JPS60235633A - High-pressure reactor - Google Patents

Abstract

PURPOSE:To prevent the leakage of reaction products or the like at the time of oscillation of the titled reactor and to prevent the corrosion of the reactor by stirring reaction materials through subjecting the horizontal type high-pressure reactor to oscillating movement and providing a prevention valve for liquid flow- out in the high-pressure reaction part. CONSTITUTION:The titled high-pressure reactor is constituted of a cylindrical reaction vessel 1, a spindle 2 formed with a path 21 of reaction gas therein, a washer 3 for pushing packings, packings 4, a setscrew 5, an auxiliary flange 6, a washer 7, a hexagon socket head bolt 8 and a spring 9. Further, a prevention valve 18 for liquid flow-out by which the flow-out of reaction liquid is prevented is provided to the lower part of the spindle 2 in a high-pressure reaction part 20. The prevention valve 18 is screwed with a screw part 18A into the lower part of the spindle 2 and also reaction gas G is introduced from a gas path 18B communicated with the reaction gas path 21.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a high-pressure reactor, particularly a high-pressure reactor that performs a reaction of hydrogen and carbon oxide at high pressures up to several thousand atmospheres in the coexistence of liquids, solids, etc. It is something.

[Prior art]

There are many technical difficulties in carrying out reactions involving hydrogen, carbon oxide, etc. under high pressures of over 1,000 atmospheres, and there have been many improvements to be made in the reactor materials, airtight systems, stirring methods, etc. .

On the other hand, high-pressure reactors usually accelerate the reaction by
Equipped with a stirrer to stir contents such as gases, liquids, and solids, reaction equipment with reaction pressures ranging from diffuse pressure to several hundred atmospheres usually uses induction rotary stirring using a motor or stirring using a magnetic stirrer. However, when the reaction pressure exceeds 1000 atm, the wall thickness of the reactor container increases, and the difficulty of using the stirrer's wheel technology. It becomes difficult to use.

If the above stirring method is not appropriate, a swinging type stirring device as shown in Figures 1 and 2 is used, with Figure 1 being a vertical type and Figure 2 being a horizontal type. Each swings in the direction of arrow S.

However, in the case of a high-pressure reaction vessel that is designed to be elongated and have a small inner diameter in order to withstand high pressure, the vertical stirring device 28 in FIG. 1 has a small stirring effect.
In addition, in the case of the horizontal borrowing device [29] shown in Fig. 2, the reaction liquid flows out to the lead pipe, gauge, etc. outside the reaction vessel main body,
It has the disadvantage that it is difficult to obtain accurate reaction results.

On the other hand, since high-pressure hydrogen, carbon oxide, etc. have a corrosive effect on metal materials, such as hydrogen embrittlement, conventional materials such as Hastelloy-276 and SUS have been used as reactor materials for these high-pressure gases at about 1000 atmospheres. -316 stainless steel and other materials are being used, but these materials do not have sufficient strength under high pressures exceeding 1,000 atmospheres, and using these materials increases the wall thickness of the reaction vessel and makes handling difficult. It was not practical because it was not easy.

[Purpose of the invention]

The present invention has been made to solve the above-mentioned conventional drawbacks, and is designed to prevent reaction products from leaking out when a horizontal high-pressure reactor is used, which has a greater stirring effect than a vertical type. It is an object of the present invention to provide a high-pressure reactor that can sufficiently ensure airtightness of a reaction vessel during reaction, prevent corrosion of the reaction vessel, and obtain efficient reaction results.

[Structure of the invention]

That is, the high-pressure reactor of the present invention is constructed by using a horizontal high-pressure reactor, stirring the reactants by swinging the high-pressure reactor, and providing a liquid outflow prevention valve in the high-pressure reaction section. The liquid outflow prevention valve provided in the high-pressure reaction section is provided with stop valves at the inflow and outflow portions of the reaction gas, and also includes a reaction vessel that forms the high-pressure reaction section and a spindle that forms a reaction gas passage therein. It is also preferable that a gasket is provided between the spindle and the gasket, and that at least a portion of the contact portion between the gasket and the spindle is in surface contact.

Further, in the present invention, it is also desirable that at least the reaction vessel and the spindle are made of a corrosion-resistant and heat-resistant nickel-based alloy.

〔Example〕

The present invention will be described in detail below with reference to the drawings, and FIG. 3 is a cross-sectional view of a high-pressure reactor in one embodiment of the present invention.
This is a horizontal swinging type stirring device 2 as shown in Figure 2.
9 and is used by swinging it in the direction of the arrow S to effectively stir the reactants filled in the high-pressure reaction section 20.

In the high-pressure reactor shown in FIG. 3, 1 is a cylindrical reaction vessel, 2 is a spindle in which a reaction gas passage 21 is formed, 3f'i is a cylinder for pushing a gasket, !
,+-・CR訃↓C口】→- Category Right-hand movement flap/ji, 7 is a washer, 8 is a hexagon socket bolt, and 9 is a spring.

The outer thread of the push screw 5 is in contact with the inner thread of the inlet of the reaction vessel 1, and the inner thread of the auxiliary flange 6 is in contact with the outer thread of the upper part of the spindle 2.

Further, about 6 to 10 hexagon socket head bolts 8 are attached to the auxiliary flange 6 in an annular manner, the lowest part of the hexagon socket head bolt 8 is in contact with the upper part of the washer 7, and the spring 9 is attached to the push screw 5. It is inserted into an annular groove on the upper surface of the holder, and is held between a set screw 5 and a washer 7.

