in the stainless steel reation kettle outside evenly welds has four groups of supporting seats, and is connected with the circulation material mouth on the cauldron body of supporting seat top, and the heat preservation chamber that the stainless steel reation kettle outside set up simultaneously passes through heating export and heating import and heating device intercommunication to heat preservation intracavity portion heating medium is one of them of conduction oil and steam.
An application of a refining device of medicinal ethyl oleate in a refining method of medicinal ethyl oleate.
The high-purity medical-grade ethyl oleate product is obtained by refining the medical ethyl oleate by adopting a refining device of the medical ethyl oleate.
According to the technical scheme, the beneficial effects of the invention are as follows:
the refining device of the medicinal ethyl oleate is suitable for refining the medicinal ethyl oleate, the processes are connected together, continuous production can be realized, the working efficiency is high, the refining method of the medicinal ethyl oleate can be matched for refining the medicinal ethyl oleate to obtain a high-purity medicinal ethyl oleate product, the refining method of the medicinal ethyl oleate fills nitrogen into a reaction tank, the nitrogen plays a role in replacing oxides, the quality and the purity of the ethyl oleate product can be greatly improved, the obtained product is low in peroxide value and light in color, meets the medicinal requirements, and has remarkable economic benefits.
Drawings
FIG. 1 is a schematic diagram of a refining apparatus for medicinal ethyl oleate;
FIG. 2 is a structural diagram of a stainless steel reaction vessel of a refining device for medicinal ethyl oleate;
FIG. 3 is a plan view of a stainless steel reaction vessel of a refining apparatus for medicinal ethyl oleate;
FIG. 4 is a schematic flow diagram of a method for refining medicinal ethyl oleate.
Reference numbers in the figures: 1. a stainless steel reaction kettle; 2. a plate frame filter; 3. a delivery conduit; 4. a first centrifugal pump; 5. a first control valve; 6. a second control valve; 7. a bag filter; 8. a barrel cartridge filter; 9. a stainless steel storage tank; 10. a second centrifugal pump; 11. a kettle body; 12. a heat preservation cavity; 13. heating the inlet; 14. a heating outlet; 15. a discharge port; 16. a stirring paddle; 17. a supporting seat; 18. an observation hole; 19. a stirring motor; 20. and (4) feeding a material inlet.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The conditions used in the examples may be further adjusted according to the manufacturer's conditions, and the unexplained conditions are generally conventional experimental conditions.
Examples
A refining method of medicinal ethyl oleate comprises the following steps: preparing materials, feeding materials, adsorbing and concentrating, mixing and filling;
step A, batching: weighing and mixing ethyl oleate and active carbon according to the feeding proportion;
step B, feeding: adding 1000Kg of ethyl oleate into a reaction kettle;
step C, adsorption concentration: adding 0.1% of activated carbon, cooling to 70-80 ℃, stirring, adsorbing and decoloring for 30 minutes, circularly filtering with a plate frame while the solution is hot, cooling the solution to below 45 ℃ after the solution is clarified, and filtering by a bag filter;
step D, mixing: pumping the filtrate into a stainless steel storage tank by a pump, mixing for 30min, inspecting, fine filtering, and packaging;
step E, filling: packing the feed liquid with a polyethylene barrel according to the specification of 20 Kg/barrel;
the adsorption concentration comprises the following steps: after the liquid medicine is clarified, the temperature is raised to 140-150 ℃, nitrogen is introduced for oxide replacement, a vacuum valve is opened, the vacuum degree is adjusted to-0.03 pa, pressure is reduced for replacement for 2 hours, the temperature is cooled to below 45 ℃, and bag filtration is carried out.
The further technical scheme is that the mixture ratio of the materials in the step A is ethyl oleate: activated carbon 100: 0.1.
the further technical proposal is that the adsorption stirring speed in the step c is 30-60 r/min, and the nitrogen replaces the stirring speed in the adsorption concentration to be 30-60 r/min.
As shown in fig. 1-4: a refining device for medicinal ethyl oleate comprises a stainless steel reaction kettle 1, a plate frame filter 2, a bag filter 7, a barrel type filter element filter 8 and a stainless steel storage tank 9, wherein a discharge port 15 at the lower end of the stainless steel reaction kettle 1 is connected with a conveying pipeline 3 with a first centrifugal pump 4 through a tee joint, the rear end of the conveying pipeline 3 is communicated with the plate frame filter 2, a liquid outlet of the plate frame filter 2 is connected with a circulating material port at the upper end of the stainless steel reaction kettle 1 through a pipeline, a discharge port 15 at the lower end of the stainless steel reaction kettle 1 is connected with the bag filter 7 through a tee joint, a discharge port of the bag filter 7 is connected with the stainless steel storage tank 9 through a pipeline with a second centrifugal pump 10, a discharge port of the stainless steel storage tank 9 is connected with the barrel type filter element filter 8, the stainless steel reaction kettle 1 comprises a kettle body 11, a heat preservation cavity 12, a stirring paddle, and the side of the upper part of the heat preservation cavity 12 is provided with a communicated heating inlet 13, the bottom of the heat preservation cavity 12 is provided with a communicated heating outlet 14, the center of the bottom of the kettle body 11 is provided with a discharge hole 15, the middle part of the top cover of the heat preservation cavity 12 is provided with a stirring motor 19, the output port of the stirring motor 19 is communicated with a stirring blade 16 arranged inside the kettle body 11, the top cover of the kettle body 11 on the left side of the stirring motor 19 is provided with an observation hole 18, and the top cover of the kettle body 11 on the right side of the stirring motor.
