CN212068760U - Production device of methylated cyclodextrin derivatives - Google Patents

Abstract

The utility model discloses a device for producing of methylation cyclodextrin derivative, including reation kettle, liquid auxiliary material jar and gaseous auxiliary material jar, gaseous auxiliary material jar is used for storing liquefied gas auxiliary material, is equipped with liquid gas two state constant voltage metering components between reation kettle and the gaseous auxiliary material jar, is equipped with the measuring pump between liquid auxiliary material jar and the reation kettle, still includes the control assembly who all links to each other with measuring pump and liquid gas two state constant voltage metering components. When the methylated cyclodextrin derivative is produced, the gas auxiliary material is decompressed by the liquid-gas two-state constant-pressure metering assembly to form a gas state, and then the gas auxiliary material enters the reaction kettle to participate in the addition reaction, and the liquid-gas two-state constant-pressure metering assembly can accurately meter the flow of the gas auxiliary material, so that the control assembly can adjust the ratio of the gas auxiliary material to the liquid auxiliary material, and the product quality is ensured.

Description

Production device of methylated cyclodextrin derivatives

Technical Field

The utility model relates to a chemical industry equipment technical field, in particular to device for producing of methylation cyclodextrin derivative.

Background

The cyclodextrin derivative is obtained by modifying natural cyclodextrin through molecules, and is a series of compounds with excellent performance. The cyclodextrin derivatives have a cavity, can be used as a binding site for a substrate or a guest molecule, and are used for constructing various supramolecules, particularly functionalized supramolecular aggregates. Methylated cyclodextrin derivatives are increasingly used in pharmaceuticals and cosmetics as a series of methylated cyclodextrin derivatives with high solubility and high permeability.

The current synthetic method of the methylated cyclodextrin is mainly obtained by synthesizing dimethyl sulfate as a methylation reagent under an alkaline condition, and although the method is carried out at normal temperature and normal pressure and has mild reaction conditions, the synthetic process is complex and a plurality of byproducts are generated; in order to solve the problems, halogenated alkane is used as a methylating agent in part of processes, so that the problem of more byproducts is solved, but the halogenated alkane is in a gaseous state and is inconvenient to measure, so that the proportion of materials is influenced, and the quality of products is finally influenced.

Therefore, how to improve the quality of methylated cyclodextrin products is a technical problem which needs to be solved urgently by the technical personnel in the field.

SUMMERY OF THE UTILITY MODEL

The utility model aims at providing a production device of methylation cyclodextrin derivative, it is through the gaseous auxiliary material of liquid gas two-state constant voltage measurement component control, has guaranteed the quality of product.

In order to realize the above-mentioned purpose, the utility model provides a device for producing of methylation cyclodextrin derivative, including reation kettle, liquid auxiliary material jar and gaseous auxiliary material jar, gaseous auxiliary material jar is used for storing liquefied gas auxiliary material, be equipped with liquid gas two state constant voltage measurement subassembly between reation kettle and the gaseous auxiliary material jar, liquid auxiliary material jar with be equipped with the measuring pump between the reation kettle, still include with the measuring pump with the equal continuous control assembly of liquid gas two state constant voltage measurement subassembly.

Preferably, still including spraying the mechanism, spray the mechanism through sealed pipeline with reation kettle's bottom links to each other, the shower nozzle that sprays the mechanism is fixed in reation kettle's top, be used for to spray the material in the reation kettle, it still is equipped with the booster pump that is used for the material pressure boost in the mechanism to spray.

Preferably, the system further comprises a water pretreatment tank for producing purified water, wherein the water pretreatment tank is connected with the reaction kettle and is used for conveying the purified water into the reaction kettle.

Preferably, the bottom of the reaction kettle is connected with a crude product tank for containing a semi-finished product obtained by the reaction, and the reaction kettle further comprises a filtering component for filtering the semi-finished product, a refining component for processing the semi-finished product and a finished product tank for containing the finished product.

Preferably, the filtration assembly comprises a filter positioned between the reaction vessel and the crude tank and an ultrafiltration mechanism positioned between the crude tank and the finished tank.

