JPH1133392A - Reaction container - Google Patents

Abstract

PROBLEM TO BE SOLVED: To compactly and easily assemble a container by throwing a reagent injection part, a cooling part and a seal part into one. SOLUTION: The reagent B injected into a container 1 is injected through the interior of the inner pipe 3 of an injection pipe 2 and the evaporated component generated in the container 1 is ready to escape to the outside through the inner pipe 3 of the injection pipe 2 but cooled by the cooling medium (e.g. water) flowing through the gap between the inner pipe 3 and an outer pipe 4 and liquefied to be returned into the container 1. An inert gas (e.g. nitrogen) is allowed to flow in from the gas inflow part 3c provided to the pipe wall of the inner pipe 3 of the injection pipe 2 and discharged from a reagent injection port 3a to seal the upper part of the inner pipe 3.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a reaction vessel for reacting two or more kinds of reagents, and more particularly to a reaction vessel capable of reacting under reflux with a seal made of an inert gas.

[0002]

2. Description of the Related Art Conventionally, when two or more kinds of reagents are allowed to react so that they can be refluxed, a reaction vessel as shown in FIG. 4 is known (issued by Maruzen Co., Ltd., 4th edition Experimental Chemistry Course 2 Basics). See operation II).

[0003] The reaction vessel comprises a flask 11 containing reagent A, a dropping funnel 12 containing reagent B, and a condenser 1.
3 and a stirrer 14.

The reaction between the reagent A and the reagent B is carried out by pouring the reagent B from the dropping funnel 12 into the flask 11 containing the reagent A. In addition, the above reaction is often performed under heating, and the reaction raw materials, reaction products, reaction solvents, and the like vaporized by heating are cooled by the condenser 13, liquefied, and returned into the flask 11. Further, in order to stabilize the reaction, stirring is usually performed by the stirrer 14.

[0005] Such a reaction is usually performed by connecting a filling tube filled with a desiccant or the like to the upper part of the condenser 13,
It has been practiced to seal the reaction system under open pressure.

As described above, the conventional reaction vessel comprises a dropping funnel 12 as a reagent injection section and a condenser 13 as a cooling section.
And a seal portion (not shown) are separately provided for the flask 11.

[0007]

However, in the above-mentioned conventional configuration, since the reagent injection section, the cooling section, and the seal section are provided separately from each other, the space becomes large and the labor for assembling the container is increased. Is also complicated.

SUMMARY OF THE INVENTION The present invention has been made to solve the above problems, and an object of the present invention is to integrate the above-mentioned reagent injection section, cooling section and seal section into a single unit, and to make the container compact and easy to assemble. It is to provide a reaction container.

[0009]

The reaction vessel according to claim 1 comprises:
In order to solve the above-described problems, the reaction container is configured to include a container portion that stores the first reagent in advance, and a second reagent injected into the container portion. The injection tube has an inner tube for injecting a second reagent, and an outer tube covering the outside of the inner wall of the inner tube. A cooling unit for cooling the evaporating component passing therethrough; a reagent injecting unit for injecting a second reagent from an upper port of the inner tube, and injecting the second reagent into a container unit from a lower port; A gas inlet from a gas inlet branched from the pipe wall.

According to the above configuration, when reacting the first and second reagents, the first reagent is put in the container in advance. Then, the second reagent is injected into the container through the injection tube. At this time, the second reagent passes through the inside of the inner tube of the injection tube. During the reaction, the evaporating component generated in the container tends to escape to the outside through the inner tube of the injection tube, and the evaporating component is cooled by a cooling medium (for example, water) flowing between the inner tube and the outer tube. ) Cooled by
It is liquefied and returned into the container. An inert gas (eg, nitrogen) is introduced from a gas inlet provided on a pipe wall at an upper portion of the injection pipe to seal the container under an open pressure by shutting off the air from the atmosphere. Is discharged from the upper port of the inner pipe of the injection pipe while being filled and filled.

Incidentally, the first and second reagents do not necessarily mean a single compound, respectively, and in some cases, two or more compounds may be mixed. Further, the first and second reagents may be mixed with the reaction solvent, respectively, or the reaction solvent may be put in the container in advance.

Thus, the reagent injecting section, the cooling section, and the sealing section provided separately for the container section can be integrated into one member, so that the reaction vessel can be made compact and the assembly of the container can be performed. Can easily obtain a reaction vessel.

