JPH0685864B2 - Hydrothermal reactor - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a hydrothermal reaction device in which a solid phase and a liquid phase are reacted with each other so that only the liquid phase can be taken out at a temperature during the reaction. , Water resistance test of materials, measurement of solubility of substances, evaluation of environmental impact of disposal of radioactive waste by conducting reaction experiments between rocks and soil and water, soil due to acid rain・ The present invention relates to a hydrothermal reaction device that can be effectively used for research in the field of earth science, such as evaluation of the buffer capacity of rocks and elucidation of the origin of ore deposits.

[0002]

2. Description of the Related Art Japanese Unexamined Utility Model Publication No. 2-107057 discloses a pressurized reaction vessel which is rotatable and agitated in order to increase the reaction rate and which is small and has good operability. In this pressurized reactor, even if there is a request to know the chemical composition of the liquid under the reaction conditions, the liquid cannot be taken out under the reaction conditions, so the composition cannot be known. on the other hand,
A hydrothermal reaction device that can take out only a liquid phase from a pressurized reaction container has been conventionally known, but this device has a large container itself.
There is a problem that the operation is complicated and time-consuming.

[0003]

The technical problem of the present invention is that the liquid extraction operation from the pressurized reaction vessel can be easily performed at any time, and the extracted liquid is immediately diluted to boil the liquid. It is to obtain a hydrothermal reaction device that does not cause precipitation and prevents precipitation.

[0004]

The hydrothermal reaction vessel of the present invention for solving the above-mentioned problems contains a solid-phase and liquid-phase sample to be reacted in a hermetically sealed manner, and rotationally stirs in a heated state. A liquid extraction hole is opened in the closed lid of the enabled pressurized reaction vessel, and a filter for flowing out only the liquid phase from the container is attached to the inner end of the liquid extraction hole, and the outer end of the liquid extraction hole is also attached. On the other hand, attach a female quick connect to the mouth of the liquid collection bottle, and connect a male quick connect that communicates with the introduction tube inserted into the inside of the liquid collection bottle. By inserting the male quick connect into the quick connect, the internal flow paths of the both can be joined liquid-tightly, and the female quick connect is provided with an outflow valve for outflowing the liquid in the container.

[0005]

Function: A solid-phase and liquid-phase sample to be reacted is housed in a pressure reaction vessel and sealed, and the vessels are arranged in parallel in the electric furnace at regular intervals and rotated in a pair in the same direction. The sample is placed horizontally on a drive rod, and the sample in the container is reacted under hot water conditions while being rotated and stirred by the rotation of the rotary drive rod. During this heating reaction, the sample in the container does not flow out because the outflow valve in the female quick connect attached to the closed lid is closed.

When it is necessary to remove the liquid, the male quick connect of the liquid collection bottle is joined to the female quick connect of the pressurized reaction vessel, thereby opening the outflow valve of the female quick connect. As a result, only the liquid flows out from the pressurized reaction vessel in the pressurized state through the filter, enters the liquid collection bottle through the flow path communicating with the male quick connect, and the liquid collection bottle is stored in advance. It is diluted with the water stored in.
Therefore, the liquid extraction operation from the pressurized reaction vessel can be easily performed at any time by simply connecting the female quick connect of the pressurized reaction vessel to the male quick connect of the liquid collection bottle. Moreover, when the extract is immediately diluted with water as described above, the extract does not boil and precipitation does not occur.

[0007]

The hydrothermal reactor of the present invention will be described in detail below with reference to the drawings. The illustrated hydrothermal reaction apparatus includes a pressure reaction container 1 and a liquid collection bottle 2 joined to it. The pressurized reaction container 1 hermetically accommodates a solid phase and liquid phase sample to be reacted therein, and enables rotational stirring in an electric furnace with a rotating mechanism in a heated state. A narrowed cylindrical outer cylinder 11, a disk-shaped bottom plate 12 attached to one end of the outer cylinder 11, a bottomed inner cylinder 13 made of fluororesin fitted in the outer cylinder 11, the outer cylinder 11 and A sealing lid 14 for sealing the mouth portion of the bottom inner cylinder 13 and a fixed ring 15 for fixing the sealing lid 14 are provided.

