KR101883440B1

KR101883440B1 - A reactor for crystallization

Info

Publication number: KR101883440B1
Application number: KR1020160014431A
Authority: KR
Inventors: 박용묵
Original assignee: 웰이앤씨 주식회사
Priority date: 2016-02-04
Filing date: 2016-02-04
Publication date: 2018-07-31
Also published as: KR20170093015A

Abstract

The present invention relates to a crystallization reactor capable of repeatedly performing rapid temperature raising and cooling of a thermal characteristic in one reactor to induce supersaturation and maximize the metastable state of crystals to obtain crystallized materials of a desired size and shape continuously .
The present invention relates to a reactor comprising a reactor body in which water, a reactant, a solvent and an antisolvent are incorporated; A jacket installed on an outer surface of the reactor body for receiving a heating medium and raising a reaction material to a predetermined temperature; An impeller installed in the reactor body and performing a stirring function to mix water, a reaction material and a solvent; A pump positioned at the upper end of the impeller and sucking the agitated reaction material; A spray nozzle mounted on an outer circumferential surface of the pump for spraying the reaction material sucked into the pump into the reactor body; And cooling means installed at the lower end of the atomizing nozzle for cooling the reaction material sprayed from the atomizing nozzle.

Description

A reactor for crystallization < RTI ID = 0.0 >

The present invention relates to a crystallization reaction apparatus used in a chemical reaction crystal and a chemical reaction crystal process during protein crystal synthesis, and more particularly to a crystallization reaction apparatus which repeatedly performs heating and cooling in a single reactor, The present invention relates to a crystallization apparatus capable of maximizing a metastable zone in a supersaturation reaction product to obtain crystals of a desired size and shape.

In general, the material industry has been given research papers and patents on reactors that perform various chemical synthesis, biosynthesis, and chemical reaction processes. However, it is often confined to a specific reaction process, and the design of the crystallization tank is insignificant.

In the Material Industry or Pharmaceutical Industry, Reactor and Crystallizer Tank have various Reactive Factors such as heating and stirring to improve reaction and crystal efficiency. Change it. Depending on the reaction conditions, the temperature can be controlled by a jacket. By varying the stirring speed and the shape of the stirrer according to the contents, the characteristics and applications of the reaction can be diversified. In addition, for the special purpose reaction, maximizing the sealing effect and selecting the impeller suitable for the application characteristics, maximizing the reaction and stirring effect, or varying the RPM and stirring blade by using the mixing device depending on the type of reactant have. Also, the reactor is designed to freely control the reaction rate and the environment.

The production of crystallized particles using most of the reactors proceeds through the course of reaction-crystallization-filtration-drying-pulverization, and is obtained by using a post-crystallization process. As a crystallization method using a reactor, an evaporative crystallization method is known in which a solvent is evaporated to crystallize or crystallized by increasing the concentration of a substance. In the case of a conventional evaporative crystallizer used in this evaporative crystallization method, The solvent is evaporated in the inside to induce the degree of supersaturation.

Reactors commonly used in the crystallization process are those in which crystals are precipitated by using the polarity of the reaction liquid and the solvent, or heated and cooled by using the attractive force of van der Waals force of the crystal molecules, Crystallization material can be made and filtered to obtain crystals. However, this general reactor has a problem that it is difficult to control the degree of supersaturation. That is, in order to control the degree of supersaturation of a solution using a conventional evaporation crystallization method reactor, it is impossible to perform a rapid temperature change. Therefore, it is possible to repeatedly perform the heating and cooling by using a plurality of reactors. In this case, the precipitation method and the cost of the crystal increase (more than 2 times), resulting in an inefficiency due to an increase in production cost.

As a continuous stirred tank type reactor for performing the crystallization process, there is a mixed suspension and mixed product removal (MSMPR) reactor. However, in the case of the MSMPR reactor, the size of the particles increases with increasing agitation speed in the agitator, and may occur locally irregularly in the solution as the agitator rotates. As a result, the size distribution of the particles is relatively wide according to the change of the supersaturation degree of the solvent, so that the uniformity can not be guaranteed.

