JP6595328B2 - Reactor - Google Patents

Description

  The present invention relates to a reaction apparatus, and more particularly, to a reaction apparatus that introduces a stock solution and hydrogen gas into a reaction column packed with a hydrogenation catalyst and causes a hydrogenation reaction.

  As a reaction apparatus that introduces a stock solution and hydrogen gas into a reaction column packed with a hydrogenation catalyst and performs a hydrogenation reaction, a reaction apparatus that holds the reaction column with a toggle structure in a reaction column packed with a hydrogenation catalyst is known. (For example, refer to Patent Document 1).

JP 2010-112907 A (FIG. 7)

  The reaction apparatus described in Patent Document 1 is effective when a single reaction column is used. However, when the operation is performed while replacing a plurality of reaction columns, it takes time to replace the reaction columns. was there. In addition, there is a difficulty in controlling the temperature of the reaction column.

  Accordingly, an object of the present invention is to provide a reaction apparatus that can easily exchange reaction columns when using a plurality of reaction columns, and that can easily and reliably control the temperature of the reaction columns.

  In order to achieve the above object, the reaction apparatus of the present invention is a reaction apparatus in which a stock solution and hydrogen gas are introduced into a reaction column packed with a hydrogenation catalyst to perform a hydrogenation reaction, and a thermostat holding the reaction column; The reaction column is filled with a hydrogenation catalyst in advance in a straight tube having a predetermined length and holds the hydrogenation catalyst at both ends in the column. The thermostat bath has a metal main body, a column insertion hole formed through the main body in the vertical direction, and an outlet side provided on the lower outlet side of the column insertion hole. A holding member, column pushing means for pushing the reaction column toward the lower outlet side, and heating means inserted into the main body, wherein the reaction column is an outlet side column provided on the lower outlet side. An end is held by the outlet side holding member, an inlet side column end provided on the upper inlet side is pushed by the column pushing means, and the column pushing means has a holding position that covers the column insertion hole. A holding lid that can be rotated to an open position, an opening / closing operation lever that opens and closes the holding lid, and a biasing means that pushes the inlet side column end toward the reaction column when the holding lid is in the holding position. The outlet column end includes a circular recess into which the lower end of the reaction column is inserted, and an outlet end surface O-ring that is provided on the outer periphery of the bottom surface of the circular recess and is in close contact with the lower end of the reaction column, The inlet-side column end includes a circular recess into which the upper end of the reaction column is inserted, and an inlet end surface O-ring that is provided on the outer periphery of the bottom surface of the circular recess and is in close contact with the upper end of the reaction column. It is characterized in.

  Furthermore, in the reaction apparatus of the present invention, the reaction column has an outer diameter corresponding to the inner diameter of the column insertion hole, and the inner diameter corresponds to the outer diameter of the reaction column via a cylindrical adapter. The inserted cylindrical adapter is characterized in that it has a length that is flush with the lower end of the column insertion hole when inserted into the column insertion hole. In addition, the reaction column is made of metal, and a circumferential groove is provided in a circumferential direction of the outer circumference on the inlet side of the column, and an inlet fitted in the circumferential groove on an inner circumferential surface of a circular recess of the inlet side column end A circumferential O-ring is provided.

  According to the reaction apparatus of the present invention, the reaction column is filled with a hydrogenation catalyst in advance, and a reaction column in which a filter for holding the hydrogenation catalyst in the column is press-fitted at both ends is used. Column handling is greatly improved. Also, the coupling and sealing of the reaction column to the outlet side column end and the inlet side column end are not performed by a screw structure, and the column pushing means pushes the inlet side column end and reaction column through the biasing means. Since it only needs to be pushed toward the outlet side column end by the means, the reaction column and the quantity column end can be easily combined and sealed. Furthermore, since the reaction column can be taken out from the column insertion hole by releasing the pushing of the reaction column by the column pushing means, the reaction column can be easily replaced without releasing the screw connection. be able to.

