KR100733969B1 - Apparatus of separating operation on crystallization over continuous drowning-out - Google Patents

Abstract

The present invention uses a Kuet-Taylor reactor that can be treated with a small capacity reactor, and saves energy by changing the concentration of the raw material, the residence time, the mixing speed, and the size of the inner and outer cylinders in order to uniformly purify the raw material solution. And relates to a continuous molten (outrowing-out) crystallization separation device that can improve the productivity,

The present invention is provided with a stirring rod 110, the raw material therein (for example, ethyl cellulose (ethyl cellulose) solution, potassium sulfate solution, potassium chloride solution, potassium phosphate (Disodium sulfate) A first stirrer (120) containing a solution, a sodium hydroxide solution, a GMP (sodium guanylate) solution, an IMP (sodium inosinate) solution, a MSG (sodium glutamate) solution, and the like; A second stirrer (130) having a stirring rod (110) therein and containing a solvent (Anti-solvent) therein; Kuet-Taylor reactor 150 that receives the material and the solvent combined between the outer cylinder 151 and the rotating rod 153 to change the rotational speed of the rotating rod to generate turbulence to provide stability of the fluid and to produce a crystallized material )Wow; It consists of a liquid pump 140 for adjusting the flow rate to inject a constant flow rate of the two feed solutions into the Kuet-reactor to introduce the raw material and the solvent.

Description

Continuous molten crystallization separator {APPARATUS OF SEPARATING OPERATION ON CRYSTALLIZATION OVER CONTINUOUS DROWNING-OUT}

1 is a process chart showing a purification process of a conventional nucleic acid-based raw material

Figure 2 is a block diagram showing the configuration of a conventional MSMPR reactor

3 is a block diagram of a continuous molten-out crystallization separation apparatus of the present invention

Figure 4 is an embodiment of the crystallization (Drowning-out)

FIG. 5 is a flow diagram of the Cuette-Taylor reactor of FIG.

6 is a detailed cross-sectional view of the Kuet-Taylor reactor of FIG.

<Explanation of symbols for the main parts of the drawings>

110: stirring rod 120: first stirrer
130: second stirrer 140: liquid pump
150: Kuet-Taylor reactor 151: outer cylinder
152: Taylor vortex 153: rotating rod
154, 155, 156, 157, 158: Inlet 159: Drain

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160: solid-liquid separator 170: pH meter
180: electron microscope 190: particle size analyzer

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The present invention relates to a continuous drowning-out crystallization separator, and more particularly, to a material that requires purification using a continuous Kuet-Taylor reactor, a solution and a solvent are introduced into the reactor and generated by rotation of the reactor. The present invention relates to a continuous drowning-out crystallization separation device that improves purity, saves energy and improves production efficiency of crystalline materials by separating crystalline and crystallized materials.

In general, nucleic acid-based materials that are frequently used in the food industry are not only stable supply of inexpensive raw materials but also cost reduction in production. The products in the food field are expensive and diverse in nature, and are characterized by producing several substances in one reactor. Batch processes are most commonly used to produce a variety of materials. In the case of a batch process, productivity is low due to long operating time, and the operation cost per production is high due to low operating efficiency. As such, domestic companies are also making efforts to reduce manufacturing costs through process improvement or yield expansion.

As one of the efforts, as shown in FIG. 1, the first purification process of the crystallization raw material currently uses many ion exchange resin processes, and the use thereof is a process of removing ionic impurities by adsorbing the crystallization raw material to the ion exchange resin. to be. The primary and secondary crystallization processes to improve the purity of the crystallization raw material is a process of depositing crystals through the drowning-out crystallization process method of a batch reactor.

However, the above structure is, firstly, to recrystallize the solution from which impurities are removed by the crystallization process. The batch reactors currently used are expensive to manufacture equipment, have high energy cost, are impossible to produce uniform particles, and are incombustible. There is a limitation. In addition, when a large amount of solvent is added during the crystallization process, and the crystal grain size is small or amorphous depending on the purity, a high efficiency crystallization separation process system is required due to an increase in working time or separation of subsequent separation processes. to be.

In order to improve the above problems, the continuous reactor can improve production efficiency because the reaction time and introduction time are very small compared to the mixing time. Prior studies of the continuous crystallization process have used a mixed suspension and mixed product removal (MSMPR) reactor, which is a continuous stirred tank type reactor. In the MSMPR reactor, the increase in the stirring speed in the stirrer increases the size of the particles, which may occur locally in the solution as the stirrer rotates, and thus the size distribution of the particles becomes relatively large as the solvent supersaturation changes. Will appear.

