JP3500870B2 - High-temperature high-pressure reactor - Google Patents

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a reaction vessel used for high temperature and high pressure reaction, and more particularly to an autoclave suitable for use in the reaction of rock and water.

[0002]

2. Description of the Related Art For example, when rock and water are reacted in a temperature range of 0 to 350 ° C., a saturated vapor pressure at a temperature of 350 ° C. is as high as 167 kgf / cm ² , so that ordinary glass having poor pressure resistance is used. Manufactured reaction vessels cannot be used.
Therefore, conventionally, a metal autoclave such as stainless steel is used, or an autoclave in which a metal tube is coated with a corrosion resistant coating such as gold plating is used.

However, the former has a problem that the metal is corroded by the reaction product, and the latter has a problem that the corrosion resistant coating is peeled off.

[0004]

SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and has no problem of corrosion by reaction products or peeling of coating even under high temperature and high pressure, and is resistant to high temperature and high pressure. It is an object of the present invention to provide a high-temperature and high-pressure reaction vessel which is rich in resistance.

[0005]

In order to achieve the above-mentioned object, in the high temperature and high pressure reaction container of the present invention, a glass reaction container main body in which a substance to be reacted is placed and sealed is made of metal. The protective container is housed in the protective container, and when the reaction container main body is housed in the protective container, a liquid is put into the protective container and the container is openably closed.

This high-temperature high-pressure reaction vessel is particularly suitable for rocks,
It is suitable for use when reacting water or an aqueous solution such as an acidic solution, and an aqueous solution such as water or an acidic solution can be put inside the reaction container body and the protective container. Also, the amount of liquid does not fill the container, and is supplied while maintaining a sufficient space. When the reaction vessel is subjected to high temperature and high pressure in order to cause a reaction of rock-water or the like, the liquid expands, for example, 35
At 0 ° C, the liquid volume is 1.7 times the original amount. However, since the liquid is also contained in the protective container and this liquid also expands, the pressure inside and outside the reaction container body will be balanced, and even if it is made of glass, the reaction container body will be damaged. There is no such thing. Also, since it is not coated, naturally there is no problem such as peeling of the coating, and since the reaction vessel body is made of glass,
Corrosion does not occur due to the reaction target.

In the above, the reaction container body is a cylindrical reaction tube, and the protective container is also a cylindrical protection tube.
It is preferable from the viewpoint of strength and the like. Further, as the glass used for the reaction tube, any composition can be used as long as corrosion resistance, strength, etc. are satisfied, but at the present stage, especially quartz glass or Pyrex glass (soft glass)
Is preferably used. This reaction tube is usually formed by degassing the inside of a cylindrical body with one end sealed and containing the reactant such as rock, while closing the other end with a burner or the like. To do.

On the other hand, the protective tube may be made of any metal as long as it has a certain strength and corrosion resistance, but stainless steel is most preferable from the viewpoint of corrosion resistance.
As the liquid to be put in the protective tube, any liquid may be used as long as it does not corrode the material of the reaction tube and the protective tube, but water or an aqueous solution such as an acidic solution is preferable.

The structure of the protective tube may be any as long as it can accommodate the reaction tube so that the reaction tube can be taken out, and in particular, can maintain a predetermined pressure resistance performance, sealing performance, etc. in the housing sealing portion. A protective tube body having an inner diameter larger than the outer diameter and one end closed and the other end open,
It is preferable that the protective tube body is provided with a sealing plug that is detachably screwed to the other end. In particular, at the other end of the protective tube body, a cylindrical portion having an inner diameter larger than the inner diameter of the protective tube body is formed on the inner side, and on the outer side, a female screw portion is formed by connecting to the cylindrical portion. , A pressing member in which a small-diameter portion is coaxially connected to a large-diameter portion having a diameter substantially the same as the inner diameter of the cylindrical portion while the annular body is brought into contact with the shoulder portion on the inner side of the cylindrical portion. Is fitted to the cylindrical portion while being in contact with the annular body. Then, a through hole into which the small diameter portion of the pressing member can be inserted is formed in the sealing plug, and the sealing plug is screwed into the female screw portion with the small diameter portion of the pressing member inserted into the through hole. Can be configured. Here, the protective tube body, the pressing member, and the sealing plug are preferably made of, for example, stainless steel as described above, but the annular body is preferably made of a metal having a slightly low hardness, for example, copper. Further, it is practical that the outer peripheral surface of the protective tube body is formed with a flat portion for facilitating fixing of the protective tube body to a vise, and the sealing plug has a hexagonal head. Is.

[0010]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings, but these are merely for exemplification and do not limit the invention.

FIG. 1 shows a preferred embodiment of the high temperature and high pressure reaction vessel of the present invention. The high-temperature and high-pressure reaction vessel 1 of the present invention is a glass reaction tube (reaction vessel body) 2 in which an object to be reacted consisting of rock G and water W is put inside and sealed.
And a protective tube (protective container) 3 made of metal, in which the reaction tube 2 and the liquid L are placed in the protective tube 3 made of metal.