It is a cross-sectional side view which shows one example of the thermostat in the reaction apparatus of this invention. It is a side view similarly. It is also a front view. It is a front view of the principal part which shows the state which opened the control lid | cover. It is VV sectional drawing of FIG. It is a disassembled perspective view around a reaction column. It is a perspective view which shows the reaction apparatus which accommodated the thermostat. Similarly, it is a cross-sectional plan view. It is a cross-sectional side view which shows an example using the reaction column from which a diameter differs. It is a cross-sectional side view of the principal part which shows the other example of a thermostat in the reaction apparatus of this invention.

  The reaction column 11 used in the reaction apparatus shown in the present embodiment is for filling the hydrogenation catalyst 12 in a stainless steel straight pipe and holding the hydrogenation catalyst 12 in the column at both ends of the straight pipe. Each of the filters 13 and 13 is press-fitted, and a circumferential groove 11 a is formed on the outer peripheral surface of the reaction column 11 on the inlet side.

  The thermostatic chamber 14 holding the reaction column 11 includes a main body portion 15 made of a rectangular parallelepiped metal block, a column insertion hole 16 penetratingly formed in the vertical direction on the front side from the center of the main body portion 15, and the column. An outlet side holding member 17 provided on the lower outlet side of the insertion hole 16 and a column pushing means 18 for pushing the inlet side of the reaction column 11 toward the outlet side are provided. Further, a heater 19, a temperature fuse 20, and a temperature sensor 21 that constitute a heating unit for heating the reaction column 11 are inserted on the rear side of the main body 15.

  The column pushing means 18 forms a four-node toggle link structure, and the holding lid 22 is rotatably connected to the upper end portion of the rear end side of the main body portion 15 by a horizontal rotation shaft 22a. A link lever 23 rotatably connected to both front and rear middle side surfaces of the main body portion 15 by a horizontal rotation shaft 23a, a rotation end of the holding lid 22 and a rotation end of the link lever 23; Are provided with an opening / closing operation lever 24 that is rotatably connected by horizontal rotation shafts 24a and 24b.

  The restraining lid 22 is formed so as to rotate horizontally from the restraining position covering the upper side of the column insertion hole 16 to the open position rising in the vertical direction with respect to the upper surface of the main body 15. The lever 23 is formed to rotate from a lower lock position rotated downward with respect to the rotation shaft 23a to an upper lock position rotated upward. The holding lid 22 is provided with a U-shaped component insertion groove 22b having an opening on the rotating end side.

  In the opening / closing operation lever 24, a handle portion 24c provided at the rotation end of the opening / closing operation lever 24 passes through the front of the main body portion 15, the holding lid 22 is held down, and the link lever 23 is in the lower locking position. From the column holding position, the holding lid 22 is formed to rotate to the open position, and the link lever 23 is rotated to the column attaching / detaching position of the upper lock position. When the opening / closing operation lever 24 is rotated from the column attaching / detaching position to the column holding position, the rotating shaft 24 b connected to the tip of the link lever 23 is linked to the rotating shaft 24 a connected to the tip of the holding lid 22. It is set so that it rotates beyond the straight line connecting the rotation axis 23a of the lever 23 from the front to the rear, that is, after the rotation exceeds the dead point of the link lever 23 and stops at the column holding position. ing.

  Further, when the restraining lid 22 rotates from the restraining position to the open position, the restraining lid 22 and the link lever 23 are located behind the vertical line through which the rotation end of the restraining lid 22 passes through the rotation shaft 22a. The link lever 23 is set so that the rotation end of the link lever 23 rotates beyond a vertical line passing through the rotation shaft 23a. That is, in the open position of the holding lid 22, the holding lid 22 and the link lever 23 are set so as to be located behind the top dead center with respect to the rotation shafts 22a and 23a.

  On the other hand, the reaction column 11 is inserted into the column insertion hole 16 via a cylindrical adapter 25 whose outer diameter corresponds to the inner diameter of the column insertion hole 16 and whose inner diameter corresponds to the outer diameter of the reaction column 11. The An inlet side column end 26 through which a raw material introduction hole 26 a having a diameter smaller than the inner diameter of the reaction column 11 passes is provided on the upper inlet side of the reaction column 11, and a diameter smaller than the inner diameter of the reaction column 11 is provided on the lower outlet side. An outlet side column end 27 is provided through which a reactant outlet hole 27a having a through-hole passes.

