CN219470076U - High-efficient crystallization device is used in production of medicinal sucrose that contains thermal cycle - Google Patents

Abstract

The utility model discloses a high-efficiency crystallization device for producing medicinal sucrose containing thermal circulation, which comprises a vacuum circulation assembly, a heating circulation assembly, a high-efficiency crystallization assembly, a cooling circulation assembly, a snake-shaped reflux condenser pipe and a reflux bottle, wherein the vacuum circulation assembly is connected with the snake-shaped reflux condenser pipe, the snake-shaped reflux condenser pipe is connected with the reflux bottle, the reflux bottle is connected with the high-efficiency crystallization assembly, and the high-efficiency crystallization assembly is connected with the heating circulation assembly; the serpentine return condenser tube is connected with the cooling circulation assembly. The utility model solves the problems that the existing reaction container needs to be frequently opened and closed, cannot be continuously produced, increases pollution risk, affects production efficiency and the like.

Description

High-efficient crystallization device is used in production of medicinal sucrose that contains thermal cycle

Technical Field

The utility model belongs to the field of pharmaceutical auxiliary material production, and particularly relates to a high-efficiency crystallization device for producing pharmaceutical sucrose containing thermal circulation.

Background

The medicinal sucrose is taken as one of important medicinal auxiliary materials and is an important component affecting the quality of the medicine. The medicinal sucrose not only can shape and increase stability of the medicinal preparation, serve as a carrier and flavor, but also has the functions of adhesion, moisture retention, solubilization assistance, freeze-drying protection and the like, can provide energy for human bodies, and is widely applied to oral preparations such as granules, tablets, syrup, oral liquid and the like, and also is applied to injection; compared with European and American countries, the medicinal sucrose in China is relatively late to produce, has relatively few varieties and specifications, and still has a large gap in key indexes such as sucrose non-sugar, color value, conductivity, dextrin, bacterial endotoxin and the like;

at present, the production method of the medicinal sucrose at home and abroad mainly comprises an ethanol-water recrystallization method, a reverse osmosis method, a carbonic acid method, a flocculating agent precipitation method and an ion exchange resin method. In the production of medicinal sucrose, the supersaturation degree of sucrose has great influence on the sucrose crystallization process according to the basic knowledge of sucrose solution nucleation theory and sucrose crystallography. The supersaturation curve of sucrose changes along with the temperature and the brix of the sucrose solution, and the change of the vacuum degree influences the temperature of the sucrose solution in the reaction container; therefore, the temperature, the brix and the vacuum degree in the reaction vessel of the sucrose solution need to be paid attention to in real time in the crystallization process of sucrose; when the existing crystallization device is used, the temperature of the sucrose solution can be observed in real time through a temperature sensor, and the vacuum degree of the reaction container can be observed through a vacuum meter of a vacuum pump; however, the acquisition of the brix data of the sucrose solution and the input of the seed crystal require the operation of starting the reaction vessel; the reaction vessel is frequently opened and closed, so that the risk of introducing microorganisms is increased, the vacuum degree is changed frequently, and the production efficiency is affected; therefore, there is a need to provide a high-efficiency crystallization device for producing medicinal sucrose, which solves the above technical problems.

Disclosure of Invention

The utility model aims to provide a high-efficiency crystallization device for producing medicinal sucrose containing thermal cycle, wherein a crystallization kettle in the system is provided with a brix probe, brix data can be observed in real time, the condition of repeated uncovering sampling monitoring is avoided, meanwhile, the material can be added in a supplementing manner when crystallization reaction is carried out through the arranged constant-pressure feeding device, the influence on the vacuum degree of a crystallization reaction system is avoided to the greatest extent, the continuous carrying out of the crystallization reaction is ensured, and the problems that the conventional reaction container needs frequent opening and closing, continuous production cannot be realized, pollution risk is increased, production efficiency is influenced and the like are solved through the system.