The reaction tube 2 has a cylindrical shape, and has a structure in which the other end 5 is closed while the above-mentioned reactant is put inside a cylindrical body whose one end 4 is closed. In this reaction tube 2, for example, a middle portion of a glass cylinder having a predetermined length, one end of which is closed and the other end of which is open, is squeezed by using a burner, and the inside is degassed from the other open end. Is completed by closing the end of the reaction tube so that it becomes the other end of the reaction tube.
Reactants, etc. are put into the pipe at an appropriate time, for example, before narrowing down the intermediate portion. The reaction tube 2 is made of glass because it requires corrosion resistance, but quartz glass or Pyrex glass is preferably used from the viewpoint of resistance to high temperature and high pressure.

The protection tube 3 has an inner diameter larger than the outer diameter of the reaction tube 2 and has a protection tube body 6 with one end 6a closed and the other end open, and the other end 6b of the protection tube body 6. It comprises a sealing plug 7 that is detachably screwed, and is made of metal, preferably stainless steel. Also,
The protection tube body 6 has a length sufficient to accommodate the reaction tube 2 in the coaxial state, and an inner diameter sufficient to spread the liquid around the outer circumference of the reaction tube 2.

Further, as shown in detail in FIG. 2, a cylindrical portion 8 having an inner diameter slightly larger than the inner diameter of the protective tube body 6 is formed on the inner side at the other end 6b of the protective tube body 6. And is connected to the cylindrical portion 8 on the outer side to form a female screw portion 9
Are formed. And, in the inner back of the cylindrical portion 8,
A washer or ring (packing), preferably made of copper
10 is provided so as to abut on an inner shoulder of the cylindrical portion 8, and a pressing member 11, which is also preferably made of stainless steel, is fitted in the cylindrical portion 8. The pressing member 11 comprises a large-diameter portion 11a coaxially connected to a large-diameter portion 11a having the same diameter and the same length as the inner diameter of the cylindrical portion 8, and the outer peripheral side of the end face of the large-diameter portion 11a. It is fitted into the cylindrical portion 8 while being in contact with the annular body 10.

The sealing plug 7 has a hexagonal head portion 7a connected to a male screw portion 7b so that it can be easily rotated by a tool. The small diameter portion 11b of the pressing member 11 is inserted through the shaft 7a. A through hole 7c extending in the direction is provided. Then,
The sealing plug 7 has a male screw portion 7b and a female screw portion 9 in a state where the small diameter portion 11b of the pressing member 11 is inserted into the through hole 7c.
It is detachably attached to the protective tube body 6 by being screwed into.

In the present invention, when the reaction tube 2 is inserted into the protection tube 3, it is particularly necessary to put not only the reaction tube 2 but also the liquid L into the protection tube 3. The liquid L is water or an aqueous solution such as an acidic solution, for example, 3
It is set to an appropriate amount in consideration of the fact that the liquid amount expands about 1.7 times the initial amount during the reaction at 50 ° C.

Further, on the outer peripheral surface of the protective tube body 6,
For example, a pair of flat portions 6c for facilitating the fixing of the protective tube body 6 with a vise are formed so as to face each other in the diametrical direction.

In the high-temperature and high-pressure reaction vessel according to the above embodiment, water or an aqueous solution such as an acidic solution is put inside the reaction tube 2 and the protection tube 3, but the liquid amount in both the reaction tube 2 and the protection tube 3 is large. Does not fill the tube, but is inserted with a sufficient space maintained. If the reaction vessel is subjected to high temperature and high pressure in order to cause a reaction between rock and water,
The liquid expands, and at about 350 ° C the liquid volume is about 1.7
It doubles. However, the liquid L of water or an aqueous solution such as an acidic solution is also contained inside the protective tube 3, and this liquid L expands similarly to the liquid in the reaction tube 2, so that the reaction tube 2
The pressures inside and outside the chamber are kept balanced, and the reaction tube 2 will not be damaged even if it is made of glass. Further, since the reaction tube 2 is made of glass, it will not be corroded by the reaction target.

FIG. 3 shows a modified example of the high-temperature and high-pressure reaction container according to the present invention, which has the same structure as that already described except for the part described below. That is, in this modification, the portion of the protective tube body 6 with which the annular body 10 abuts and the portion of the pressing member 11 with which the annular body 10 abuts have a mountain-shaped (triangular) cross section, for example, about 1 mm. The annular protrusions 12 and 13 each having a height of 1 are formed. In addition, in the illustrated example, one protrusion (the protrusion 12 in the illustrated example) has a larger diameter than the other protrusion (the protrusion 13 in the illustrated example), but the protrusions may have the same diameter. Of course it doesn't matter. By providing the protrusions 12 and 13, the annular body 10 is completely protected by the protection tube body 6 and the pressing member 1.
1, so that there is no risk of leakage of water vapor from the contact part between the ring-shaped body 10 and the protection tube body 6 and the contact part between the ring-shaped body 10 and the pressing member 11, and the seal is made more complete. be able to.

