KR102433094B1 - Medication recrystallization device including glass reactor - Google Patents

Abstract

The present invention is a pharmaceutical recrystallization apparatus including a glass reactor, the glass reactor is fixed to the reactor support, agitating module for supplying a liquid or solid sample to the agitation to the glass reactor; and a controller for controlling the temperature and pressure of the glass reactor.

Description

Medicine recrystallization device including glass reactor

The present invention relates to a pharmaceutical recrystallization apparatus including a glass reactor.

In general, a chemical reactor is a device widely used in chemistry (petrochemical, fine chemistry), industrial fields, schools, pharmaceuticals, and the like, and is used as a container for reacting chemical substances.

The heating method in the conventional chemical reactor requires a circulator to circulate the heating medium as well as the heating medium 1' to transfer heat by using the jacket method when heating is desired. There was a problem that not only made the cost of the vehicle excessive, but also made the operation complicated.

In addition, the conventional sealing method by the reactor uses a sealing method by an 0-ring (0-ring). In the case of high temperature and high pressure, the reaction gas penetrates between the 0-ring and the parts adjacent thereto, and in severe cases, the reactor There was a problem in that there is a risk of damage to itself, and limits are set on the temperature and pressure of its use.

Furthermore, the conventional reactor is a method in which the reactor is fixed to the reactor support installed above, below or around the reactor in order to prevent shaking of the reactor and effectively respond to the reaction pressure. · There was a problem that was difficult to dismantle.

Korean Patent Registration No. 10-0374190

An object of the present invention is a pharmaceutical recrystallization apparatus comprising a glass reactor capable of facilitating the recrystallization reaction by increasing or decreasing the temperature as it has a wide use temperature while blocking the interaction with the reactants by making the main part of glass provides

The technical problems of the present invention are not limited to the technical problems mentioned above, and other technical problems not mentioned will be clearly understood by those skilled in the art from the following description.

A method for purifying a composition using a glass reactor according to an embodiment of the present invention comprises the steps of heating and dissolving a solid containing impurities to make a solution; limiting the upper limit of the temperature to the boiling point of the solvent and cooling the solution again; and filtering out crystals generated as the solution cools.

Pharmaceutical recrystallization apparatus including a glass reactor according to an embodiment of the present invention, the glass reactor may be fixed to the reactor support.

A pharmaceutical recrystallization apparatus including a glass reactor according to an embodiment of the present invention, a stirring module for supplying a liquid or solid sample to the glass reactor by stirring; and a controller for controlling the temperature and pressure of the glass reactor.

According to one embodiment, the glass reactor, a supply unit for supplying a sample of liquid or solid; a condensation supply unit for condensing and supplying the liquid or solid sample; a reaction unit formed of a glass material having heat resistance, pressure resistance and heat insulation properties, and performing a concentrated distillation reaction by applying heat or cooling to extract a high-purity sample from the sample supplied from the supply unit or the condensation supply unit; and a receiving unit for receiving the sample on which the concentration distillation reaction is completed in the reaction unit.

The pharmaceutical recrystallization apparatus including a glass reactor according to an embodiment of the present invention heats and melts a solid containing impurities to make a solution, limits the upper limit of the temperature to the boiling point of the solvent, cools the solution again, and the solution is By filtering out the crystals that occur as they cool, the drug recrystallization process can be carried out.

According to an embodiment, the glass reactor may be provided with a reactor tightening member positioned to surround and protect one side.

According to an embodiment, the reactor tightening member includes: a tightening unit positioned to face a fixed column located on one side of the glass reactor; a first fixing part having one end fixedly installed on the fixing column part, and the other end extending outwardly and fixed to the tightening part; a buffer member having one end inserted into the first fixing part; and a second fixing part fixed to the other end of the first fixing part to prevent separation of the buffer member and the tightening part.

According to an embodiment, the buffer member may refer to a coil spring that relieves an impact applied to the glass reactor by alleviating an impact generated from the outside.

According to an embodiment, the buffer member may contract and relax along the axial direction of the first fixing part.

According to an embodiment, the first fixing part may be formed to have a different length depending on the thickness of one side of the glass reactor.

According to an embodiment, the buffer member may be formed to have a different length depending on the thickness of one side of the glass reactor.