The disadvantages of MSMPR reactors are that they do not have a high energy reduction rate compared to batch reactors, and because of the uneven particle size distribution, the process efficiency is reduced to make high purity materials, and there are few commercialization cases.

The present invention has been made to solve the above problems, the object is that the production efficiency is higher than the MSMPR reactor Kuet-Taylor reactor that can be processed in a small capacity reactor is a raw material for uniform purification of the solution and solvent The present invention provides a continuous drowning-out crystallization separation device that can improve energy saving and productivity by changing the concentration, stirring time, mixing speed, and size of inner and outer cylinders.
Features of the present invention for achieving the above object,
A stirring rod 110 is provided, wherein a raw material (for example, ethyl cellulose solution, potassium sulfate solution, potassium chloride solution, potassium phosphate solution, and hydroxide therein) (Sodium hydroxide) solution, GMP (sodium guanylate) solution, IMP (sodium inosinate) solution, MSG (sodium glutamate) solution, and the like;
A second stirrer (130) having a stirring rod (110) therein and containing a solvent (Anti-solvent) therein;
Kuet-Taylor reactor 150 that receives the material and the solvent combined between the outer cylinder 151 and the rotating rod 153 to change the rotational speed of the rotating rod to generate turbulence to provide stability of the fluid and to produce a crystallized material )Wow;
It consists of a liquid pump 140 for adjusting the flow rate to inject a constant flow rate of the two feed solutions into the Kuet-reactor to introduce the raw material and the solvent.

