JPH07180Y2 - Pressure reaction vessel - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial application] The present invention relates to a pressure reaction vessel, for example, a stress reaction vessel that can be used for experiments and research.

[Prior Art] When various chemical reactions are carried out under pressure, especially in a laboratory,
When carrying out on a small scale in a laboratory, a pressure reaction vessel (autoclave) made of metal having sufficient pressure resistance is used.

In experiments using this type of pressure reaction vessel, a portion of the reaction product was regularly removed at regular time intervals in order to understand the change over time of the reaction or to measure the reaction rate. The conversion rate, selectivity, etc. are calculated by collecting the sample and analyzing the sample.

When collecting a sample in a container using a conventional pressure reaction container, open the valve of the sample collection pipe that is connected from the inside of the container to the outside, and eject part of the reaction product by self-pressure. The sample was collected in a receiver and used as a sample for analysis.

[Problems to be Solved by the Invention] According to the conventional sampling using the pressure reaction vessel described above, for example, when the reaction is carried out using a solvent at a temperature higher than the boiling point of the solvent, the mouth of the vessel is Since it is in an open state, part of the solvent evaporates and the concentration of the sample changes during and after the collection of the sample and before the analysis,
Since the sample was not cooled immediately after collection, the reaction proceeded to some extent and an accurate analysis result could not be obtained. In addition, the solvent of the collected sample evaporates and scatters, which poses a problem of high risk of ignition.

It is an object of the present invention to provide a pressure reaction vessel capable of collecting a sample and performing an accurate analysis without accompanying a chemical change or a concentration change of the sample to be collected.

[Means for Solving the Problems] A pressure reaction vessel according to the present invention is characterized in that a vessel is provided with a sample collection tube communicating from the inside to the outside, and a plurality of sample tubes are detachably attached to the sample collection tube. And

The sample tube may be provided with fins. The shape and number of the fins are arbitrary.

Further, as the sample tube, a tube having a double tube structure, which allows a cooling medium to flow in one tube and collect a sample in the other tube, can be used.

Further, the sample tube may have a curved portion. It is desirable that the curved portion has a shape and size that can store a sample of a volume necessary for analysis.

Each of the fin, double tube structure, and curved portion of the sample tube may be provided individually, or a plurality of fins and curved portions may be simultaneously provided.

The sample tube may be attached to the sample collecting tube in a so-called side branch shape in which each straight tube portion is branched into a T shape, or there is no straight tube portion, and the sample tube is radially or parallel through a common distributor. A method of branching into a shape may be used.

[Operation] When conducting an experiment using a pressure reaction vessel, the reaction solution is sequentially introduced into each sample tube through a sample collection tube communicating from the inside of the vessel to the outside at predetermined time intervals or continuously, Remove the sample tube from the sampling tube and use the sample collected for analysis.

By providing the sample tube with fins, the sample collected through the fins can quickly dissipate heat.

Further, the sample tube has a double structure, and the cooling medium is circulated in one of the tubes while the sample is being collected, so that the collected sample is quickly cooled. This more effectively suppresses the progress of the chemical reaction of the collected sample.

Furthermore, by forming a curved portion in the sample tube, a required amount of sample is stored in this curved portion.

[Embodiment] A first embodiment of the present invention will be described with reference to FIG.

The pressure reaction container 1 is composed of a container body 2 and a lid portion 3 attached to the upper portion thereof. Inside the container 1, a stirring rod 4 connected to a driving means (not shown) such as a motor through a hole 3A formed in the center of the lid 3 is provided. Further, the thermocouple insertion tube 5 and the sampling tube 6 are arranged through the holes 3B and 3C formed in the lid 3 at positions that do not hinder the rotation of the stirring rod 4 in the container 1.

In the portion of the sampling tube 6 extending outside the container 1,
The first ball valve 7A, the three T-shaped tubes 9A to 9C, and the second ball valve 7B are sequentially arranged in series. These three T-tubes 9A
Ball valves 7C to 7E are removably attached to the sample collection ports 10 to 9C, and three sample tubes 8A to 8C are fixed via the ball valves 7C to 7E. As a result, each sample tube 8A ~
8C can be attached to and detached from the sampling tube 6 together with the ball valves 7C to 7E. Lids 11A to 11C are attached to the ends of these sample tubes 8A to 8C. In addition, each sample tube 8A-8C
A large number of circular fins 12 are fixed around the circumference of.

Next, a method of collecting a sample in the case where an experiment is carried out using the present pressure reaction container 1 and a change with time of the reaction product during the experiment is analyzed, for example, every 15 minutes, will be described.

First, all the ball valves 7A to 7E are closed, and 15 minutes after the start of the reaction, the first and second ball valves 7A, 7A of the sampling pipe 6 are closed.
By opening B in this order and discharging the gas, liquid, etc. in the sampling tube 6 to the outside of the sampling tube 6, after filling the sampling tube 6 with the reaction product 13 in the container 1, the second Ball valve
Close 7B. After this, the T that communicates with the first sample tube 8A
The ball valve 7C of the character tube 9A is opened, the reaction product 13 is introduced into the sample tube 8A, and after the introduction, the ball valve 7C is closed.

Then, 30 minutes after the start of the reaction, as in the case of the first sample tube 8A, the first and second ball valves of the sampling tube 6 are
After 7A and 7B are opened and the gas, liquid, etc. in the sampling tube 6 are discharged to the outside of the sampling tube 6, after filling the sampling tube 6 with the current reaction product 13 in the container 1, 2 ball valve 7B is closed. Thereafter, the ball valve 7D of the T-shaped tube 9B communicating with the second sample tube 8B is opened, the reaction product 13 is introduced into this sample tube 8B, and after the introduction, the ball valve 7D is closed.