According to an embodiment, when the thickness of the glass reactor is relatively thick, one end of the buffer member may be inserted into the first fixing part in a long or relaxed form.

The glass reactor according to an embodiment of the present invention may be fixed to the reactor support.

Glass reactor according to an embodiment of the present invention, a supply unit for supplying a sample of liquid or solid; a condensation supply unit for condensing and supplying the liquid or solid sample; a reaction unit formed of a glass material having heat resistance, pressure resistance and heat insulation properties, and performing a concentrated distillation reaction by applying heat or cooling to extract a high-purity sample from the sample supplied from the supply unit or the condensation supply unit; and an accommodating unit accommodating the sample on which the concentration distillation reaction is completed in the reaction unit.

According to an embodiment, the reaction unit may heat or cool the sample based on a set value input through the control unit.

According to an embodiment, the control unit is located inside the opening and closing part formed of a glass plate in which the upper part of one side can be visually confirmed, and the set value is exposed so that it can be confirmed with the naked eye through the upper one side of the opening and closing part. can

According to an embodiment, the opening/closing unit may be opened in front, but an opening/closing fixing member may be provided on one side of the front side.

According to an embodiment, the opening and closing fixing member may include a fixing part fixed to a side surface of the opening and closing part; and an insertion part fixed to the fixing part with an opening/closing fixing screw so as to be detachable and attachable to the fixing part.

According to an embodiment, the fixing unit includes: a fixing plate in which a screw groove is formed so as to be in close contact with the opening and closing unit and fixed with an insertion screw; an insertion forming part for detaching and mounting the insertion part on the outer surface of the fixing plate; an insertion hole formed on the inner surface of the insertion forming unit to fit the diameter of the insertion unit so that the insertion unit is inserted through the upper and lower sides; and an opening/closing fixing groove formed in a side portion of the insertion forming part so that the opening/closing fixing screw passes through and is fastened.

According to one embodiment, the fixing plate, the inner surface may be characterized in that the fixing portion is attached to the opening and closing portion, it is characterized in that it is provided with a waterproof attachment that is adhered to block water flowing into the insertion screw.

According to an embodiment, the insertion part may be fixed in the insertion hole by the opening/closing fixing screw having an upper surface charged into the insertion hole and fastened to the opening/closing fixing groove.

According to an embodiment, the insertion unit may have a protrusion formed on one side of the upper end to be inserted into the insertion hole to prevent being charged over a predetermined length by being caught by the insertion forming unit.

According to one aspect of the present invention described above, the pharmaceutical recrystallization apparatus including the glass reactor proposed by the present invention blocks the interaction with the reactants by making the main part of glass, and at the same time has a wide use temperature. The recrystallization reaction can be facilitated by adding or subtracting.

In addition, it is possible to produce high-purity pharmaceuticals by increasing the purity of pharmaceuticals and concentrating them through recrystallization in a glass reactor made of glass.

In addition, since it is positioned to surround one side of the glass reactor, there is an advantage in that it is possible to reduce the defect rate caused by the reactor being damaged from an external impact.

In addition, it is located at the center of the reactor clamp member to absorb vibrations that may be generated from an external shock, but it is possible to protect the reactor clamp member from external impact.

The effects of the present invention are not limited to the above-mentioned effects, and various effects may be included within the range apparent to those skilled in the art from the description below.

1 and 2, and 6 to 8 are views showing the configuration of a glass reactor according to an embodiment of the present invention.
3 to 5 are views showing the configuration of a glass reactor according to another embodiment of the present invention.
9 and 10 are diagrams showing a pharmaceutical recrystallization apparatus including a glass reactor according to an embodiment of the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS [0012] DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS [0014] DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS [0016] Reference is made to the accompanying drawings, which show by way of illustration specific embodiments in which the present invention may be practiced. These embodiments are described in sufficient detail to enable those skilled in the art to practice the present invention. It should be understood that the various embodiments of the present invention are different but need not be mutually exclusive. For example, certain shapes, structures, and characteristics described herein with respect to one embodiment may be implemented in other embodiments without departing from the spirit and scope of the invention.