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은 상기 회전봉(153)의 반지름을 나타내고, R

는 상기 외부원통(151)의 반지름을 나타내고, d 는 상기 원료 및 용매가 위치한 곳을 나타낸 다.
한편, 상기와 같이 입구(154)로 원료가 주입되고, 입구(155)로 용매가 주입되면, 상기와 같이 구성된 쿠에트-테일러 반응기(150)는 외부원통(151)과 회전봉(153) 사이로 유체가 흐르게 되고, 상기 직류전동기 즉, 모터(부호 미도시)가 구동되어 상기 쿠에트-테일러 반응기(150)의 회전봉(153)이 회전함에 따라 축 방향을 따라 테일러 와류(152)들이 형성된다.
상기와 같이 회전봉(153)이 회전함에 따라 테일러 와류(152)가 형성되고, 상기 쿠에트-테일러 반응기(150)의 상부 부분에 다수개로 구성된 입구(156, 157, 158)에 의해 상기 테일러 와류(152)에 의해 유입된 두 물질의 결정화 여부를 샘플형태로 확인할 수 있다.
한편, 상기의 입구(156, 157, 158)에 의해 측정, 확인된 유입 두 물질의 결정화 여부에 따라 해당 결정화된 물질을 상기 쿠에트-테일러 반응기(150) 외부로 유출하는 배수구(159)를 나타내는데, 상기 배수구(159)에 의해 유출된 결정화된 물질은 고-액 분리기(160)로 전송되어 보관된다.Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Figure 3 shows a block diagram of a continuous drowning-out crystallization separation apparatus of the present invention, Figure 4 shows an embodiment of the drowning-out crystallization. FIG. 5 shows the flow pattern of the Kuet-Taylor reactor of FIG. 3, and FIG. 6 shows a detailed cross-sectional view of the Kuet-Taylor reactor of FIG. 3.
Looking at the configuration of the present invention with reference to Figure 3, reference numeral 120 is a first stirrer having a stirring rod 110, a raw material (for example, ethyl cellulose) in the interior of the first stirrer 120 Solution, Potassium Sulfate Solution, Potassium Chloride Solution, Potassium Phosphate Solution, Sodium Hydroxide Solution, GMP (Sodium Guanylate) Solution, IMP (Sodium Inosinoate) Solution, MSG (Sodium Glutamate) ) Solution, etc.).
In addition, reference numeral 130 denotes a second stirrer having a stirring rod 110, and contains methanol, an anti-solvent, in the second stirrer 130.
Here, the solvent may be applied variably according to the raw material, it may be used as an alcohol-based organic material.
The alcohol-based organic compound represents a compound in which a hydrogen atom of a hydrocarbon is substituted with a hydroxyl group -OH, and may be selectively used among ethanol, butanol, propanol, propanol, hexanol, and pentanol. Can be.
On the other hand, reference numeral 150 denotes a Kuet-Taylor reactor, which changes the rotational speed of the rotating rod therein to generate turbulence to provide stability of the fluid.
In addition, reference numeral 140 denotes a liquid pump that adjusts the flow rate so as to inject a constant flow rate of the two feed solutions into the Kuet-Taylor reactor 150 in order to introduce the raw material or the solvent into the Kuet-Taylor reactor 150. 160 represents a solid-liquid separator separating liquid from the crystallized material obtained from the Kuet-Taylor reactor 150, and 170 represents an ion concentration of the crystallized material obtained from the Kuet-Taylor reactor 150. The pH meter which measures is shown.
In addition, reference numeral 180 denotes an electron microscope capable of attaching the crystallized material obtained from the solid-liquid separator 160 to the stage using conductive carbon tape to analyze the shape and size of individual particles, and 190 denotes a particle size. As an analyzer, it sprays particles using ultrasonic waves from the material obtained from the solid-liquid separator 160 to determine the size of the agglomerated crystals.
The particle size analyzer 190 uses ultrasonic waves, and the crystals are aggregated due to physical weak attraction, so that the particle size is analyzed every minute, and after a specific time, there is no further change in the particle size or is combined with a strong force. Agglomerates are not separated by ultrasound, so the size of the aggregated crystals can be measured.
Figure 4 shows one embodiment of the drowning-out crystallization, Drowning-out crystallization is a separation by the addition of a third material having a separation effect, compared to other crystallization techniques that rely on evaporation or temperature change, but heat-sensitive material, Its solubility is particularly suitable for the separation of substances that are not highly dependent on temperature, and thus are widely used in the fine chemical, food, pharmaceutical and biochemical industries. The components used as external materials in drowning-out crystallization are gases, liquids, supercritical fluids or solids, which are used as antisolvent, diluent, drowning-out agents, precipitant, salting-out, solventing-out, or watering-out agents. . It is well soluble in water, but in organic solvents such as alcohol, the solubility is remarkably reduced, and the process of precipitating separation by adding an external substance alcohol to the crystallization target solution is widely used.
Figure 5 shows the internal flow form of the Kuet-Taylor reactor of Figure 3, each configuration and operation first, the raw material (for example, ethyl cellulose solution, potassium sulfate (potassium) to the first stirrer 120 add sulfate solution, potassium chloride solution, potassium phosphate solution, sodium hydroxide solution, GMP (sodium guanylate) solution, IMP (sodium inosinate) solution, MSG (sodium glutamate) solution, etc. After the solvent is introduced into the second stirrer 130, the first stirrer 120 and the second stirrer 130 are driven. Accordingly, the raw materials are well mixed in the first stirrer 120, and the solvent is well mixed in the second stirrer 130.
Then, the raw material and the solvent are put into the Kuet-Taylor reactor 150 through the liquid pump 140. At this time, the Kuet-Taylor reactor 150 is largely divided into a fixed outer cylinder 151 and a rotating rod 153 that can be rotated by a motor. The raw material is a liquid pump as shown in FIG. 6. It is discharged to the inlet 154 of the outer cylinder 151 through the 140, the solvent is discharged to the inlet 155 of the outer cylinder 151 through the liquid pump 140, as shown in FIG. .
In addition, the material of the outer cylinder 151 and the rotating rod 153 may be selectively used as acrylic or stainless steel according to those skilled in the art.
Fluid flowed between the outer cylinder 151 and the rotating rod 153, and was installed horizontally to reduce the influence of the pressure change.
In addition, the power required to rotate the rotating rod 153 uses a DC motor (not shown), that is, a motor, and adjusts the rotation speed by using a DC voltage regulator (not shown).
In addition, a plurality of inlets 156, 157, 158 are further provided on the outer circumferential surface of the outer cylinder 151.
In the Kuet-Taylor reactor 150 configured as described above, as the rotating rod 153 rotates when the fluid flows, a Taylor vortex 152 is formed along the rotating rod 153 direction.
On the other hand, the rotating rod 153 can be configured variably according to those skilled in the art, can be used by appropriately changing according to the raw material and the solvent to be introduced.
Thus, the Kuet-Taylor flow can easily generate turbulence by varying the rotational speed of the rotating rod and thus utilize the stability of the fluid.
6 shows a detailed cross-sectional view of the Kuet-Taylor reactor of FIG. 3. Looking at the configuration and operation of the reactor, reference numeral 154 denotes a constant flow rate of the raw material contained in the first stirrer 120 by the operation of the liquid pump 140. As shown in the inlet to be supplied into the Kuet-Taylor reactor 150, 155 is the Kuet-Taylor reactor 150 at a constant flow rate by the operation of the liquid pump 140, the solvent contained in the second stirrer 130 Inlet is supplied to the inside, wherein each of the liquid pump 140 controls the flow rate flowing into the Kuet-Taylor reactor 150.
R in the accompanying drawings