The closed lid 14 of the above pressurized reaction vessel is made of titanium which is resistant to corrosion even under high temperature and high pressure, and a liquid extraction hole 16 is opened in the center thereof. A gold filter 17 for letting out only the water is attached by screwing an attachment screw ring 18, and a female quick connect 19 is attached to the outer end of the liquid extraction hole 16. As the filter 17, for example, a filter made of fluororesin can be used. In addition, the bottomed inner cylinder 13
Has a seating surface 13a at its mouth, and
Is a conical mating surface 1 that is seated on this seating surface 13a.
4a is provided. The sealing lid 14 is mounted by inserting the sealing lid 14 into the outer cylinder 11 and providing the female screw 11a provided at the mouth of the outer cylinder.
Then, the thick ring-shaped fixed ring 15 provided with the male screw 15a on the outer peripheral portion is screwed into the outer peripheral portion.

On the other hand, in the liquid collecting bottle 2, the bottle body 21 is attached to the lid 22 screwed to the mouth of the heat resistant bottle body 21.
The introduction pipe 23 made of stainless steel introduced to the inside of the above is attached by a fitting 24, and a male quick connect 25 having a through hole communicating with the introduction pipe 23 is attached on the fitting 24. .

The female quick connect 19 attached to the sealing lid 14 has an outflow valve 32 in a flow path 31 for letting out the liquid in the container, and a male quick connect 25 attached to the liquid collecting bottle 2. An inflow valve 42 is provided in the inner flow path 41. Also, the flow path 31 of the female quick connect 19
A seal member 36 is provided therein for liquid-tightly joining the internal flow paths 31 and 41 of the male quick connect 25 when the male quick connect 25 is fitted therein.

Outflow valve 3 in the female quick connect 19
Reference numeral 2 denotes a valve seat 33 which is pressed against a valve seat 34 on the outlet end side of the flow path 31 from the inner end side of the flow path 31 by a spring 35. Although it is in a closed state due to the pressure inside the container, when it is pushed inward by the valve rod 43 at the tip of the male quick connect 25 due to the connection with the male quick connect 25, the valve element 33 separates from the valve seat 34. The valve is opened to allow the liquid in the container to flow out.

On the other hand, the inflow valve 42 in the male quick connect 25 has a valve body 44 at the tip of the valve rod 43 inserted in its flow path from the bottle body 21 side to the male quick connect 25 by a spring (not shown). It is designed to be pressed against the valve seat 45 inside, and is opened by the pressing of the valve rod 43.
The liquid can flow into the bottle body 21 through the.

The outflow valve 32 and the inflow valve 42 allow the liquid in the pressurized reaction container to flow out to the liquid collection bottle only by the joining operation of the female quick connect 19 and the male quick connect 25. The structure is merely an example, and other suitable structures can be adopted, and the inflow valve 42 of the male quick connect 25 can be omitted.

In the hydrothermal reaction apparatus having the above-mentioned structure, the solid-phase and liquid-phase samples to be reacted are pressurized reaction vessel 1
It is housed in a container and sealed, and the container is placed horizontally on a pair of rotary drive rods that are arranged in parallel in the electric furnace at regular intervals and rotate in the same direction, and rotated by the rotation of the rotary drive rods. While stirring, the sample in the container is reacted under hot water conditions. During this heating reaction, the sample in the container does not flow out because the outflow valve 32 in the female quick connect 19 attached to the closed lid 14 is closed.

When it is necessary to take out the liquid, the female quick connect 19 of the pressurized reaction vessel is joined to the male quick connect 25 of the liquid collecting bottle 2 in which water has been put in the bottle body 21 in advance, whereby the female quick connect is carried out. At the same time as the outflow valve 32 of the connect 19 is opened, the inflow valve 42 of the male quick connect 25 is opened. As a result, only the liquid flows out from the pressurized reaction container 1 in the pressurized state through the filter 17, flows into the liquid collection bottle 2 through the flow path communicating with the male quick connect, and collects the liquid. It is diluted with the water contained in the bottle body 21 of the bottle 2.