[0013]

DESCRIPTION OF THE PREFERRED EMBODIMENTS One embodiment of the present invention will be described below with reference to FIGS. As shown in FIG. 1, the reaction container according to the present embodiment includes a container 1 (container part) and an injection pipe 2 installed on the upper part of the container 1.

The container 1 is made of, for example, a cylindrical glass tube and has a capacity of about 100 ml.

As shown in FIG. 2, the injection pipe 2 has a double structure composed of an inner pipe 3 and an outer pipe 4, and the inner pipe 3 and the outer pipe 4 are completely connected to each other. Are separated. The inner tube 3 has a reagent inlet 3 at its upper part.
a (upper port), and a reagent dropping port 3
b (lower port) is provided, and a gas inlet 3c is provided in the pipe wall near the upper part. Further, a cooling medium supply port 4a and a cooling medium discharge port 4b are provided in the upper and lower portions of the pipe wall of the outer pipe 4.

When the reaction between the reagent A (first reagent) and the reagent B (second reagent) is carried out using the above-mentioned reaction vessel, the reagent A is previously placed in the vessel 1, The reagent B is injected into the container 1 from the injection tube 2 inserted at the top. At this time, the reagent B is injected from the reagent injection port 3a of the injection pipe 2, passes through the passage pipe of the inner pipe 3, and is injected into the container 1 from the reagent dropping port 3b.

The reagents A and B are terms used for convenience in explanation of the operation, and do not necessarily mean a single compound. In some cases, two or more compounds are mixed. Sometimes. Further, the reagents A and B may be mixed with the reaction solvent, respectively.
The reaction solvent may be put in the container 1 in advance.

A reaction occurs when the reagent A and the reagent B are mixed in the container 1 in this manner. When the reaction is performed under heating, a heating device for heating the container 1 is provided. In the present embodiment, an aluminum block thermostat 5 (see FIG. 1) is used for the heating device. The aluminum block thermostat 5 heats the container 1 by a heating unit (not shown) and passes cooling water, for example, a mixture of ethylene glycol and water, through a hole 5a formed inside the aluminum block thermostat 5. Cooling can be performed. Thereby, the aluminum block thermostat 5 can be heated while keeping the container 1 at a constant temperature. still,
The method of heating the container 1 is not limited to this.

When such heating is performed or due to an exothermic reaction, the reaction raw materials, reaction products, reaction solvents, and the like in the container 1 evaporate due to heat and pass through the inner pipe 3 of the injection pipe 2 to the atmosphere. Try to escape inside. In order to prevent this, a cooling medium is supplied from a cooling medium supply port 4a provided in a lower part of the pipe wall of the outer pipe 4 and is circulated between the inner pipe 3 and the outer pipe 4 so that the cooling medium discharge port 4b By further discharging, the pipe wall of the inner pipe 3 is cooled, and the evaporation component passing through the inner pipe 3 is liquefied and returned to the container 1.

Further, in such a reaction, in order to avoid direct contact of the reaction system with the atmosphere, it is necessary to seal the reaction system by shutting off the upper part of the injection pipe, which is the contact portion with the atmosphere, from the atmosphere. There is. For such sealing purposes,
An inert gas is supplied from the gas inlet 3c of the inner tube 3 and discharged into the atmosphere from the reagent inlet 3a. As a result, the upper part of the inner tube 3 is filled with the flowing inert gas, and the reaction system is sealed off from the atmosphere by the inert gas. The inert gas supplied from the gas inlet 3c is typically nitrogen. In this embodiment, nitrogen is used. However, the inert gas is not limited to this as long as it is inert to the reaction. Other inert gases such as, argon, helium, carbon dioxide may be used.

In the reaction, stirring is usually performed. In the present embodiment, a magnetic stirrer 6 (see FIG. 1) is placed in the container 1 and the magnetic stirrer 6 is The rotation inside the container 1 is performed by rotation.

As described above, the reaction vessel according to the present embodiment is composed of the vessel 1 and the injection pipe 2, and in the injection pipe 2, the reagent is injected through the inner pipe 3, the reagent injection port 3a and the reagent dropping port 3b. A cooling unit is formed by the inner pipe 3, the outer pipe 4, the cooling medium supply port 4a, and the cooling medium discharge port 4b, and the inner pipe 3, the gas inlet 3c, and the reagent inlet 3a.
Constitutes a seal portion. The reagent injection section, the cooling section, and the sealing section are integrated into one in the injection pipe 2, whereby a reaction vessel for reacting a reagent can be formed compact.