  A large-diameter insertion portion 16a into which a large-diameter outer peripheral portion 25a formed at the upper portion of the cylindrical adapter 25 is inserted is provided at the upper portion of the column insertion hole 16, and the lower surface of the large-diameter outer peripheral portion 25a of the cylindrical adapter 25 is provided. When the cylindrical adapter 25 is inserted into the column insertion hole 16 from above and the lower surface of the large-diameter outer peripheral portion 25a comes into contact with the positioning step portion 16b, a cylindrical step 25 is provided. The lower end of the cylindrical adapter 25 is formed to be flush with the lower end opening of the column insertion hole 16. Further, a circumferential groove 25 b is provided on the outer periphery of the upper end portion of the large-diameter outer peripheral portion 25 a of the cylindrical adapter 25 to be a handle portion when the cylindrical adapter 25 is extracted from the column insertion hole 16.

  Further, the outlet side holding member 17 detachably attached to the lower end portion of the main body part 15 with two screws (not shown) has a U-shape in a plan view in which a part holding the outlet side column end 27 is opened at the front. The outlet side column end 27 is detachable from the front. In addition, the upper surface of the outlet side holding member 17 is provided with a fitting recess 17a in which a flange portion 27b provided on the outer periphery of the upper end of the outlet side column end 27 is fitted, and the outlet side column end 27 is positioned. It can be held in a state.

  A female screw hole 27 c for screwing an outlet-side connector 29 that connects the reaction solution outlet pipe 28 to the outlet-side column end 27 is provided at the lower portion of the outlet-side column end 27. In addition, a circular concave portion 27d into which the lower end of the reaction column 11 protruding from the lower end of the cylindrical adapter 25 is inserted is provided at the upper portion of the outlet side column end 27, and a reaction is provided on the bottom outer periphery of the circular concave portion 27d. An outlet-side O-ring mounting groove 27e for mounting the outlet end surface O-ring 30 that is in close contact with the lower end of the column 11 is provided in a ring shape.

  On the other hand, on the inlet side of the reaction column 11, the inlet side column end 26, a coil spring 31 which is an urging means disposed on the outer periphery of a small diameter portion 26b provided on the upper side of the inlet side column end 26, and the The holding lid 22 holds the coil spring 31 through an inlet-side cap 32 that covers the upper portion of the coil spring 31 and has a through hole 32 a that passes through the upper portion of the inlet-side column end 26. The upper inner periphery of the cylindrical adapter 25 is provided with a medium-diameter inner peripheral portion 25c into which the inlet-side column end 26 is inserted and a large-diameter inner peripheral portion 25d into which the inlet-side cap 32 is inserted. The inlet side column end 26 is provided with a circular recess 26c into which the upper end of the reaction column 11 is inserted at the lower part, and an inlet side connector 34 for connecting the raw material supply pipe 33 to the inlet side column end 26 is screwed to the upper part. A female screw hole 26d is provided.

  In addition, an inlet-side O-ring mounting groove 26e for mounting an inlet end surface O-ring 35 that is in close contact with the upper end of the reaction column 11 is provided in a ring shape on the outer periphery of the bottom surface of the circular recess 26c. On the peripheral surface, a peripheral surface O-ring mounting groove 26f for mounting an inlet peripheral surface O-ring 36 that can be fitted in the peripheral groove 11a of the reaction column 11 is provided in the circumferential direction. When the inlet side of the reaction column 11 is inserted into the circular recess 26c of the inlet side column end 26, the inner peripheral portion of the inlet peripheral surface O-ring 36 is fitted into the peripheral groove 11a. The space between the inner peripheral surface of the circular recess 26 c and the outer peripheral surface of the reaction column 11 is sealed. In addition, since the inner and outer sides of the inlet peripheral surface O-ring 36 are fitted in the grooves 11a and 26f, the reaction column 11 and the inlet-side column end 26 are integrated.