In order to solve the technical problems, the utility model is realized by the following technical scheme:

the utility model provides a medicinal sucrose production is with high-efficient crystallization device that contains thermal cycle, includes vacuum circulation subassembly, heating circulation subassembly, high-efficient crystallization subassembly, cooling circulation subassembly, snakelike backward flow condenser pipe and backward flow bottle, vacuum circulation subassembly and snakelike backward flow condenser pipe are connected, snakelike backward flow condenser pipe is connected with the backward flow bottle, backward flow bottle and high-efficient crystallization subassembly are connected, high-efficient crystallization subassembly and heating circulation subassembly are connected; the serpentine return condenser tube is connected with the cooling circulation assembly.

Preferably, the vacuum circulating assembly comprises a circulating water vacuum pump and a hose, wherein one end of the hose is connected with the circulating water vacuum pump, and the other end of the hose is connected with the serpentine reflux condenser pipe.

Preferably, the heating circulation assembly comprises a heating circulation machine and heating connecting pipes, and the two heating connecting pipes are arranged; one end of each heating connecting pipe is connected with the heating cycle machine, and the other end of each heating connecting pipe is connected with the high-efficiency crystallization component.

Preferably, the efficient crystallization component comprises a rectangular support frame, a reaction kettle body, a stirring motor, a stirring rod, a reaction kettle interlayer and a reaction kettle cover body, wherein the rectangular support frame is internally connected with the reaction kettle body, and the reaction kettle interlayer is arranged on the outer wall of the reaction kettle body; the top end of the reaction kettle body is connected with a reaction kettle cover body, a stirring rod penetrates through the reaction kettle cover body, and one end of the stirring rod outside the reaction kettle body is connected with a stirring motor; and a discharge hole is formed in the bottom end of the reaction kettle body.

Preferably, the reaction kettle cover body is provided with a decompression port, a condenser interface, a brix probe interface, a thermometer interface, a material feeding port, a seed crystal filling port, a syrup filling port and a sealing stirring port, wherein the sealing stirring port is arranged in the middle of the reaction kettle cover body, and the stirring rod penetrates through the reaction kettle cover body through the sealing stirring port.

Preferably, the cooling circulation assembly comprises a cooling circulation pump and cooling connection pipes, and two cooling connection pipes are arranged; one end of each cooling connecting pipe is connected with the cooling circulating pump, and the other end of each cooling connecting pipe is connected with the serpentine reflux condensing pipe.

Preferably, the serpentine reflux condenser tube comprises a cooling liquid inlet, a cooling liquid outlet and a vacuum pumping port, wherein the vacuum pumping port is connected with a hose, and the cooling liquid inlet and the cooling liquid outlet are respectively connected with a cooling connecting pipe.

Preferably, the pressure reducing port is connected with an exhaust valve with an opening and closing function; the condenser interface is connected with a serpentine reflux condenser pipe through a reflux bottle; the brix probe interface is connected with a brix probe with a digital display function; the thermometer interface is connected with a temperature probe; the seed crystal filling port and the syrup filling port are connected with a constant pressure funnel; the material feed opening is provided with a fixable top cover.

Preferably, the reaction kettle interlayer is provided with an interlayer liquid inlet positioned at the bottom of the reaction kettle and an interlayer liquid outlet positioned at the middle part of the reaction kettle, and the interlayer liquid inlet and the interlayer liquid outlet are respectively connected with the heating connecting pipe.

The utility model has the following beneficial effects:

1. according to the efficient crystallization system of medicinal sucrose containing thermal circulation, disclosed by the utility model, the heat source is circularly conveyed to the interlayer of the reaction kettle by adding the circulator, so that the heat source required by crystallization of the efficient crystallization device is ensured, the utilization efficiency of the heat is improved by recycling, and the production cost is reduced.