As a process system for carrying out the crystallization of a reactant, a continuous lupturing crystallization separator of Patent No. 10-0733957 is disclosed, and the construction thereof will be briefly described with reference to FIG.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a block diagram showing a conventional continuous lignite crystallization separation process system according to the prior art; FIG.

In the continuous batch crystallization process system shown in FIG. 1, after the reaction material is introduced into the first stirrer 120 and the solvent is introduced into the second stirrer 130, stirring is sufficiently performed through the operation of the stirrer 110 . The reactants and the solvent stirred in the first and second stirrers 120 and 130 are introduced into the Kuett-Taylor reactor 150 and reacted by rotation of the rotating rod mounted in the quartetailer reactor 150 The crystallization process of the material is performed. The crystallized material in the Kuett-Taylor reactor 150 is subjected to a series of processes for separating the liquid and the crystallized material through the solid-liquid separator 160.

Reference numeral 140 denotes a liquid pump, 170 denotes a pH meter, 180 denotes an electron microscope, and 190 denotes a particle size analyzer.

As described above, the conventional continuous crystallization reactor can not control the particle size because the size of the particles is determined according to the rotation speed of the rotating bar of the quartetailer, and the reaction with the solvent to induce the crystallization of the reaction material, The cooling rate can not be controlled and it is difficult to obtain desired crystal grains.

Another conventional reactor structure for obtaining a crystallization material is shown in Fig. The crystallization reaction system shown in FIG. 2 relates to an apparatus for chemical recycling of peroxide disclosed in Korean Patent No. 10-1386683.

As shown in the drawing, the system includes a first reactor 200 in which a glycolysis reaction takes place using a raw material supplied from a raw material feeder 210; A second reactor (300) for subjecting the product of the first reactor (200) to methanoldisis reaction; A rectification tower 400 separating the methanol discharged from the upper end of the second reactor 300 by direct contact with the liquid at the lower end of the rectification column to separate and separate the methanol and recycle it into the second reactor 300 in the vapor phase; And a crystallization tank 500 for cooling the outer wall surface by the heat insulating material, forced cooling by the fan, and cooling by the cooled methanol to crystallize dimethyl phthalate from the liquid phase at the lower end of the rectification column 400. The internal gas of the crystallization tank 500 is forcibly passed through the condenser by the fan, cooled, and then introduced into the crystallization tank.

Such a separation type reaction tank can not control the stirring speed and the cooling temperature arbitrarily, so that it can not be produced by adjusting the desired size or shape.

As described above, the prior art does not disclose techniques for digesting reactions of various kinds and capacities into one reactor. Particularly, it is very difficult to make a reaction to obtain the crystallization material suitable for the purpose in the production facility site. Therefore, there is a case that a laboratory or a simple reaction tank is used, and thus the quality is not guaranteed and the efficiency is deteriorated.

SUMMARY OF THE INVENTION Accordingly, the present invention has been made in view of the above problems, and it is an object of the present invention to provide a method and apparatus for continuously heating and cooling a thermal characteristic in a single reactor to induce supersaturation, And to provide a crystallization reaction apparatus capable of obtaining a crystallization material in the form of crystals.

In order to accomplish the above object, the present invention provides a method of manufacturing a semiconductor device, including: a reactor body in which water, a reactant, a solvent, and an antisolvent are embedded; A jacket installed on an outer surface of the reactor body for receiving a heating medium and raising a reaction material to a predetermined temperature; An impeller installed in the reactor body and performing a stirring function for mixing the reaction material and the solvent; A pumping unit positioned at the upper end of the impeller for sucking the agitated reaction material; A spray nozzle mounted on an outer circumferential surface of the pumping unit for spraying the reacted reactant into the reactor body; And a cooling unit installed at a lower end of the spray nozzle for cooling a reaction material sprayed from the spray nozzle.

In an embodiment of the present invention, the cooling means may be arranged in a zigzag fashion up and down, and may be a heat exchange plate through which coolant flows in and out. In another embodiment, the cooling means may be wound on the outer circumferential surface, and may be formed of a heat exchange coil through which refrigerant flows in and out.