Preferably, the polishing assembly includes a polishing tank connected to the filter assembly and a polishing mechanism located after the polishing tank, the polishing mechanism being connected to the product tank.

Preferably, the finished product tank is connected with a sterilization system for sterilizing the finished product liquid.

Preferably, the sterilization system is connected with a dryer, and the sterilized finished product liquid is dried and processed by the dryer to be made into a finished product.

Preferably, the top of reation kettle even has the gas replacement subassembly that is used for replacing gaseous in the reation kettle and is used for measuring the manometer of reation kettle internal pressure, the gas replacement subassembly with the manometer all with control assembly links to each other.

Preferably, the top of the reaction kettle is further provided with a pressure relief mechanism connected with the control assembly and used for adjusting the pressure in the reaction kettle.

The utility model provides a production device of methylation cyclodextrin derivative, including reation kettle, liquid auxiliary material jar and gaseous auxiliary material jar, gaseous auxiliary material jar is used for storing liquefied gas auxiliary material, is equipped with liquid gas two state constant voltage metering components between reation kettle and the gaseous auxiliary material jar, is equipped with the measuring pump between liquid auxiliary material jar and the reation kettle, still includes the control assembly who all links to each other with measuring pump and liquid gas two state constant voltage metering components.

When the methylated cyclodextrin derivative is produced, the gas auxiliary material is decompressed by the liquid-gas two-state constant-pressure metering assembly to form a gas state, and then the gas auxiliary material enters the reaction kettle to participate in the addition reaction, and the liquid-gas two-state constant-pressure metering assembly can accurately meter the flow of the gas auxiliary material, so that the control assembly can adjust the ratio of the gas auxiliary material to the liquid auxiliary material, and the product quality is ensured.

In addition, a spraying mechanism is arranged in the reaction kettle, the spraying mechanism can extract the materials from the bottom of the reaction kettle, and the materials are sprayed at the top of the reaction kettle. The spraying mechanism can increase the contact area between the liquid material and the gas auxiliary material, accelerate the reaction speed, and enable the material to form circulation, thereby improving the utilization rate of the material.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.

Fig. 1 is a schematic structural diagram of a production apparatus for methylated cyclodextrin derivatives provided by the present invention.

Wherein the reference numerals in fig. 1 are:

the system comprises a water pretreatment tank 1, a reaction kettle 2, a gas replacement component 3, a pressure gauge 4, a liquid auxiliary tank 5, a gas auxiliary tank 6, a metering pump 7, a liquid-gas two-state constant-pressure metering component 8, a filter 9, a crude product tank 10, an ultrafiltration mechanism 11, a refining tank 12, a refining mechanism 13, a finished product tank 14, a sterilization system 15, a dryer 16, a spraying mechanism 17 and a pressure relief mechanism 18.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.

In order to make the technical field of the present invention better understand, the present invention will be described in detail with reference to the accompanying drawings and the detailed description.

Referring to fig. 1, fig. 1 is a schematic structural diagram of a production apparatus for methylated cyclodextrin derivatives according to the present invention.

The utility model provides a production device of methylation cyclodextrin derivative, as shown in figure 1, including reation kettle 2, be equipped with the stirring rake in reation kettle 2, the reaction raw materials is reacted to the postemergence of predetermineeing the temperature through heating up in reation kettle 2, can generate the reaction of methylation cyclodextrin derivatives such as methyl alpha cyclodextrin, methyl beta cyclodextrin or methyl gamma cyclodextrin in reation kettle 2.