In the reaction vessel according to the present embodiment,
Since the reagent injection section, the cooling section, and the sealing section are integrated into one member, the complicatedness in the assembly of the reaction vessel as in the related art is eliminated. This is a great advantage particularly when the reaction experiment is performed by an automated apparatus.

When the reaction apparatus according to the present embodiment is used in an automated apparatus, it is desirable to further have the following configuration.

That is, the container 1 containing the reagent A in advance
The opening of the container 1 is sealed with a lid (septum) 7 as shown in FIG. 3 to prevent the reagent A from spilling or volatilizing during movement. The lid 7 has a cylindrical cap portion 7a made of, for example, polyethylene.
Is sealed with an extremely thin Teflon sheet 7b having a thickness of about 2 μm. When the reagent B is injected into the container 1, the reagent dropping port 3b of the injection tube 2 breaks the Teflon sheet and is inserted into the container 1 (see FIG. 1). Thereby, it is not necessary to remove the lid 7 from the container 1 when assembling the reaction container in the automated apparatus, and the assembly of the reaction container becomes extremely easy.

When the reagent B is injected in an automated apparatus, a thin tubular needle 8 (see FIG. 1) is inserted into the passage of the inner pipe 3 of the injection pipe 2, and the needle 8
Reagent B is poured through the narrow tube. For this reason, a funnel-shaped guide portion 3d for securely guiding the needle 8 into the passage of the inner tube 3 is provided at the reagent inlet 3a of the injection tube 2.
Is more preferably provided.

Further, the method of using the above-mentioned reaction vessel is not limited to the above-mentioned method, but the following use is also possible. For example, instead of using the gas inlet 3c for supplying inert gas, a pump is connected to the gas inlet 3c via a trap. Thus, for example, when a toxic gas is generated by the reaction, if the suction is performed by the pump through the gas inlet 3c, the generated toxic gas is prevented from being released into the atmosphere from the reagent inlet 3a. be able to.

In the reactor according to the present embodiment, the shape of the container 1 is cylindrical, but the present invention is not limited to this. Of course, the capacity and material of the container 1 are not limited.

[0029]

As described above, the reaction container according to the first aspect of the present invention is configured such that the reaction container has a container portion for storing the first reagent in advance and an injection pipe for injecting the second reagent into the container portion. Wherein the injection tube has an inner tube for injecting a second reagent, and an outer tube that covers the outside of the inner wall of the inner tube, and a cooling medium passes through the outer tube to evaporate through the inner tube. A cooling section for cooling the components, a reagent injecting section for injecting a second reagent from an upper port of the inner tube and injecting the second reagent into a container section from a lower port, And a seal portion through which gas flows in from a branched gas inlet.

Therefore, the reagent injecting section, the vapor cooling section and the gas inflow section conventionally provided separately for the vessel section can be integrated into one member, and the reaction vessel can be made compact. This has the effect that a reaction container in which the container can be easily assembled can be obtained. Further, the inventive container according to the present invention can be suitably used as a reaction container in an automated automatic synthesis apparatus.

[Brief description of the drawings]

FIG. 1, showing an embodiment of the present invention, is a side view illustrating a configuration of a reaction apparatus.

FIG. 2 is a cross-sectional view showing a structure of an injection tube of the reaction apparatus.

FIG. 3 shows a lid of a container part of the reaction container, and FIG.
3A is a plan view of the lid, and FIG. 3B is a side view of the lid.

FIG. 4 is a side view showing a conventional reaction vessel.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Container 2 Injection pipe 3 Inner pipe 3a Reagent inlet 3b Reagent inlet 3c Gas inlet 4 Outer pipe 4a Coolant supply port 4b Coolant outlet

Claims (1)

[Claims] 1. A reaction vessel for reacting first and second reagents, wherein the reaction vessel comprises: a vessel section for storing the first reagent in advance;
An injection tube for injecting a second reagent into the container portion, wherein the injection tube has an inner tube for injecting the second reagent, and an outer tube for covering the outside of the tube wall of the inner tube; A cooling unit for passing a cooling medium through the outer tube to cool the evaporating component passing through the inner tube; a second reagent is injected from an upper port of the inner tube, and the second reagent is injected into a container from a lower port. A reaction container, comprising: a reagent injecting section; and a seal section through which gas flows in from a gas inlet branched from a wall of the inner tube.