Control valves are respectively arranged on pipelines connected with the stainless steel reaction kettle 1, the stainless steel storage tank 9 and the discharge port at the lower end of the plate frame filter 2, and a feed port of the bag filter 7 and a feed port of the plate frame filter 2 are respectively provided with a control valve; the stainless steel reaction kettle 1 adopts a carbon steel jacket liner enamel reaction kettle, and the upper end of the stainless steel reaction kettle 1 is provided with an observation hole 18 made of transparent glass, a temperature sensor mounting hole, a feeding hole 20, a pressure sensor mounting hole, a liquid level meter mounting hole and a vacuum valve mounting hole; evenly welded has four groups of supporting seats 17 on the heat preservation chamber 12 shell in the stainless steel reation kettle 1 outside, and is connected with the circulation material mouth on the cauldron body 11 of supporting seat 17 top, the heat preservation chamber 12 that the stainless steel reation kettle 1 outside set up simultaneously is through heating export 14 and heating import 13 and heating device intercommunication, and heat preservation chamber 12 inside heating medium is one of them kind of conduction oil and steam, and install temperature sensor and temperature control device on heat preservation chamber 12, insert pressure sensor in heat preservation chamber 12 inside simultaneously.
A refining device of medicinal ethyl oleate is applied to a refining method of medicinal ethyl oleate, 1000Kg of ethyl oleate and 1Kg of medicinal active carbon are weighed by an electronic scale, 1000Kg of ethyl oleate is added into a kettle body 11 through a feed inlet 20, a heating inlet 13 and a heating outlet 14 which are arranged on the side surface of a heat preservation cavity 12 are connected with a heating device, the kettle body 11 is provided with a pressure sensor, a temperature sensor and other related devices, 10Kg of active carbon is added into the kettle body 11 through the heating outlet 14, the heating device heats a stainless steel reaction kettle 1, the internal temperature of the stainless steel reaction kettle 1 is kept between 70 and 80 ℃, a stirring motor 19 operates to drive a stirring paddle 16 to rotate to stir materials, half effect is stirred, a first control valve 5 is opened while hot, a second control valve 6 is closed, a first centrifugal pump 4 and a plate frame filter 2 operate, circulating and filtering the hot liquid medicine in the stainless steel reaction kettle 1 for half an hour, closing the first centrifugal pump 4 and the plate-frame filter 2 after the liquid medicine is clarified, and a first control valve 5, wherein the heating device raises the temperature inside the stainless steel reaction kettle 1 to 140-150 ℃, introducing nitrogen through an air inlet above the stainless steel reaction kettle 1 for oxide replacement, opening a vacuum valve arranged at the upper end of the stainless steel reaction kettle 1, adjusting the vacuum degree to-0.03 pa, decompressing and replacing for 2 hours, cooling to below 45 deg.C, opening second control valve 6 to filter the medicinal liquid via bag filter 7, delivering into stainless steel storage tank 9 via second centrifugal pump 10, installing stirring device on stainless steel storage tank 9, stirring and mixing for half an hour, after the product is qualified, the product is subjected to precision filtration and filling to obtain the high-purity medicinal ethyl oleate product.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art should understand that they can make various changes, modifications, additions and substitutions within the spirit and scope of the present invention.
Claims (8)
1. A refining method of medicinal ethyl oleate comprises the following steps: batching, throw material, adsorb concentrated, mix and the filling, its characterized in that:
step A, batching: weighing and mixing ethyl oleate and active carbon according to the feeding proportion;
step B, feeding: adding 1000Kg of ethyl oleate into a reaction kettle;
step C, adsorption concentration: adding 0.1% of activated carbon, cooling to 70-80 ℃, stirring, adsorbing and decoloring for 30 minutes, circularly filtering with a plate frame while the solution is hot, cooling the solution to below 45 ℃ after the solution is clarified, and filtering by a bag filter;
step D, mixing: pumping the filtrate into a stainless steel storage tank by a pump, mixing for 30min, inspecting, fine filtering, and packaging;
step E, filling: packing the feed liquid with a polyethylene barrel according to the specification of 20 Kg/barrel;
the adsorption concentration comprises the following steps: after the liquid medicine is clarified, the temperature is raised to 140-150 ℃, nitrogen is introduced for oxide replacement, a vacuum valve is opened, the vacuum degree is adjusted to-0.03 pa, pressure is reduced for replacement for 2 hours, the temperature is cooled to below 45 ℃, and bag filtration is carried out.
2. The refining method of medicinal ethyl oleate of claim 1, wherein the mixture ratio of materials in the step A is ethyl oleate: activated carbon 100: 0.1.