2. According to the utility model, the constant-pressure feeding device is connected with the material feeding port, and the constant-pressure feeding device is used for feeding seed crystals and syrup in the crystallization reaction process, so that the problems of low crystallization reaction efficiency and the like caused by the change of the vacuum degree in a reaction system due to frequent uncovering are avoided, and the probability of microbial pollution is reduced to the greatest extent.

3. The crystallization kettle is provided with the brix probe and the temperature probe, the brix probe has a digital display function, can display the brix of the sucrose solution in real time, and avoids frequent uncapping sampling monitoring in the reaction process, thereby enabling crystallization reaction to be continuously carried out.

Of course, it is not necessary for any one product to practice the utility model to achieve all of the advantages set forth above at the same time.

Drawings

FIG. 1 is an overall schematic diagram of a high-efficiency crystallization device for producing medicinal sucrose containing thermal cycle according to the present utility model;

FIG. 2 is a schematic diagram of a high efficiency crystallization assembly of the present utility model;

FIG. 3 is a schematic top view of the reactor cover of the present utility model.

In the drawings, a 1-vacuum circulating component, a 11-circulating water vacuum pump, a 12-hose, a 2-heating circulating component, a 21-heating circulating machine, a 22-heating connecting pipe, a 3-efficient crystallizing component, a 31-rectangular supporting frame, a 32-reaction kettle body, a 33-stirring motor, a 34-stirring rod, a 35-reaction kettle interlayer, a 351-interlayer liquid inlet, a 352-interlayer liquid outlet, a 36-discharge port, a 37-reaction kettle cover body, a 371-decompression port, a 372-condenser interface, a 373-brix probe interface, a 374-thermometer interface, a 375-material feeding port, 376-seed crystal feeding port, 377-syrup feeding port, 378-sealing stirring port, a 4-cooling circulating component, a 41-cooling circulating pump, a 42-cooling connecting pipe, a 5-serpentine reflux condensing pipe, a 51-cooling liquid inlet, a 52-cooling liquid outlet, a 53-vacuum pumping port and a 6-reflux bottle.

Detailed Description

The present utility model will now be described in detail with reference to the drawings and examples, wherein it is apparent that the examples described are some, but not all, of the examples of the present utility model. The components of the present utility model, which are generally described and illustrated in the figures herein, may be arranged and disposed in a variety of different configurations.

Example 1

Referring to fig. 1-3, a high-efficiency crystallization device for producing medicinal sucrose containing thermal cycle comprises a vacuum circulation assembly 1, a heating circulation assembly 2, a high-efficiency crystallization assembly 3, a cooling circulation assembly 4, a serpentine reflux condenser pipe 5 and a reflux bottle 6, wherein the vacuum circulation assembly 1 is connected with the serpentine reflux condenser pipe 5, the serpentine reflux condenser pipe 5 is connected with the reflux bottle (6), the reflux bottle 6 is connected with the high-efficiency crystallization assembly 3, and the high-efficiency crystallization assembly 3 is connected with the heating circulation assembly 2; a serpentine return condenser tube 5 is connected to the cooling circulation assembly 4.

The vacuum circulation assembly 1 comprises a circulating water vacuum pump 11 and a hose 12, wherein one end of the hose 12 is connected with the circulating water vacuum pump 11, and the other end of the hose 12 is connected with the serpentine return condensation pipe 5.

The heating circulation assembly 2 comprises a heating circulation machine 21 and heating connecting pipes 22, and the heating connecting pipes 22 are arranged in two; one end of the two heating connecting pipes 22 is connected with the heating cycle machine 21, and the other end is connected with the high-efficiency crystallization component 3.

The high-efficiency crystallization assembly 3 comprises a rectangular supporting frame 31, a reaction kettle body 32, a stirring motor 33, a stirring rod 34, a reaction kettle interlayer 35 and a reaction kettle cover 37, wherein the reaction kettle body 32 is connected in the rectangular supporting frame 31, and the reaction kettle interlayer 35 is arranged on the outer wall of the reaction kettle body 32; the top end of the reaction kettle body 32 is connected with a reaction kettle cover body 37, a stirring rod 34 is arranged penetrating the reaction kettle cover body 37, and one end of the stirring rod 34 outside the reaction kettle body 32 is connected with a stirring motor 33; a discharge port 36 is arranged at the bottom end of the reaction kettle body 32.