Therefore, the liquid extraction operation from the pressurized reaction container 1 can be performed at any time by a simple operation of joining the male quick connect 25 of the liquid collection bottle 2 to the female quick connect 19 of the pressurized reaction container. Can be done easily. Moreover, even if the liquid rapidly comes out from the pressurized reaction vessel,
All the extract can be collected without splashing outside. Further, when the extract is immediately diluted with water as described above, the extract does not boil and precipitation does not occur.

Next, an example of use of the hydrothermal reaction device thus constructed will be described. As a sample to react,
1 g of alumina silica gel in which the atomic ratio of aluminum to silicon is 1: 4 and 10 g of 0.5N KOH solution are put into a bottomed inner cylinder 13 made of fluororesin, and the seating surface 1 of the bottomed inner cylinder is placed.
The fitting surface 14a of the sealing lid 14 was seated on 3a, the fixing ring 15 was screwed into the outer cylinder 11, and the container was closed by the sealing lid 14 to complete the storage of the sample.

In this state, the male quick connect 25 connected to the N ₂ gas cylinder was connected to the female quick connect 19 of the pressurized reaction vessel, and the pressure in the pressurized reaction vessel was increased to 30 atm so that there was no leakage in the vessel. After confirmation, the internal pressure was then reduced to 10 atm, and the male quick connect 25 was cut off from the female quick connect 19.

Pressurized reaction vessel 1 thus prepared
Is horizontally installed on a pair of rotation drive rods that rotate in the same direction and are provided in parallel in an electric furnace (not shown) at regular intervals, and the electric furnace is heated to 200 ° C. The container was rotated by the rotation of the rotary drive rod, and the container was operated in this state for 12 days. On the other hand, add 2 distilled water to the liquid collection bottle.
00 g was put into the tube, the lower end of the introduction tube 23 was allowed to bathe in a water bath, and the weight of the liquid collection bottle was measured.

When the female quick connect 19 of the pressurized reaction vessel 1 heated for 12 days is joined to the male quick connect 25 of the liquid collection bottle 2, only the liquid in the pressurized reaction vessel 1 passes through the filter 17 and the introduction pipe 23. Came out from the bottom edge of. Liquid extraction was completed in 2 to 3 seconds, and the extracted liquid was transparent with no precipitate. The weight of the liquid collection bottle 2 was measured, and the amount of the extraction liquid and the liquid dilution rate were calculated from the weight difference before and after the extraction. By chemical analysis of the diluted solution, the chemical composition of the solution under the reaction conditions could be determined. Also, the pressurized reaction vessel 1 was cooled to room temperature and the sample inside was taken out, but no liquid remained inside.

[0021]

EFFECTS OF THE INVENTION According to the hydrothermal reaction apparatus of the present invention described in detail above, by using the quick connect for taking out the liquid from the pressurized reaction vessel, the liquid taking-out portion can be downsized and the pressurized reaction can be performed at the same time. The liquid extraction operation from the container can be easily performed at any time, and the extracted liquid can be immediately diluted so that the liquid does not boil and the precipitation is prevented.

[Brief description of drawings]

FIG. 1 is a cross-sectional view showing an example of a pressurized reaction container of the present invention.

FIG. 2 is a vertical cross-sectional view showing an example of a liquid collection bottle joined to the pressure reaction container.

[Explanation of symbols]

1 pressurized reaction container, 2 liquid collection bottle, 14 closed lid, 16 liquid extraction hole, 17 filter, 19 female quick connect, 23 introduction pipe, 25 male quick connect, 31, 41 flow path, 32
Outflow valve.

Claims (1)

[Claims] 1. A liquid extraction hole is provided in a closed lid of a pressure reaction container which accommodates a solid phase sample and a liquid phase sample to be reacted in a sealed manner and which can be rotated and stirred in a heated state. A filter is attached to the inner end of the liquid extraction hole to allow only the liquid phase to flow out of the container, and a female quick connect is attached to the outer end of the liquid extraction hole. A male quick connect that communicates with the introduction pipe inserted into the inside of the liquid collection bottle is attached, and the female quick connect and male quick connect can be joined liquid-tightly by inserting the male quick connect into the female quick connect. The hydrothermal reaction device is characterized in that the female quick connect is provided with an outflow valve for outflowing the liquid in the container.