3. the method for refining ethyl oleate as claimed in claim 1, wherein the stirring speed in step c is 30-60 rpm under adsorption, and 30-60 rpm under nitrogen replacement in adsorption concentration.
4. A refining device for medicinal ethyl oleate comprises a stainless steel reaction kettle (1), a plate-frame filter (2), a bag filter (7), a barrel-type filter element filter (8) and a stainless steel storage tank (9), and is characterized in that a discharge port (15) at the lower end of the stainless steel reaction kettle (1) is connected with a conveying pipeline (3) with a first control valve (5) and a first centrifugal pump (4) through a tee joint, the rear end of the conveying pipeline (3) is communicated with the plate-frame filter (2), a liquid outlet of the plate-frame filter (2) is connected with a circulating material port at the upper end of the stainless steel reaction kettle (1) through a pipeline, a discharge port (15) at the lower end of the stainless steel reaction kettle (1) is connected with the bag filter (7) through a tee joint and a pipeline with a second control valve (6), and a discharge port of the bag filter (7) is connected with the stainless steel storage tank (9) through a pipeline with, a discharge port of the stainless steel storage tank (9) is connected with a barrel type filter element filter (8), the stainless steel reaction kettle (1) comprises a kettle body (11), a heat preservation cavity (12), a stirring paddle (16) and a stirring motor (19), the heat preservation cavity (12) is arranged on the outer side of the kettle body (11), and the side surface above the heat preservation cavity (12) is provided with a communicated heating inlet (13), a communicated heating outlet (14) is arranged at the bottom of the heat preservation cavity (12), a discharge hole (15) is arranged at the center of the bottom of the kettle body (11), a stirring motor (19) is arranged in the middle of the top cover of the heat preservation cavity (12), the output port of the stirring motor (19) is communicated with a stirring blade (16) arranged in the kettle body (11), the top cover of the kettle body (11) on the left side of the stirring motor (19) is provided with an observation hole (18), and a top cover of the kettle body (11) on the right side of the stirring motor (19) is provided with a feeding hole (20).
5. The refining device of ethyl oleate for pharmaceutical use of claim 4, wherein the stainless steel reaction kettle (1), the stainless steel storage tank (9) and the pipe connected with the discharge port at the lower end of the plate-and-frame filter (2) are all provided with control valves, and the feed port of the bag filter (7) and the feed port of the plate-and-frame filter (2) are all provided with control valves.
6. The refining device of ethyl oleate for medicine according to claim 4, wherein the stainless steel reaction kettle (1) is a carbon steel jacket-lined enamel reaction kettle, and the upper end of the stainless steel reaction kettle (1) is provided with a transparent glass observation hole (18), a temperature sensor mounting port, a feed inlet (20), a pressure sensor mounting port, a liquid level meter mounting port, a vacuum valve mounting port and an air inlet.
7. The refining device of medicinal ethyl oleate according to claim 4, wherein four groups of supporting seats (17) are uniformly welded on the shell of the heat preservation cavity (12) outside the stainless steel reaction kettle (1), the kettle body (11) above the supporting seats (17) is connected with a circulating material port, the heat preservation cavity (12) arranged outside the stainless steel reaction kettle (1) is communicated with a heating device through a heating outlet (14) and a heating inlet (13), and a heating medium inside the heat preservation cavity (12) is one of heat conduction oil and steam.
8. An application of a refining device of medicinal ethyl oleate in a refining method of medicinal ethyl oleate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010622798.9A CN111704958A (en) | 2020-07-01 | 2020-07-01 | Method and device for refining medicinal ethyl oleate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010622798.9A CN111704958A (en) | 2020-07-01 | 2020-07-01 | Method and device for refining medicinal ethyl oleate |
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| CN111704958A true CN111704958A (en) | 2020-09-25 |
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| CN202010622798.9A Withdrawn CN111704958A (en) | 2020-07-01 | 2020-07-01 | Method and device for refining medicinal ethyl oleate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112979466A (en) * | 2021-03-02 | 2021-06-18 | 江西益普生药业有限公司 | Refining device for medicinal ethyl oleate and use method thereof |
| CN115181022A (en) * | 2022-07-26 | 2022-10-14 | 江西益普生药业有限公司 | Purification method for purifying and refining ethyl oleate |
-
2020
- 2020-07-01 CN CN202010622798.9A patent/CN111704958A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112979466A (en) * | 2021-03-02 | 2021-06-18 | 江西益普生药业有限公司 | Refining device for medicinal ethyl oleate and use method thereof |
| CN112979466B (en) * | 2021-03-02 | 2023-08-25 | 江西益普生药业有限公司 | Application method of refining device of medicinal ethyl oleate |
| CN115181022A (en) * | 2022-07-26 | 2022-10-14 | 江西益普生药业有限公司 | Purification method for purifying and refining ethyl oleate |
| CN115181022B (en) * | 2022-07-26 | 2023-08-11 | 江西益普生药业有限公司 | Purification method for purifying and refining ethyl oleate |
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