The reaction kettle interlayer 35 between the inner layer and the outer layer of the double-layer glass reaction kettle can be connected with the heating circulator 21 to be introduced with a heat source, the heat source can adopt hot water or hot oil (dimethyl silicone oil) and the like, and the heating circulator 21 is controlled by a temperature controller and can display the heating temperature.

The reaction kettle cover 37 is provided with a decompression port 371, a condenser interface 372, a brix probe interface 373, a thermometer interface 374, a material feeding port 375, a seed crystal filling port 376, a syrup filling port 377 and a sealing stirring port 378, wherein the sealing stirring port 378 is arranged in the middle of the reaction kettle cover 37, and the stirring rod 34 penetrates through the reaction kettle cover 37 through the sealing stirring port 378.

The cooling circulation assembly 4 includes a cooling circulation pump 41 and a cooling connection pipe 42, the cooling connection pipe 42 being provided in two; one end of the two cooling connecting pipes 42 is connected with the cooling circulating pump 41, and the other end is connected with the serpentine return condensing pipe 5.

The serpentine return condenser tube 5 includes a coolant inlet 51, a coolant outlet 52, and a vacuum suction port 53, the vacuum suction port 53 being connected to the hose 12, and the coolant inlet 51 and the coolant outlet 52 being connected to the cooling connection tube 42, respectively.

The pressure reducing port 371 is connected with an exhaust valve (not labeled in the figure) having an opening and closing function; the condenser interface 372 is connected with the serpentine reflux condenser pipe 5 through the reflux bottle 6; the brix probe interface 373 is connected with a brix probe (not labeled in the figure) with a digital display function; a temperature probe (not shown) is connected to the thermometer interface 374; seed filler 376 and syrup filler 377 are connected to a constant pressure hopper (not shown); the material inlet 375 is provided with a fixable top cover (not shown).

The reaction kettle interlayer 35 is provided with an interlayer liquid inlet 351 positioned at the bottom of the reaction kettle and an interlayer liquid outlet 352 positioned at the middle part of the reaction kettle, and the interlayer liquid inlet 351 and the interlayer liquid outlet 352 are respectively connected with the heating connecting pipe 22.

Example 2

The present example provides a method for performing a crystallization reaction using the apparatus of example 1, comprising the steps of:

s1, connecting equipment: firstly, a vacuum circulation assembly 1, a heating circulation assembly 2, a high-efficiency crystallization assembly 3, a cooling circulation assembly 4, a serpentine reflux condenser pipe 5 and a reflux bottle 6 are arranged;

specifically, a brix probe (not shown) is correctly connected to a brix probe interface 373, a temperature probe (not shown) is correctly connected to a thermometer interface 374, a seed filling port 376 is connected to a constant pressure funnel (not shown), a syrup filling port 377 is connected to a constant pressure funnel (not shown), an exhaust valve (not shown) is connected to a decompression port 371, a condenser interface 372 is connected to a serpentine reflux condenser pipe 5 through a reflux bottle 6, a stirring rod 34 passes through a sealed stirring port 378 to be connected to a stirring motor 33, a cooling liquid inlet 51 and a cooling liquid outlet 52 of the serpentine reflux condenser pipe 5 are connected to a cooling liquid circulating pump 41 through a cooling connecting pipe 42, and the other interface is connected to the circulating water vacuum pump 11 through a hose 12;

s2, checking the air tightness of equipment: closing the exhaust valve, closing the material feeding port 375, opening the circulating water vacuum pump 11, and observing whether the reading is kept unchanged for a period of time after the vacuum reading reaches the minimum;

s3, sterilizing the device: opening a material feeding port 375, closing the material feeding port 375 after adding alcohol, confirming that a decompression port 371 is closed, sequentially starting a heating circulation machine 21, a cooling circulation pump 41 and a circulating water vacuum pump 11, opening the decompression port 371 for pressure relief after alcohol is completely evaporated, closing the circulating water vacuum pump 11, closing the decompression port 371, and repeating the operation for 2-3 times.