Represents the radius of the rotating rod 153, R

Denotes the radius of the outer cylinder 151, and d denotes where the raw material and the solvent are located.
On the other hand, when the raw material is injected into the inlet 154 as described above, and the solvent is injected into the inlet 155, the Kuet-Taylor reactor 150 configured as described above is the fluid between the outer cylinder 151 and the rotating rod 153 When the direct current motor, that is, the motor (not shown) is driven to rotate the rotary rod 153 of the Kuet-Taylor reactor 150, Taylor vortices 152 are formed along the axial direction.
As the rotating rod 153 rotates as described above, a Taylor vortex 152 is formed, and the Taylor vortex is formed by a plurality of inlets 156, 157, and 158 formed at an upper portion of the Kuet-Taylor reactor 150. The crystallization of the two substances introduced by 152) can be confirmed in the form of a sample.
On the other hand, according to the inlet (156, 157, 158) shows the drain outlet 159 that outflows the crystallized material to the outside of the Kuet-Taylor reactor 150 according to the crystallization of the two inlet materials measured and confirmed The crystallized material discharged by the drain 159 is sent to the solid-liquid separator 160 for storage.

The present invention is not limited to the embodiments described above, and various modifications and changes can be made by those skilled in the art, which are included in the spirit and scope of the present invention as defined in the appended claims.

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As discussed above, the continuous drop-out crystallization separator according to the present invention uses a Kuet-Taylor reactor that can replace the conventional batch and MSMPR continuous reactors to purchase cheap solvents according to the purification capacity. It can be used to reduce the cost and to produce a raw material with a constant particle size distribution, thus enabling a highly efficient continuous process.

In addition, the Kuet-Taylor reactor can be applied not only to food but also to medicine and fine chemical industry, where small amounts of customized crystallization processes are applied. Therefore, it is possible to grow economically and industrially, and maximize the ripple effect of the industry. have.

In addition, the continuous crystallization separation process can be improved to achieve energy reduction effect and import reduction effect, and when applied to GMP, IMP, MSG, etc. of nucleic acid series used as food, it can obtain even greater energy reduction effect. Extending the product to the field can also achieve significant energy savings nationally.

In addition, by using crystallization technology through Kuet-Taylor reactor, it is possible to commercialize energy-saving continuous crystallization separation process and to improve the demonstration technology, and to improve product productivity by reducing manufacturing cost, water cost, power cost and raw material cost. In addition, it is possible to compact the device by a continuous process design and to recrystallize to a uniform particle size, thereby replacing and improving the existing high energy and low efficiency separation process.

In addition, the crystallization process and procedures can be simplified to justify the government's policy through the development and commercialization of energy-saving process technology, accelerating the transition to advanced industrial structures such as food, medicine, and fine chemical industries and creating high value-added products. It can contribute to vitalizing the national economy and improving national income.

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Claims (7)

A stirring rod 110 is provided, wherein a raw material (for example, ethyl cellulose solution, potassium sulfate solution, potassium chloride solution, potassium phosphate solution, and hydroxide therein) (Sodium hydroxide) solution, GMP (sodium guanylate) solution, IMP (sodium inosinate) solution, MSG (sodium glutamate) solution, and the like; A second stirrer (130) having a stirring rod (110) therein and containing a solvent (Anti-solvent) therein; Kuet-Taylor reactor 150 that receives the material and the solvent combined between the outer cylinder 151 and the rotating rod 153 to change the rotational speed of the rotating rod to generate turbulence to provide stability of the fluid and to produce a crystallized material )Wow; Continuous-out crystallization separation, characterized in that consisting of a liquid pump 140 for adjusting the flow rate so as to inject a constant flow rate of the two feed solutions into the Kuet-reactor to introduce the raw material and the solvent Device. delete The method of claim 1, A solid-liquid separator (160) for separating solids or liquids, which are crystallization materials produced by the operation of the Kuet-Taylor reactor (150); A pH meter 170 for measuring the ion concentration of the crystallized material separated in the solid-liquid separator 160; An electron microscope (180) capable of attaching the crystallized material separated in the solid-liquid separator (160) to a stage using a conductive carbon tape to analyze the shape and size of individual particles; The crystallization material separated in the solid-liquid separator 160 by spraying particles using ultrasonic waves, and further comprising a particle size analyzer 190 for measuring the size of the agglomerated crystals (Drowning-out) Crystallization Separator. delete delete delete delete

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