JP2003251101A - Crystallization apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a crystallization apparatus capable of easily obtaining crystals mutually aligned in crystallographic axis direction. <P>SOLUTION: Introducing pipe 3 from an evaporation part 1 is introduced into the lower part at the center part of the container 2a of a crystallization part 2 to communicate with the container 2a and connected to the evaporation part 1 from the side wall of the container 2a by a return pipe 4. A supply pipe 5 of a raw material solution is connected to the intermediate part of the return pipe so as to communication with the return pipe 4 and a magnetic force generation means 6 comprising an electromagnet is provided to the outer side wall of the container 2a. The raw material solution is allowed to flow in the evaporation part 1 through the supply pipe 5 and the return pipe 4 to flow in the crystallization part 2 through the introducing pipe 3 while it is evaporated. The raw material solution becomes a supersaturation state in the crystallization part 2 to obtain crystals grown and formed by the magnetic field action of the magnetic force generation means 6 so as to be mutually aligned in crystallographic axis direction. <P>COPYRIGHT: (C)2003,JPO

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a crystallizer applied to medical products, food products, optical products, electric device materials, tape filler materials and the like.

[0002]

2. Description of the Related Art As a conventional crystallization apparatus of this type, as shown in FIG. 6, it comprises an evaporation part a arranged above and a crystallization part b arranged below it, and the crystallization part from this evaporation part a. The return pipe d is connected from the crystallization part b to the evaporation part a by the introduction pipe c into the part b, and the classifying leg e hangs from the crystallization part b. The raw material liquid supplied from the supply pipe f to the pipe d is partially evaporated in the evaporation part a, and the concentrated raw material liquid is crystallized in the crystallization part b via the introduction pipe c in a supersaturated state. Then, the remaining raw material liquid returns to the evaporation part a via the return pipe d, and the raw material liquid is replenished from the supply pipe f, and the crystal formed in the crystallization part b can be obtained from the classification leg e. Are known.

[0003]

According to this conventional crystallizer, the crystal is simply grown from the raw material liquid in the supersaturated state in the crystallizing part b, so that the orientation of the obtained grown crystal is as shown in FIG. As described above, there is a problem in that a uniform drug or the like having a high pharmacological effect cannot be obtained.

It is an object of the present invention to solve the above problems and to provide a crystallizer capable of obtaining crystals in which the orientation, that is, the crystal axis directions are the same.

[0005]

To achieve this object, the present invention is characterized in that a magnetic force generating means is provided in the crystallization part.

[0006]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 shows a first embodiment of the present invention.
Will be described.

Reference numeral 1 denotes an evaporation portion, 2 denotes a crystallization portion, the evaporation portion 1 is formed by equipping a container with heating means such as a heater, and the crystallization portion 2 located below the evaporation portion 1 Container 2
An introducing pipe 3 is provided so as to hang down in the lower part of the central portion in a, and the evaporating part 1 and the crystallization part 2 are connected by the introducing pipe 3.

Further, a return pipe 4 extending from the upper portion of the side wall of the container 2a of the crystallization part 2 to the evaporation part 1 is connected and connected,
A raw material liquid supply pipe 5 was connected in the middle of the return pipe 4.

Reference numeral 6 denotes a magnetic force generating means, which is composed of a cylindrical electromagnet and is used for the container 2a of the crystallization part 2.
It is provided on the outside of the side wall so as to surround it.

Reference numeral 7 denotes a tubular classifying leg through which crystals fall, and the classifying leg 7 is provided so as to hang from the bottom surface of the container 2a of the crystallization part 2.

Next, the operation of the first embodiment will be described.

When the raw material liquid is supplied from the supply pipe 5, the raw material liquid reaches the evaporation unit 1 through the return pipe 4, and the evaporation unit 1
At, a part is evaporated and concentrated.

Then, the concentrated raw material liquid flows out from the introduction pipe 3 to the lower part of the center part of the container 2a of the crystallization part 2.

In the container 2a, the concentrated raw material liquid is cooled by the surrounding solution, becomes supersaturated, and gradually flows upward, and crystals grow and form while crystallizing during the upward flow. At this time, due to the action of the magnetic field in the container 2a generated by the outer electromagnet 6 in the container 2a, crystals grow and form with their crystal axis directions aligned as shown in FIG.
That is, the crystal grows with its crystal axis direction parallel to the magnetic field direction in which the magnetic susceptibility due to the magnetic field force is minimized.

The remaining raw material liquid after being crystallized in this way is returned to the evaporator 1 by the return pipe 4.
At this time, the raw material liquid is replenished to the return pipe 4 from the supply pipe 5, and the crystals formed in the container 2a and having the same crystal axis direction are taken out from the classifying leg 7.

Here, the inventor put the liquid of L-alanine into the container of the crystallization part to make it supersaturated, and variously changed the strength of the magnetic field by the electromagnet to obtain the orientation ratio R. The result is shown in FIG. Is a graph of.

In the graph, when the horizontal axis is the magnetic field strength terrace (T) and the vertical axis is the orientation ratio (R), the orientation ratio R is Therefore, it was found that the ratio of the orientation of each crystal, that is, the precipitated crystal in which the angle difference θ in the crystal axis direction is smaller than 3 ° to the total measured precipitated crystal is about 100% when the magnetic field strength is 1 T or more. did.