Specifically, the alcohol is 75% alcohol, the amount of added 75% alcohol is 100-200ml, and the mixture is heated to 60-80 ℃.

S4, crystallization operation: opening a material feeding port 375, adding sucrose solution, closing a constant-pressure funnel liquid adding valve, adding seed solution and syrup replenishing liquid into constant-pressure funnels at a seed crystal adding port 376 and a syrup adding port 377 respectively, starting a circulating water vacuum pump 11, a heating circulating machine 21 and a stirring device, performing reduced pressure distillation, adding the seed solution and the syrup replenishing liquid respectively when crystallization reaction reaches a certain degree, closing the heating circulating machine 21 when the crystallization reaction reaches the end point, opening the pressure reducing port 371 for pressure relief, closing the circulating water vacuum pump 11, closing a cooling circulating pump 41, opening a discharge port 36 for discharging, opening the material feeding port 375 after discharging is completed, cleaning a reaction kettle body 32 by purified water, wherein the adding condition of the seed solution is that the weight is more than 73%, the temperature is 40-50 ℃, the adding condition of the syrup replenishing liquid is that the weight is 73-75%, and the condition of the crystallization reaction reaches the end point is that the weight is 80-85%.

Specifically, when the brix is more than 73 percent and the temperature is 40-50 ℃, a seed crystal constant pressure funnel liquid adding valve is opened, 3-4 drops of seed crystal solution are dripped, reduced pressure distillation is continued for about 0.5h, visual inspection is carried out, the syrup is crystallized, the reading of a brix meter is 73-75 percent, a syrup supplementing liquid constant pressure funnel liquid adding valve is opened, syrup is slowly dripped for supplementing and adjusting, and the dripping speed is controlled to ensure that the reading of the brix meter is stable; in the supplementing process, the vacuum degree and the temperature change are observed, and if the vacuum degree is reduced, the vacuum stability can be maintained by replacing condensed water and other modes, so that the proper reaction temperature is ensured; visually checking the production condition of the crystal grains, wherein the reading number of the brimeter is 80% -85%, judging the reaction end point, closing the heating, opening the pressure relief port 371 for pressure relief, closing the circulating water vacuum pump 11, and closing the cooling circulating pump 41; the stirring speed is adjusted to the minimum, the sealed stirring port 378 and the discharging port 36 below the reaction kettle body 32 are opened to discharge massecuite, the material feeding port 375 is opened, and the reaction kettle body 32 is cleaned by purified water.

The present utility model is not limited to the preferred embodiments, and any equivalent embodiments which can be changed or modified by the technical content explained above can be used in other fields by those skilled in the art, but any simple modification, equivalent change and modification to the above embodiments according to the technical matter of the present utility model still fall within the scope of the technical protection of the present utility model, unless departing from the technical content of the present utility model.

Claims (9)

1. The utility model provides a medicinal sucrose production is with high-efficient crystallization device that contains thermal cycle, includes vacuum circulation subassembly (1), heating circulation subassembly (2), high-efficient crystallization subassembly (3), cooling circulation subassembly (4), snakelike backward flow condenser pipe (5) and backward flow bottle (6), its characterized in that, vacuum circulation subassembly (1) are connected with snakelike backward flow condenser pipe (5), snakelike backward flow condenser pipe (5) are connected with backward flow bottle (6), backward flow bottle (6) are connected with high-efficient crystallization subassembly (3), high-efficient crystallization subassembly (3) are connected with heating circulation subassembly (2); the serpentine reflux condenser pipe (5) is connected with the cooling circulation assembly (4).