Auxiliary materials, such as chloralkane, bromoalkane and the like, need to be added in the production process of the methylated cyclodextrin derivatives, and an auxiliary material tank is further arranged in the production device, specifically, the auxiliary material tank comprises a liquid auxiliary material tank 5 and a gas auxiliary material tank 6, and the liquid auxiliary material tank and the gas auxiliary material tank are hermetically connected with the reaction kettle 2. In order to improve the sealing performance, the reaction kettle 2 and the auxiliary material tank are connected by adopting a seamless stainless steel pipe fitting, so that the sealing gas is prevented from leaking. A metering pump 7 is arranged between the reaction kettle 2 and the liquid auxiliary material tank 5, a liquid-gas two-state constant-pressure metering assembly 8 is arranged between the reaction kettle 2 and the gas auxiliary material tank 6, and the liquid-gas two-state constant-pressure metering assembly 8 can accurately meter the feeding amount of the gas auxiliary material. The gas auxiliary materials are stored in a gas auxiliary material tank 6 after being compressed and liquefied, and in the charging process, the gas auxiliary materials enter the reaction kettle through a liquid-gas two-state constant-pressure metering component 8 and are gasified in the liquid-gas two-state constant-pressure metering component 8 under reduced pressure. In addition, still be equipped with the control assembly among the apparatus for producing, measuring pump 7 and liquid gas two-state constant voltage measurement subassembly 8 all link to each other with the control assembly, and the feeding volume of two kinds of auxiliary materials of control assembly control makes two kinds of auxiliary materials carry into reation kettle with invariable pressure and feeding volume, realizes the continuous feeding or the semi-continuous feeding of auxiliary material, guarantees that reaction material ratio is more accurate, product quality homogeneous. The control component can be a MCU microcontroller, a PLC controller or an industrial personal computer and the like.

Optionally, the liquid-gas two-state constant-pressure metering assembly 8 may specifically include a pressure reducing mechanism and a gas flowmeter, the pressure reducing mechanism may enable the liquid gas auxiliary material to be subjected to pressure reduction gasification and output at a constant pressure, and the structure of the pressure reducing mechanism may refer to a pressure reducing valve in the prior art. The gas flowmeter is positioned behind the decompression mechanism and measures the flow of the gas auxiliary materials, and the accuracy of the measurement result is obviously improved because the pressure of the decompressed gas auxiliary materials is constant.

Optionally, in order to improve the mixing efficiency between the liquid material and the gas material, the production device further comprises a spraying mechanism 17, and the spraying mechanism 17 comprises a spray head and a booster pump. Specifically, the shower nozzle setting is in reation kettle to be located reation kettle's top, the one end of sealed pipeline links to each other with the shower nozzle, and the other end links to each other with reation kettle's bottom, and the booster pump is arranged in the sealed pipeline. The booster pump pumps the materials out of the bottom of the reaction kettle 2 and then conveys the materials to the spray head, and the materials are sprayed back into the reaction kettle by the spray head. Wherein, the spray nozzle can be embodied as a universal spray nozzle, and the booster pump can be embodied as a sanitary-grade variable-frequency automatic booster pump. In addition, the number of the spray heads can be more than or equal to two, and the plurality of spray heads spray the materials into the reaction kettle 2, so that the contact area between the gas auxiliary materials and the materials is larger.

Optionally, the apparatus for producing still includes pretreatment of water jar 1, and pretreatment of water jar 1 is used for producing purified water, and pretreatment of water jar 1 links to each other with reation kettle 2, and purified water is carried to reation kettle 2 after equipment such as water pump pressurizes. The structure of the water pretreatment tank 1 can refer to the prior art, and is not described herein.

Optionally, the production apparatus for methylated cyclodextrin derivatives further includes a crude product tank 10, the bottom of the reaction kettle 2 is connected to the crude product tank 10 through an output pipeline, and the semi-finished product obtained by the reaction flows into the crude product tank 10 along the output pipeline, so that the production apparatus can continuously produce. In addition, the bottom of reaction kettle 2 is provided with an emptying valve, and the residual materials in reaction kettle 2 can be discharged through the emptying valve after the production device is stopped.

In addition, the crude liquid contains more impurities, and the crude liquid can be used as a finished liquid after being filtered and refined. Therefore, the production device of the methylated cyclodextrin derivatives further comprises a filtering component and a refining component which are connected with the crude product tank 10, the filtering component can filter solid impurities in the semi-finished product, and the refining component desalts the semi-finished product and intercepts small-molecule impurities to generate finished product liquid. Finally, the finished product liquid flows into a finished product tank 14 for storage.