When a component is referred to as being “connected” or “fastened” to another component, it may be directly connected or engaged with the other component, but it is understood that other components may exist in between. it should be On the other hand, when it is mentioned that a certain element is "directly connected" or "directly fastened" to another element, it should be understood that the other element does not exist in the middle.

In addition, it should be understood that the location or arrangement of individual components within each disclosed embodiment may be changed without departing from the spirit and scope of the present invention. Accordingly, the detailed description set forth below is not intended to be taken in a limiting sense, and the scope of the present invention, if properly described, is limited only by the appended claims, along with all scope equivalents to those claimed. Like reference numerals in the drawings refer to the same or similar functions throughout the various aspects.

Hereinafter, preferred embodiments of the present invention will be described in more detail with reference to the drawings.

In general, a glass reactor is a reaction device used for organic synthesis, and has the main purpose of concentrating and distilling substances by heating or cooling the reactor.

The glass reactor according to an embodiment of the present invention may use a recrystallization method to increase the purity of the reagent.

This is a method that melts a solid sample once and catches the crystal again. Recrystallization is a method of supersaturating a substance in a solvent that dissolves the product and impurities, dissolving the impurities in the solvent, and cooling it to crystallize only high-purity substances.

More specifically, if the solid containing impurities is heated and melted and then cooled again, crystals are formed and settled, and the amount of crystals at this time can be determined by the difference in solubility between the cold temperature and the warm temperature. .

Here, the upper limit of the temperature is limited up to the boiling point of the solvent, and the lower limit is determined as necessary. The impurities in the original solid are melted into the solvent by heating and can remain dissolved even after the solution is completely cooled.

Finally, by filtering the settled crystals, crystals with high purity can be obtained.

A glass reactor and a purification method using the same will be described together with reference to the drawings to be described later.

1 and 2, and 6 to 8 are diagrams showing the configuration of a glass reactor according to an embodiment of the present invention.

1 and 2 and 6 to 8, the glass reactors 550 and 550' according to an embodiment of the present invention include a supply unit 150, a condensation supply unit 170, a reaction unit 130 and a receiving unit. part 190 may be included.

The supply unit 150 may supply a liquid or solid sample to the reaction unit 130 .

The condensation supply unit 170 may supply a liquid or solid sample by condensing, in the case of a sample to be supplied by condensing.

The reaction unit 130 may be formed of a glass material having heat resistance, pressure resistance and heat insulation properties, and concentrated distillation by applying heat or cooling to extract a high-purity sample from the sample supplied from the supply unit 150 or the condensation supply unit 170 . can react

The receiving unit 190 may receive the sample on which the concentration distillation reaction is completed in the reaction unit 130 and periodically discharge a predetermined amount.

The reaction unit 130 of the glass reactors 100 and 300 according to an embodiment of the present invention may be fixed to the reactor supports 110 and 310 .

On the other hand, the glass reactor according to an embodiment of the present invention is a reactor that promotes a chemical reaction, and may aim to obtain crystals with high purity by using a reactor in which a chemical reaction of a sample occurs.

In addition, the glass reactor according to an embodiment of the present invention may further include a temperature measuring unit and a pressure measuring unit (330, 370, 390) for measuring the temperature and pressure applied to the reactor.

Here, the temperature measuring unit and the pressure measuring unit (330, 370, 390) may be provided with an analog pressure gauge, a digital pressure sensor, a safety valve, a temperature measuring sensor, and a pressure measuring tube, but is not limited thereto. Any device for measuring temperature and pressure may be included regardless of its name.

The pressure measuring tube may be configured to enter the reactor, so that some gas inside the reactor in which a chemical reaction occurs passes through the pressure measuring tube and enters the analog pressure gauge and the digital pressure sensor to indicate the pressure.

9 and 10 are diagrams showing a pharmaceutical recrystallization apparatus including a glass reactor according to an embodiment of the present invention.

9 and 10, the drug recrystallization apparatus 500 including a glass reactor according to an embodiment of the present invention is a glass reactor (550, 550'), agitation modules (530, 530') and a controller 570 ) may be included.

Since the configuration of the glass reactors 550 and 550 ′ is described in FIGS. 1 to 5 above, a description thereof will be omitted.