Next, 45 minutes after the start of the reaction, a sample is sampled from the third sample tube 8C in the same manner as in the case of the first and second sample tubes 8A and 8B.

After collecting the samples in all the sample tubes 8A to 8C in this way, the first ball valve 1A is closed, and the respective sample tubes 8A to 8C are removed together with the ball valves 7C to 7E, and the collected samples are subjected to analysis.

If samples are to be analyzed after 60 minutes and thereafter, new sample tubes 8A-8C are attached to T-shaped tubes 9A-9C to which sample tubes 8A-8C are not attached, and the sample tubes 8A-8C are attached. A sample is taken in the same manner as above.

By using the pressure reaction vessel 1 according to this example,
At the time of sampling, even if the temperature of the sample immediately after being collected is high, heat is radiated through the fins 12 fixed to the sampling tubes 8A to 8C, so that the reaction of the sample can be suppressed. , Accurate analysis is possible. In addition, since the mouths of the sample tubes 8A to 8C are not open during the sampling of the sample and before the analysis is performed, the solvent in the sample does not evaporate or scatter. Also, there is no fear that the sample concentration will change and the ignition will occur. Further, by opening and closing the ball valves 7A to 7E provided on the sample collecting pipe 6 and the T-shaped pipes 9A to 9C, it is possible to collect samples over a predetermined period of time or continuously.

Next, a second embodiment of the present invention will be described with reference to FIG.

In the present embodiment, each sample tube 8A to 8C is a cylindrical inner tube 14 and an outer tube concentrically arranged with respect to the inner tube 14.
It consists of 15 double tube structures.

In the sample tubes 8A to 8C configured as described above, when the sample is collected in the inner tube 14, the cooling medium (for example, cooling water) 16 is put into the outer tube 15 from one inlet port 15A, and the other outlet port 15B. Then, the cooling medium 16 is continuously circulated.

In this way, while the cooling medium 16 is flowing through the outer pipe 15, the inner pipe 14
By collecting the sample therein, the sample in the sample tube 6 can be cooled more quickly, and the progress of the reaction of the sample can be suppressed, so that the sample can be accurately analyzed.

Next, a third embodiment of the present invention will be described with reference to FIG.

In this embodiment, each sample tube 8A to 8C has a curved portion.
17 is formed, and the sample tubes 8A to 8C are attached to the T-shaped tubes 9A to 9C so that the curved portion 17 is located below. This bend
Although the shape of 17 is arbitrary, the volume of this portion is approximately equal to the volume of the sample to be collected (volume required for analytical test).

When collecting a sample using these sample tubes 8A to 8C, a required amount of sample is stored in the curved portion 17.

By using the sample tubes 8A to 8C in which the curved portion 17 is formed, it is possible to obtain an effect that the width of the sampleable volume is widened as compared with the case where the curved portion 17 is not formed.

Next, a fourth embodiment of the present invention will be described with reference to FIG.

In this embodiment, ball valves 7C to 7E and 7F to 7H are provided between the T-shaped tubes 9A to 9C and the sample tubes 8A to 8C, respectively, and these ball valves 7C to 7H are detachably provided. As a result, both ball valves 7C to 7E immediately after the sample is introduced into the sample tubes 8A to 8C.
Also, the sample tubes 8A to 8C can be removed from between 7F and 7H and the collected sample can be immediately analyzed.

The present invention is not limited to the above-described embodiments, and modifications within a range in which the object of the present invention can be achieved are included in the present invention.

For example, the number of sample tubes 8A to 8C to be attached is not limited to three, and may be two or four or more, and in short, may be plural.

Further, the attachment of the sample tubes 8A to 8C to the sample collecting tube 6 does not necessarily have to be a so-called side branch shape in which the straight tube portions are branched into T-shapes using the T-shaped tubes 9A to 9C. Other attachment means such as a plurality of sample tubes attached radially or in parallel via a common distribution portion provided at the end of 6 may be used. In short, a plurality of sample tubes may be detachably attached to the sample collecting tube 6.

Further, each ball valve 7A to 7H may be a conventional general type valve other than the ball valve. In the above embodiment, the opening / closing operation of these ball valves 7A to 7E is performed manually, but it is also possible to perform the opening / closing operation automatically by using an electromagnetic valve or the like instead of the ball valve. it can.

Furthermore, a valve may be provided in each of the lids 11A to 11C of the sample tubes 8A to 8C to facilitate the introduction of the sample.

[Advantage of Device] By collecting a sample by using the pressure reaction container according to the present invention, the progress of the reaction of the sample can be suppressed,
Further, since the solvent in the sample does not evaporate or scatter, accurate analysis becomes possible.

[Brief description of drawings]

FIG. 1 is a sectional view of a first embodiment of the present invention, FIG. 2 is a sectional view showing an essential part of a second embodiment, FIG. 3 is a perspective view showing an essential part of a third embodiment, and FIG. [FIG. 8] is a sectional view showing an essential part of a fourth embodiment. DESCRIPTION OF SYMBOLS 1 ... Pressure reaction container, 6 ... Sampling pipe, 7A-7H ... Ball valve, 8A-8C ... Sample pipe, 12 ... Fin, 14 ... Inner pipe, 15 ... Outer pipe, 17 ... Curved part.

Claims (4)

[Scope of utility model registration request] 1. A pressure reaction container comprising a container with a sample collection tube communicating from the inside to the outside, and a plurality of sample tubes are detachably attached to the sample collection tube. 2. The pressure reaction vessel according to claim 1, wherein the sample tube is provided with fins. 3. A sample tube having a double tube structure, wherein a cooling medium can be circulated in one tube and a sample can be collected in the other tube. Alternatively, the pressure reaction vessel according to claim 2. 4. The pressure reaction container according to claim 1, wherein the sample tube is formed with a curved portion.