The curve of this graph showed the same tendency for other raw material liquids. Also, in this embodiment,
Although the magnetic force generating means 6 is provided outside the container 2a, the magnetic force generating means 6 may be provided inside the container 2a.

FIG. 4 shows a second embodiment of the present invention,
In this embodiment, the evaporation part 1 and the crystallization part 2 are formed as a common container 8, and the container 8b at the part of the crystallization part 2 is formed to have a larger diameter than the container 8a at the part of the evaporation part 1. The lower portion of the side wall of the container 8a at the evaporation portion 1 is the crystallization portion 2
Partition wall 9 extending downward partway inside container 8b
And the partition wall 9 forms a crystal forming portion 2a on the inner side thereof.
The outer microcrystal removing portion 2b was partitioned, and the draft tube 10 was provided in the center of the partition wall 9. In addition, the return pipe 4a is provided from the lower portion of the side wall of the container 8b.
The raw material liquid supply pipe 5 was connected to the lower portion of the draft tube 10 on the bottom surface of the No. 3 and the return pipe 4a.

Thus, the raw material liquid from the supply pipe 5 is heated together with the return liquid from the return pipe 4a, and the container 8 of the crystallization part 2 is heated.
b, it flows from the bottom surface thereof, rises in the draft tube 10 and then flows down the outside of the draft tube 10, and a part of the flowing-down raw material liquid is generated in the draft tube 1
While rising in 0, the remaining raw material liquid rises in the minute crystal removing portion 2b outside the partition wall 9 and reaches the return pipe 4a.
The raw material liquid is replenished from the supply pipe 5 in the middle of the return pipe 4a and flows into the container 8b.

During the above-mentioned flow of the raw material liquid in the container 8,
In the container 8a of the evaporation unit 1, the liquid surface of the raw material liquid evaporates and the raw material liquid is supersaturated and crystallized. The crystal axis direction coincides with the crystallization process of the crystal due to the magnetic force of the electromagnet 6. Come on.

In the second embodiment, the flow of the raw material liquid is rectified and differentiated inside and outside by the draft tube 10 and crystallized by the action of the magnetic field force. Consistent crystals are obtained.
Although the cylindrical magnetic force generating means 6 is provided outside the container 8b in FIG. 4 of the present embodiment, it may be provided inside the container 8b.

FIG. 5 shows a third embodiment of the present invention.
In this embodiment, the magnetic force generating means 6 is provided on the partition wall 9 in the container 8, and the strength of the magnetic field is efficiently increased as compared with the second embodiment. Here, the magnetic force generating means 6
May be provided inside the partition wall 9 or outside the partition wall 9.

As the magnetic force generating means 6, a permanent magnet or a superconducting magnet may be used instead of the electromagnet. Further, these magnetic force generating means 6 may be coated to form a liquid seal.

Further, in the above embodiment, an example in which the present invention is applied to the evaporation type crystallizer is shown, but the present invention may be applied to other type of crystallizer such as a cooling type crystallizer. .

[0026]

As described above, according to the present invention, since the magnetic force generating means is provided in the crystallization part, crystals having the same crystal axis direction can be obtained, and thus, the medical material material or the light transmissive material having an improved pharmacological effect is obtained. An optical material having improved characteristics such as optical signal transmission and the like has an effect that it can be easily obtained with good filterability.

[Brief description of drawings]

FIG. 1 is an explanatory diagram of a first embodiment of the present invention.

FIG. 2 is an explanatory diagram showing a growth and formation state of crystals of the present invention.

FIG. 3 is a graph showing the relationship between magnetic field strength and crystal orientation ratio.

FIG. 4 is an explanatory diagram of a second embodiment of the present invention.

FIG. 5 is an explanatory diagram of a third embodiment of the present invention.

FIG. 6 is an explanatory diagram of a conventional crystallizer.

FIG. 7 is an explanatory view showing a state of crystal growth and formation by a conventional crystallizer.

[Explanation of symbols]

1 Evaporator 2 Crystallization part 2a container 6 Magnetic force generating means 9 partition walls 10 Draft tube

Front page continuation (51) Int.Cl. ⁷ Identification code FI theme code (reference) B01D 9/02 605 B01D 9/02 605 609 609 609B 611 611Z 621 621 (72) Inventor Kaoru Ogawa 4-chome Takamatsu, Morioka, Iwate Prefecture 17-19-102

Claims (6)

[Claims] 1. A crystallizer in which a magnetic force generating means is provided in the crystallizing portion. 2. A crystallizer comprising a vaporizer and a crystallizer communicating with the vaporizer, wherein a magnetic force generating means is provided in the crystallizer. 3. The crystallizer according to claim 1, wherein the magnetic force generating means is provided on the wall surface of the container of the crystallization part. 4. A crystal forming part in a central part and a fine crystal removing part in a peripheral part are formed in a container of the crystallization part through a cylindrical partition wall, and the magnetic force generating means is provided on the partition wall. The crystallizer according to claim 2. 5. The crystallizer according to claim 3, wherein a substantially cylindrical draft tube is provided in the partition wall. 6. The crystallizer according to claim 1, wherein the magnetic force generating means comprises an electromagnet or a permanent magnet.