Optionally, the filtering component includes a filter 9 and an ultrafiltration mechanism 11, the filter 9 is located between the crude product tank 10 and the reaction kettle 2, the filter 9 may be a filter bag, a plate-and-frame filter or a titanium rod filter, etc., the aperture of the filter 9 is usually not greater than 5 μm, the filter 9 and the crude product tank 10 may be provided with a circulation pipeline, and the crude product liquid enters the crude product tank 10 after passing through the circulation filtration. Ultrafiltration mechanism 11 is located behind crude jar 10 for filter macromolecular impurity, and ultrafiltration mechanism 11 can specifically adopt membrane filtration equipment, and the aperture of filtration pore is not more than 20000 dalton.

After filtration, salt and small molecular impurities still exist in the product, so the production device further comprises a refining component, specifically, the refining component comprises a refining tank 12 and a refining mechanism 13, the filtered product enters the refining tank 12 and then is input into the refining mechanism 13 from the refining tank 12, the refining mechanism 13 can be specifically a reverse osmosis membrane system, a nanofiltration membrane system or an ion exchange resin system, and the like, the product treated by the refining mechanism 13 is conveyed back into the refining tank 12, the product forms circulation between the refining tank 12 and the refining mechanism 13 until the conductivity and the pH of the product are qualified, the product is transferred into a finished product tank 14, and the pressure of the product circulating between the refining tank 12 and the refining mechanism 13 can be provided by a pump.

The finished product liquid is required to be sterilized after impurities are filtered, the production device of the methylated cyclodextrin derivatives further comprises a sterilization system 15, the sterilization system 15 is connected with the finished product tank 14, and the finished product liquid enters the sterilization system 15 from the finished product tank 14 for sterilization.

Optionally, the sterilization system 15 may be specifically a polyethersulfone filter, the selectable pore sizes of which include 0.1, 0.22, 0.45, 0.65, 0.8, 1.2, and 3.0 μm, and the polyethersulfone filter filters the finished product liquid to remove the infectious microbes therein, thereby completing the sterilization operation.

The sterilized finished liquid needs to be dried to obtain a finished product, and in this embodiment, a dryer 16 connected to the sterilization system 15 is provided, and the finished product is obtained after drying processing by the dryer 16. Of course, the user may use drying equipment such as spray drying or fluidized bed drying, if necessary, and the drying equipment is not limited herein.

In this embodiment, methylated cyclodextrin derivative's apparatus for producing passes through filter 9, ultrafiltration mechanism 11 and refined mechanism 13 and carries out further processing to crude liquid, and solid particle, macromolecular impurity and the output finished product liquid of small molecule impurity in the filtration crude liquid, remove the miscellaneous fungus in the finished product liquid through degerming system 15 afterwards, process finished product liquid into the finished product through drying equipment at last. Production can be completed through automatic control of the control assembly in the production process, and production efficiency of products is improved.

In addition, in order to avoid impurity atoms to enter into the reation kettle, influence product quality, the apparatus for producing has still set up gas replacement subassembly 3, specifically, gas replacement subassembly 3 includes vacuum pump and sealed air supply, and reation kettle 2's top links to each other with the vacuum pump, and the vacuum pump is arranged in taking out the gas in reation kettle 2. The top of the reaction kettle 2 is also connected with a sealing gas source through a sealing gas pipeline, a sealing gas pressure regulating valve is arranged in the sealing gas pipeline, a pressure gauge 4 is also arranged at the top of the reaction kettle, the pressure-resistant range of the pressure gauge 4 can be selected from-0.1-2.4 MPa, the pressure gauge 4, the sealing gas pressure regulating valve and the vacuum pump are all connected with a control assembly, and the control assembly can control the gas replacement pressure to be 0.05-0.1 MPa. The control assembly pumps out air in the reaction kettle 2 through the vacuum pump, then the sealing gas is filled into the reaction kettle 2 through the sealing gas source, the control assembly adjusts the pressure regulating valve of the sealing gas to control the pressure in the reaction kettle 2, the gas in the reaction kettle 2 is pumped out through the vacuum pump again after the gas is filled to the preset pressure, and the reaction kettle 2 can almost completely replace the gas in the kettle into the sealing gas after three times of replacement. Specifically, the sealing gas may be nitrogen, an inert gas, or the like which does not react with the reactant or the reaction product in the reaction vessel 2.