The stirring module (530, 530') can supply a liquid or solid sample to the glass reactor (550, 550') by stirring, and the controller 570 is connected to one side of the glass reactor (550, 550'). The temperature and pressure of the glass reactors 550 and 550' can be controlled.

Here, the stirring modules 530 and 530' are devices for stirring and mixing gas, liquid, and solid phase substances during chemical experiments, and may refer to devices mainly used to quickly uniformly uniform components in a liquid.

The stirring module (530, 530') may be used to stir two or more different samples as a whole and to see a reaction thereto, and a motor for rotating the stirring module (530, 530') may be provided, a motor It may be formed so that the stirrer is attached to the end of the rotation shaft of the

The shape of the stirrer head (impeller) at the end of the motor shaft may be configured to vary according to the properties of the sample.

On the other hand, the stirring module (530, 530') of the present invention is characterized in that there are cases where the purpose of stirring each sample is, but in the case of stirring, the torque value of the stirring may be required.

That is, in the glass reactor proposed by the present invention, agitarion can also be carried out in parallel, and various reaction experiments such as chemical synthesis, polymerization reaction, extraction filtration, etc. can be performed in a pressure vacuum state by stirring at a constant temperature (heating/cooling). It can be studied by setting the temperature (heating/cooling) pressure vacuum stirring/dispersing speed and strength according to the desired conditions.

3 to 5 are views showing the configuration of a glass reactor according to another embodiment of the present invention.

3 and 4 , the glass reactor according to another embodiment of the present invention may be provided with a reactor tightening member positioned to surround and protect one side.

The reactor tightening member 200 may include a first fixing part 220 , a buffering member 230 , a tightening part 210 , and a second fixing part 250 .

The tightening part 210 is positioned to face the fixed column part 204 provided at one end of the glass reactors 350 and 550, but may be positioned horizontally.

The first fixing unit 220 may be configured to be inserted into both ends of the tightening unit 210 to be fixed to the fixing pillar unit 204 positioned to face the tightening unit 210 .

The first fixing part 220 may have one end fixedly installed on the fixing pillar part 204 , and the other end may be extended outwardly and fixed to the tightening part 210 .

One end of the buffer member 230 may be inserted into the first fixing unit 220 , and may be installed between one end of the first fixing unit 220 and the tightening unit 210 to provide elasticity to the tightening unit 210 . have.

The buffer member 230 may mean a coil spring, but is not limited thereto, and is a device for alleviating the shock applied to the glass reactors 350 and 550 by mitigating the shock generated from the outside, regardless of the name. can all be included.

That is, the buffer member 230 may be included regardless of its name as long as it is a device that contracts or relaxes in order to alleviate an external shock.

The other end of the first fixing part 220 may be inserted into the tightening part 210 , and the buffer member 230 may contract and relax along the axial direction of the first fixing part 220 by elasticity.

One side of the glass reactors 350 and 550 may be located in the inner space formed by the fixed pillar 204 , the first fixing unit 220 and the tightening unit 210 .

The first fixing part 220 and the buffer member 230 may be formed to have different lengths depending on the thickness of one side provided in the glass reactors 350 and 550 .

That is, when the thickness of the glass reactors 350 and 550 is relatively thick, the first fixing part 220 may have a wide spacing between the fixing pillars 204 and the tightening part 210, and the glass reactor 350 When the thickness of the , 550 is relatively thin, the interval between the fixed pillars 204 and the tightening portion 210 may be narrowed.

In addition, when the thickness of the glass reactors 350 and 550 is relatively thick, the length of the buffer member 230 may be long or one end may be inserted into the first fixing part 220 in a relaxed form.

The second fixing part 250 may be fixedly installed at the other end of the first fixing part 220 to prevent separation of the buffer member 230 and the tightening part 210 .

Referring to FIG. 5 , the buffer member 230 according to another embodiment of the present invention may include a frame portion 231 , a spring portion 232 , a first fixing portion 233 , and an opening portion 234 . have.

The frame portion 231 may be formed in a cylindrical or rectangular shape, and may be formed in a shape with an empty interior.

The spring part 232 is mounted in the frame part 231, and when the second fixing part 235 is inserted into the opening part 234, it descends from the top to the bottom by the action of the spring part 232, so that the vibration is absorbed. First, it may be absorbed by the spring part 232 .