Furthermore, as shown in FIG. 3, the high-pressure reaction apparatus of the present invention is provided with a liquid outflow prevention valve 18 at the bottom of the spindle 2 in the high-pressure reaction section 20 to prevent the reaction liquid from flowing out. The outflow prevention valve 18 is screwed into the lower part of the spindle 2 with a threaded portion 18A, as shown in FIG.
is about to be introduced.

Further, at the tip of this liquid outflow prevention valve 18, the gas passage 18B and an inflow section 18C for the reaction gas G into the high pressure reaction section 20 are provided.
A stop valve 18E consisting of a valve body 24 pressed by a tin ring 26 is provided between the gas passage 18B and the gas passage 18B.
A stop valve 18F consisting of a valve 26, which is pressed by a spring 25, is provided between the outflow portion 18D of the reaction gas G from the high-pressure reaction portion 20.

Therefore, when pressurizing the high-pressure reaction gas G into the high-pressure reaction section 20 filled with a catalyst and solvent in advance through the liquid outflow prevention valve 18, the reaction gas G is transferred to the valve body 2 of the inflow section 18C.
While pushing back the spring 23 of 4, the high pressure reaction part 20
However, once the high-pressure reaction section 20 is filled with the reaction gas G, it does not return to the reaction gas passage 21 side due to the action of stop valves 18E and 18F provided in the inflow section 18C and outflow section 18D, respectively.

Therefore, when a reaction is carried out at a constant temperature while swinging horizontally as shown in Fig. 2, even if this high-pressure reactor is turned downward, the reaction product liquid in the high-pressure reaction section 20 will not react with the spindle 2. It is possible to prevent leakage to the outside via the gas passage 21.

Next, FIG. 4 is an enlarged view of the contact area of the reaction vessel 1, the spindle 2, and the packing 4. The reaction vessel 1 has a seven-shoulder shoulder facing the center on the inner wall, and the packing 4 is attached to the surface 12 of this shoulder. is in contact with the outer surface 16 of.

It has two spindles that point outward from the center,
At least a portion of the shoulder surface 11 is in surface contact with the inner surface 10 of the packing 4.

Figure 5 shows the plane 10 relative to the straight line passing through the center of the spindle 2.
and the angle α of the surface 11 and the angle β of the surface 11 are shown.

Here, the material of the above-mentioned cylindrical reaction vessel 1 and spindle 2 is a nickel-based alloy-based corrosion-resistant and heat-resistant alloy (for example, AS
This material is stronger than the conventionally used Hastelloy 276 and stainless steel, and has heat and corrosion resistance. By using materials such as K,
The reactor can be made smaller and easier to handle.

High-pressure reactors are normally used under heating from room temperature to several hundred degrees Celsius.
The thermal expansion of the materials differs due to the difference in materials, and the difference in thermal expansion causes leakage of the reactor.

Therefore, in order to maintain airtightness, it is necessary to
It is also necessary to maintain good contact with the spindle 2.

Therefore, the surface 11 of the spindle 2 and the surface 10 of the packing 40 are brought into contact with each other, and pressure for maintaining airtightness is obtained by tightening the auxiliary flange 6.

1. By tightening hexagon socket head bolt 8.

The contact of the contact surfaces 10, 11 between the seal 4 and the spindle 2 is strengthened, and the spring 9 also strengthens the surface contact at this contact surface 10,11.

For airtightness, the angles α and β shown in FIG. 4 and the spindle 2 are brought into surface contact at least in part.

In addition, by tightening the set screw 5, the surface 1 of the reaction container 1 can be tightened.
2 and the surface 16 of the seal 4 come into contact.

The lower part 14 of the gasket 4 expands outward, and the surfaces 16 and 12
A force which further strengthens the contact is obtained by pulling the spindle 2 upwards.

〔Effect of the invention〕

The high-pressure reactor of the present invention as described above has a horizontal oscillating motion, so it can stir the reactants more effectively than a vertical type. Since a prevention valve is provided, there is an advantage that there is no risk of reaction products etc. leaking outside even though it is a horizontal type.

1. Sufficient airtightness can be maintained by making surface contact between the gasket provided between the reaction container and the spindle forming the reaction gas passage and the spindle.

Furthermore, if the reaction vessel and spindle are made of a nickel-base alloy-based corrosion-resistant and heat-resistant alloy, the high-pressure reactor can be made smaller than hK, and handling becomes easier.

Therefore, by employing the high-pressure reactor of the present invention as described above, the disadvantages of stirring, airtightness, and materials in conventional high-pressure reactors can be improved, and reactions can be carried out efficiently.

[Brief explanation of the drawing]

Fig. 1 is a front view of a vertical oscillating type stirring device of a conventional reaction apparatus, and Fig. 2 is a front view of a horizontal oscillating type stirring device.
FIG. 3 is a longitudinal cross-sectional view of the reaction vessel of the reaction apparatus in the embodiment of the present invention, FIG. 29... Stirring device, G... Reaction gas.

Claims (1)

[Scope of Claims] 1. A high-pressure reactor characterized in that the high-pressure reactor is horizontal, the reactants are stirred by shaking the reactor, and a liquid outflow prevention valve is provided in the high-pressure reaction section. 2. The high-pressure reaction device according to claim 1, wherein the liquid outflow prevention valve provided in the high-pressure reaction section is provided with stop valves at the inlet and outlet of the reaction gas, respectively. 3. A patent claim in which a gasket is provided between a reaction vessel forming a high-pressure reaction section and a spindle forming a reaction gas passage therein, and at least a portion of the contact area between the gasket and the spindle is surface contact. The high-pressure reactor according to item 1 or 2. 4. The high-pressure reactor according to claim 1, 2, or 3, wherein at least the materials of the reaction vessel and the spindle have been inspected by the Nickel Subcommittee and Co., Ltd.