Optionally, for controlling the pressure in reaction kettle 2, the top of reaction kettle 2 is further provided with a pressure relief assembly, the pressure relief assembly includes a pressure gauge 4 for measuring the pressure in reaction kettle 2 and a pressure relief mechanism 18 connected with the control assembly, and pressure relief mechanism 18 may specifically be a pressure relief valve. When the pressure in the reaction kettle 2 is too high, the control assembly controls the pressure relief valve to be opened, so that the overpressure of the reaction kettle 2 is avoided.

In this embodiment, methylated cyclodextrin derivative's apparatus for producing uses the gas in reation kettle 2 through vacuum pump and sealed air supply cooperation and carries out the replacement, realizes taking sealed gas as reaction environment, avoids introducing other atoms in the reaction process. In addition, the auxiliary material is controlled by the control assembly to be fed, so that the full-automatic feeding of the auxiliary material is realized, and the production process is safer and more efficient.

It is noted that, in this specification, relational terms such as first and second, and the like are used solely to distinguish one entity from another entity without necessarily requiring or implying any actual such relationship or order between such entities.

The production device of the methylated cyclodextrin derivative provided by the utility model is described in detail above. The principles and embodiments of the present invention have been explained herein using specific examples, and the above descriptions of the embodiments are only used to help understand the method and its core ideas of the present invention. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, the present invention can be further modified and modified, and such modifications and modifications also fall within the protection scope of the appended claims.

Claims (10)

1. The utility model provides a production device of methylation cyclodextrin derivative, a serial communication port, including reation kettle (2), liquid auxiliary material jar (5) and gaseous auxiliary material jar (6), gaseous auxiliary material jar (6) are used for storing liquefied gaseous auxiliary material, reation kettle (2) with be equipped with liquid gas two state constant voltage measurement subassembly (8) between gaseous auxiliary material jar (6), liquid auxiliary material jar (5) with be equipped with between the reation kettle measuring pump (7), still include with measuring pump (7) with the control assembly that liquid gas two state constant voltage measurement subassembly (8) all link to each other.

2. The production device of claim 1, further comprising a spraying mechanism (17), wherein the spraying mechanism (17) is connected with the bottom of the reaction kettle through a sealed pipeline, a nozzle of the spraying mechanism (17) is fixed on the top of the reaction kettle and used for spraying materials into the reaction kettle, and a booster pump for boosting the materials is further arranged in the spraying mechanism (17).

3. The production device according to claim 1, further comprising a water pretreatment tank (1) for producing purified water, wherein the water pretreatment tank (1) is connected to the reaction kettle (2) and is used for conveying the purified water into the reaction kettle (2).

4. The production apparatus according to claim 3, wherein the bottom of the reaction vessel (2) is connected to a crude tank (10) for containing a semi-finished product obtained by the reaction, and further comprises a filtering unit for filtering the semi-finished product, a refining unit for processing the semi-finished product, and a finished product tank (14) for containing a finished product.

5. The production plant according to claim 4, characterized in that the filtration assembly comprises a filter (9) between the reaction vessel (2) and the crude tank (10), and an ultrafiltration mechanism (11) between the crude tank (10) and the finished tank (14).

6. The production device according to claim 4, characterized in that the refining assembly comprises a refining tank (12) connected to the filter assembly and a refining mechanism (13) located after the refining tank (12), the refining tank (12) being connected to the product tank (14).

7. The production plant according to claim 4, characterized in that the finished product tank (14) is connected to a sterilization system (15) for sterilizing the finished product liquid.

8. The production device according to claim 7, wherein the sterilization system (15) is connected to a dryer (16), and the sterilized product liquid is dried and processed by the dryer (16) to form a finished product.

9. The production device according to any one of claims 1 to 8, wherein a gas replacement assembly (3) for replacing gas in the reaction kettle and a pressure gauge (4) for measuring pressure in the reaction kettle are connected to the top of the reaction kettle (2), and the gas replacement assembly (3) and the pressure gauge (4) are both connected to the control assembly.

10. The production device according to claim 8, wherein the top of the reaction kettle (2) is further provided with a pressure relief mechanism (18) connected with the control component for adjusting the pressure in the reaction kettle (2).

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