As described above, the present invention has the following effects.

First, by repeating the process of heating the reaction material that performs the chemical reaction at a certain temperature through the jacket, and also by sucking the reactant using the pumping unit and contacting the cooling heat exchanger, The metastable region can be expanded to produce a crystallized material having a desired size and shape.

Second, the heating and cooling of the reaction material can be repeated using a single reactor, which can improve the production efficiency of the crystallization material and enable high-cleanliness product management (GMP) required in pharmaceutical products.

Third, the size and shape of the crystallization material can be adjusted as required by the user by observing the growth process of the crystal grains through the spectroscope.

Fig. 1 and Fig. 2 are a schematic configuration diagram of a chemical reactor according to the prior art,
3 is a structural view showing a first embodiment of the crystallization reactor according to the present invention,
4 is a structural view showing a second embodiment of the crystallization reactor according to the present invention,
5 is a graph of the solubility curve showing the relationship between the concentration and the temperature.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings of FIGS. 3 to 5. FIG.

The crystallization reactor according to the present invention can be used in a metastable (metastable) state by inducing super saturation through thermodynamic, unsaturated or under-saturated processes using a single reactor Metastable) and the unstable state of Labile are maximized to produce crystallized materials of desired size and shape. Here, the thermodynamic method refers to maximizing the metastable zone by quickly heating the reactants and rapidly cooling them.

3 is a schematic cross-sectional view showing a configuration of a first embodiment of the crystallization reactor according to the present invention.

In the first embodiment of the present invention, a reactor body 2 in which water, a reactant and a solvent, and an antisolvent are contained; A jacket 4 installed on the outer surface of the reactor body 2 for raising a reaction material to a predetermined temperature; An impeller (6) installed in the reactor body (4) and performing an aberration function while stirring to mix water, a reaction material and an antisolvent; A pumping unit (8) having a cylinder structure for pumping reaction material placed at the upper end of the impeller (6) and stirring the reaction material; A motor 10 connected to an upper portion of the pumping unit 8 and providing a rotational force for allowing the pumping unit 8 to suck the reactive material; A spray nozzle 12 mounted on an outer circumferential surface of the pumping unit 8 for spraying the reaction material sucked into the pumping unit 8 back into the reactor body 2; And a heat exchange plate (14) installed at the lower end of the atomizing nozzle (12) for cooling the reaction material sprayed from the atomizing nozzle (12); A chiller 16 connected to the heat exchange plate 14 to supply a coolant such as cooling water or a brain to the heat exchange plate 14; A TCU (18) for supplying a heating medium roll to the jacket (4) to perform heat exchange with a reaction material inside the reactor body (2); A spectroscope (ATR FTIR) 22 connected to the reactor body 2 for monitoring the crystallization form of the growing reactant while repeating heating and cooling; A solid-liquid separator 24 for separating and discharging the crystallization material and the solvent branched from the reactor body 2 by branching to the crystallization material discharge pipe 24a and the solution discharge pipe 24b at the lower end of the reactor body 2, ).

In the above-described first embodiment, the heat exchange plates 14 are arranged in a zigzag fashion up and down, and the refrigerant flows in and out. Therefore, the reactive material sprayed from the spray nozzle 10 in a sprayed state is brought into contact with the upper surface of the heat exchange plate 14 and flows downwardly while being sufficiently cooled through the zigzag shape. By repeating such cooling and heating, Crystallized material having a size of 1 to 5 mu m.

In the second embodiment of the present invention, instead of the heat exchange plate 14, the heat exchanging coil 20 may be wound around the outer circumferential surface of the pump 8 and through which the refrigerant flows.

The crystallization method of the present invention constituted as described above will be described.

First, in the present invention, water and a reactant are introduced into the reactor body 2, and a solvent and an antisolvent are introduced to induce a crystallization reaction of the reactant.