Even if there is an aftershock, the vibration may not be transmitted to the outside of the reactor tightening member 200 by being absorbed once again by the first fixing part 233 fixed to the top of the table.

The frame portion 231 may be formed with a diameter within which the spring portion 232 can be located, and the spring portion 232 is inserted into the frame portion 231 through the opening 234 formed at the top. can be located.

In addition, the material of the frame part 231 may be formed of hard rubber or plastic, but is not limited thereto. It is located in the center of the reactor clamping member 200 to absorb vibrations that may occur from an external shock, but the reactor clamping member (200) Any material that can protect it from external impact may be included regardless of its name.

On the inner upper side of the opening 234 located at the upper end of the frame part 231 , an upper screw part 236 may protrude and be formed in the shape of a screw thread, and a lower screw part formed on the lower exterior of the second fixing part 235 . It may be formed to correspond to the shape of the lower screw portion 237 so as to be screwed into and fitted with the 237 .

That is, after the lower screw part 237 rotates the upper screw part 236 and passes through the upper screw part 236 , it can freely move up and down in the inside of the frame part 231 .

The second fixing part 235 can be prevented from falling out from the inside of the frame part 231 through the top screw part 236 formed to protrude from the top.

On the other hand, in the buffer member 230 according to another embodiment of the present invention, a sponge may be laminated between the bottom of the frame part 231 under the spring part 232 in order to increase the buffer effect.

The above-described embodiments are for illustration, and those of ordinary skill in the art to which the above-described embodiments pertain can easily transform into other specific forms without changing the technical idea or essential features of the above-described embodiments. You will understand. Therefore, it should be understood that the above-described embodiments are illustrative in all respects and not restrictive. For example, each component described as a single type may be implemented in a dispersed form, and likewise components described as distributed may also be implemented in a combined form.

The scope to be protected through the present specification is indicated by the following claims rather than the detailed description, and it should be construed to include all changes or modifications derived from the meaning and scope of the claims and their equivalents.

100, 300: glass reactor
500: drug recrystallization device including a glass reactor

Claims (4)

In the pharmaceutical recrystallization apparatus comprising a glass reactor, the glass reactor is fixed to the reactor support,
The glass reactor,
A reactor tightening member is provided to surround and protect one side,
The reactor tightening member,
a tightening part positioned to face the fixed column part positioned on one side of the glass reactor;
a first fixing part having one end fixedly installed on the fixing column part, and the other end extending outwardly and fixed to the tightening part;
a buffer member having one end inserted into the first fixing part; and
and a second fixing part fixed to the other end of the first fixing part to prevent separation of the buffer member and the tightening part;
The buffer member,
It means a coil spring that relieves the shock applied to the glass reactor by mitigating the shock generated from the outside,
The buffer member,
contraction and relaxation along the axial direction of the first fixing part;
The first fixing part,
The length is formed differently depending on the thickness of one side of the glass reactor,
The buffer member,
The length is formed differently depending on the thickness of one side of the glass reactor,
The buffer member,
When the thickness of the glass reactor is relatively thick, one end is inserted into the first fixing part in a long-formed or relaxed form, a pharmaceutical recrystallization apparatus comprising a glass reactor. According to claim 1,
a stirring module for stirring a liquid or solid sample and supplying it to the glass reactor; and
Including; a controller for controlling the temperature and pressure of the glass reactor;
The glass reactor,
a supply unit for supplying a liquid or solid sample;
a condensation supply unit for condensing and supplying the liquid or solid sample;
a reaction unit formed of a glass material having heat resistance, pressure resistance and heat insulation properties, and performing a concentrated distillation reaction by applying heat or cooling to extract a high-purity sample from the sample supplied from the supply unit or the condensation supply unit; and
A pharmaceutical recrystallization apparatus comprising a glass reactor, including; an accommodating part for accommodating the sample on which the concentration distillation reaction is completed in the reaction part. The method of claim 1,
A glass reactor that heats and melts a solid containing impurities to make a solution, limits the upper limit of the temperature to the boiling point of the solvent, cools the solution again, filters the crystals generated as the solution cools, and performs a pharmaceutical recrystallization process. Drug recrystallization device comprising.

delete

Images