In the above embodiment, both the reaction vessel and the protective vessel are tubular bodies, but other shapes can be manufactured. Also, the structure for closing the protective tube may be of any structure as long as pressure resistance and sealing performance can be secured.

[0021]

As described above, in the high temperature and high pressure reaction container of the present invention, the reaction container body made of glass, in which the reactant is put and sealed, is housed in the metal protection container. In addition, when the reaction container body is housed in the protective container, the liquid is put inside the protective container and sealed so that it can be opened. Therefore, when used to react rocks with water or an aqueous solution, for example, the reaction Even if the container is subjected to high temperature and high pressure, the external liquid expands as well as the liquid inside the reaction container body, so the pressure inside and outside the reaction container body will be balanced. Will not be damaged.

Further, since it is not coated, there is naturally no problem such as peeling of the coating, and since the reaction container body is made of glass, it will not be corroded by the reaction target.

[Brief description of drawings]

FIG. 1 is a partial cross-sectional view of a high temperature and high pressure reaction container according to the present invention.

FIG. 2 is a partially cutaway sectional view in which a part of FIG. 1 is enlarged.

FIG. 3 is a developed cross-sectional view of a part of a high temperature and high pressure reaction container according to a modification of the present invention.

[Explanation of symbols]

1 High temperature and high pressure reactor 2 Reaction tube (reaction container body) 3 Protection tube (protection container) 6 Protection tube body 7 Sealing plug 10 ring 11 Pressing member 12 Projections 13 Projection

─────────────────────────────────────────────────── ───Continued from the front page (56) Reference JP-A 63-45196 (JP, A) JP-A 8-162423 (JP, A) JP-A 7-284650 (JP, A) JP-A 52- 85981 (JP, A) (58) Fields surveyed (Int.Cl. ⁷ , DB name) B01J 3/00-3/08

Claims (10)

(57) [Claims] 1. A reaction container body made of glass, in which a substance to be reacted is placed and hermetically sealed, is housed in a metal protection container, and the protection container can be opened with a liquid inside. A high-temperature and high-pressure reaction vessel, which is hermetically sealed. 2. The high-temperature high-pressure reaction vessel according to claim 1, wherein the reaction vessel body is a reaction tube, and the protection vessel is a protection tube. Wherein the reactants, rocks and, high-temperature high-pressure reaction vessel according to claim 1 or 2 is water or an aqueous solution. 4. The reaction tube is formed by degassing the inside of a tubular body with one end sealed and the other end sealed while degassing the inside. Or 3
The high-temperature, high-pressure reaction vessel according to. 5. The protective tube has an inner diameter larger than the outer diameter of the reaction tube, one end is sealed and the other end is open, and a screw is detachably attached to the other end of the protective tube body. The high-temperature high-pressure reaction vessel according to any one of claims 2 to 4, further comprising: 6. The protective tube comprises at least a protective tube main body, an annular body, a pressing member, and a sealing plug, the protective tube main body having an inner diameter larger than an outer diameter of the reaction tube and one end thereof. Is closed and the other end is opened, and at the other end, a cylindrical portion having an inner diameter larger than the inner diameter of the protective tube main body, and an internal thread portion provided so as to be connected to the cylindrical portion on the axially open side of the cylindrical portion. The pressing member is provided with a large-diameter portion having substantially the same diameter as the inner diameter of the cylindrical portion, and connected to the large-diameter portion on the axially open side of the large-diameter portion.
And a vignetting small-diameter portion, the sealing plug, the small diameter portion of the pressing member has an insertion which can be holes, the annular body is in contact with the shoulder portion of the inner back of the cylindrical portion, the The pressing member is fitted into the cylindrical portion in a state where the large diameter portion is in contact with the annular body, and the sealing plug is screwed to the female screw portion in a state where the small diameter portion of the pressing member is inserted into the through hole. The high-temperature high-pressure reaction vessel according to any one of claims 2 to 4, wherein 7. The portion of the protection tube body with which the annular body abuts and the portion of the pressing member with which the annular body abuts are projections having a mountain-shaped cross section, respectively. The high temperature and high pressure reaction vessel described. 8. A peripheral surface of the protective tube body, the flat portion is formed to facilitate fixing of the protective tube body, to the closed stopper claims 5 having a hexagonal-shaped head 7 either 1 The high-temperature high-pressure reaction vessel according to the item . 9. The high-temperature high-pressure reaction container according to claim 6, wherein the protection tube body, the pressing member and the sealing plug are made of stainless steel, and the annular body is made of copper. 10. The high-temperature and high-pressure reaction vessel according to claim 3, wherein the aqueous solution that reacts with rock and the liquid that is put into the protective tube are acidic aqueous solutions.