2. The efficient crystallization device for producing medicinal sucrose containing thermal circulation according to claim 1, wherein the vacuum circulation assembly (1) comprises a circulating water vacuum pump (11) and a hose (12), one end of the hose (12) is connected with the circulating water vacuum pump (11), and the other end of the hose (12) is connected with a serpentine reflux condenser tube (5).

3. A high-efficiency crystallization apparatus for producing sucrose for pharmaceutical use with thermal cycle according to claim 1 wherein said heating cycle assembly (2) comprises a heating cycle machine (21) and a heating connection tube (22), said heating connection tube (22) being provided in two; one end of each heating connecting pipe (22) is connected with the heating cycle machine (21), and the other end of each heating connecting pipe is connected with the high-efficiency crystallization component (3).

4. A high-efficiency crystallization device for producing medicinal sucrose containing thermal cycle as in claim 3, wherein the high-efficiency crystallization component (3) comprises a rectangular support frame (31), a reaction kettle body (32), a stirring motor (33), a stirring rod (34), a reaction kettle interlayer (35) and a reaction kettle cover body (37), wherein the rectangular support frame (31) is internally connected with the reaction kettle body (32), and the reaction kettle interlayer (35) is arranged on the outer wall of the reaction kettle body (32); the top end of the reaction kettle body (32) is connected with a reaction kettle cover body (37), a stirring rod (34) penetrates through the reaction kettle cover body (37), and one end of the stirring rod (34) outside the reaction kettle body (32) is connected with a stirring motor (33); and a discharge port (36) is arranged at the bottom end of the reaction kettle body (32).

5. The efficient crystallization device for producing medicinal sucrose containing a thermal cycle according to claim 4, wherein the reaction kettle cover body (37) is provided with a decompression port (371), a condenser port (372), a brix probe port (373), a thermometer port (374), a material feeding port (375), a seed crystal feeding port (376), a syrup feeding port (377) and a sealing stirring port (378), the sealing stirring port (378) is arranged in the middle of the reaction kettle cover body (37), and the stirring rod (34) penetrates through the reaction kettle cover body (37) through the sealing stirring port (378).

6. A high-efficiency crystallization apparatus for producing sucrose for pharmaceutical use containing a thermal cycle according to claim 2 wherein said cooling cycle assembly (4) comprises a cooling cycle pump (41) and a cooling connection pipe (42), said cooling connection pipe (42) being provided with two; one end of each cooling connecting pipe (42) is connected with the cooling circulating pump (41), and the other end is connected with the serpentine return condensing pipe (5).

7. The efficient crystallization device for producing medicinal sucrose containing thermal cycle according to claim 6, wherein the serpentine reflux condenser (5) comprises a cooling liquid inlet (51), a cooling liquid outlet (52) and a vacuum pumping port (53), wherein the vacuum pumping port (53) is connected with a hose (12), and the cooling liquid inlet (51) and the cooling liquid outlet (52) are respectively connected with a cooling connecting pipe (42).

8. The efficient crystallization apparatus for pharmaceutical sucrose production with thermal cycle as defined in claim 5, wherein the decompression port (371) is connected with an exhaust valve having an opening and closing function; the condenser interface (372) is connected with a serpentine reflux condenser pipe (5) through a reflux bottle (6); the brix probe interface (373) is connected with a brix probe with a digital display function; the thermometer interface (374) is connected with a temperature probe; the seed crystal filling port (376) and the syrup filling port (377) are connected with a constant pressure funnel; the material feed opening (375) is provided with a fixable top cover.

9. The efficient crystallization device for producing medicinal sucrose containing thermal cycle as defined in claim 4, wherein the reaction kettle interlayer (35) is provided with an interlayer liquid inlet (351) located at the bottom of the reaction kettle and an interlayer liquid outlet (352) located at the middle of the reaction kettle, and the interlayer liquid inlet (351) and the interlayer liquid outlet (352) are respectively connected with the heating connecting pipe (22).