When a heating medium having a predetermined temperature is supplied from the TCU 18 to the jacket 4 to obtain crystal grains of the reaction material, the heating medium circulating through the jacket 4 is heat-exchanged with the reaction material in the reactor body 2, The temperature of the reactant increases. In the present invention, the reaction material and the solvent are heated by raising the temperature to about 100 ° C. After the impeller 6 is rotated by the operation of the motor 10, the reaction material and the semi-solvent are stirred, and the stirred reaction material is sucked through the pumping unit 8 and introduced into the spray nozzle 10. At this time, refrigerant of 0 ° C is supplied to the heat exchange plate 12 through the chiller 16.

The spray nozzle 12 rotates while spraying the reaction material. The sprayed reaction material is cooled while being heat-exchanged with the refrigerant passing through the heat exchange plate 14, and flows to the lower portion of the reactor body 2. That is, since the heat exchange plate 14 is installed in a zigzag shape, the reaction material naturally falls and sufficiently cooled over the area of the heat exchange plate 12.

As another example, as shown in Fig. 4, in the case of the heat exchange coil 18 instead of the heat exchange plate 12, the reaction material sprayed from the spray nozzle 10 flows down the coil to cool down by heat exchange.

In the course of repeating heating and cooling of the reaction material as described above, phase equilibrium is obtained to obtain crystallized particles having a desired shape and size.

That is, by repeating heating and cooling of the reaction material, the solubility curve graph of FIG. 5 is obtained by using the thermodynamic method, the strength of the van der Waals force, the polarity of the solvent and the antisolvent, And maximizes the metastable region (Metastable region) and the unstable state (Labile) to derive desired crystals by inducing supersaturation as shown in Fig. This process can be confirmed by analysis through the spectroscope 22.

In the graph of FIG. 5, the stable zone is an area where crystals can not be precipitated, and the metastable zone (MSZ) and Labile mean zones where crystals can be precipitated . Supersatuation or labile refers to the presence of a substance in a non-equilibrium state beyond the limit of supersaturation. For example, since supersaturation is a metastable state, the system is allowed to stand for a long time, or when an impact is applied, crystals precipitate, or water vapor coagulates, and the state of phase equilibrium is reached and stabilized.

After the elution is completed, the crystalline material and the liquid are separated and discharged through the solid-liquid separator 24 provided at the lower end of the reactor body 2.

The specific embodiments of the present invention have been described above. It is to be understood, however, that the scope and spirit of the present invention is not limited to these specific embodiments, and that various modifications and changes may be made without departing from the scope of the present invention. If you are a person, you will understand.

Therefore, it should be understood that the above-described embodiments are provided so that those skilled in the art can fully understand the scope of the present invention, and are therefore to be considered in all respects as illustrative and not restrictive, The invention is only defined by the scope of the claims.

2: Reactor body 4: Jacket
6: impeller 8: pumping unit
10: Motor 12: Spray nozzle
14: heat exchange plate 16: chiller
18: TCU 20: heat exchange coil
22: spectroscope 24: solid-liquid separator

Claims

A reactor body in which water, a reactant, a solvent and an antisolvent are contained;
A jacket installed on an outer circumferential surface of the reactor body for supplying the heat medium to the reaction material and raising the reaction material to a predetermined temperature;
An impeller installed in the reactor body and performing a stirring function for mixing water, a reaction material, a solvent, and an anti-solvent;
A pumping unit positioned at the upper end of the impeller and sucking the agitated reaction material;
A spray nozzle mounted on an outer circumferential surface of the pumping unit for spraying the reaction material sucked into the pumping unit back into the reactor body; And
And a cooling means installed at a lower end of the atomizing nozzle for cooling the reaction material sprayed from the atomizing nozzle.

The method according to claim 1,
Further comprising a spectroscope for monitoring the size and shape of the crystallized particles of the growing reactant while repeating heating and cooling in the reactor body.

The method according to claim 1,
And a solid-liquid separator provided at the lower end of the reactor body for separating and discharging the crystallization material and the solvent.

4. The method according to any one of claims 1 to 3,
Wherein the cooling means is arranged in an up-and-down zigzag manner and is made of a heat exchange plate through which coolant flows.

4. The method according to any one of claims 1 to 3,
Wherein the cooling means is wound around the outer circumferential surface of the pumping unit and comprises a heat exchange coil through which the coolant flows.