  The coil spring 31 is configured to push the inlet side column end 26 to the reaction column 11 with a preset pressing force when the holding lid 22 is rotated to the holding position. By pushing and pressing the inlet side column end 26 with a strong pressure higher than the pressure, the inlet end of the reaction column 11 is brought into close contact with the inlet end surface O-ring 35, and the outlet end of the reaction column 11 is connected to the outlet end surface O-ring 30. Adhere closely.

  Further, the lower end portion of the small-diameter portion 26b is formed to have a slightly larger diameter to provide a coil spring engaging portion 26g, and the inner periphery of the lower end of the coil spring 31 is engaged with the coil spring engaging portion 26g. The end 26 and the coil spring 31 can be integrated. Further, the upper inner periphery of the inlet side cap 32 is formed to have a slightly smaller diameter to provide a coil spring engaging portion 32b, and the upper end outer periphery of the coil spring 31 is engaged with the coil spring engaging portion 32b. 32 and the coil spring 31 can be integrated. Thereby, the reaction column 11, the inlet side column end 26, the coil spring 31, and the inlet side cap 32 can be integrated.

  The thermostat 14 formed in this way is accommodated in the heat retaining case 51 shown in FIGS. The heat insulating case 51 is provided with a rectangular tube shaped thermostatic chamber accommodating portion 52 that accommodates the thermostatic chamber 14 in the center in the vertical direction, and between the inner and outer partition walls 53 a and 53 b provided around the thermostatic chamber accommodating portion 52. The heat insulating case 51 is provided with an opening 51a for attaching / detaching the thermostatic chamber 14 and an outer lid 55 for opening / closing the opening 51a. Yes. Between the outer partition wall 53 b and the outer wall 56, a ventilation path 57 having ventilation holes 57 a at the top and bottom is provided in order to prevent the temperature of the outer wall 56 from rising.

  In addition, the outer lid 55 is provided with a pipe insertion portion 55a for inserting a pipe connected to the reaction column 11 from the central portion of the outer lid to the front end portion. Further, a slit 51b for allowing the opening / closing operation lever 24 to pass is provided from the front wall to the upper wall of the heat retaining case 51, and a handle portion of the opening / closing operation lever 24 is provided at the center of the front wall of the heat retaining case 51. A handle portion 58 is provided in a state facing 24c. Further, fixing poles 59 used for fixing the reaction apparatus to a stand or the like are provided above and below the rear surface of the heat retaining case 51. Lead wires 60 connected to heaters, sensors, etc. are provided on the rear surface and the bottom surface. An outlet (not shown) for pulling out the reaction liquid outlet pipe 28 is provided.

  Next, the procedure for using the reaction apparatus will be described. First, a predetermined number of reaction columns 11 filled with the hydrogenation catalyst 12 and press-fitted with filters 13 and 13 are prepared in advance, and a cylindrical adapter 25, an inlet-side column end 26, an outlet corresponding to the shape of the reaction column 11 are prepared. A side column end 27, a coil spring 31, and an inlet side cap 32 are prepared. An inlet end surface O-ring 35 and an inlet peripheral surface O-ring 36 are mounted on the inlet-side column end 26, and a raw material supply pipe 33 for introducing a raw solution and hydrogen gas is provided with a coil spring 31 and an inlet-side cap 32. In the state of being inserted through the connector, the connection is made through the inlet side connector 34. Similarly, an outlet end surface O-ring 30 is attached to the outlet side column end 27, and a reaction liquid outlet pipe 28 for leading a reaction product is connected via an outlet side connector 29.

  After the outlet-side column end 27 is inserted into the outlet-side holding member 17 of the main body 15 from the front and positioned by fitting the flange 27b into the fitting recess 17a, the opening / closing operation lever 24 is turned upward to restrain it. With the lid 22 in the open position, the cylindrical adapter 25 is inserted into the column insertion hole 16 from above. Further, the reaction column 11 is inserted into the cylindrical adapter 25 with the circumferential groove 11a on the upper side, and then the inlet side column end 26, the coil spring 31 and the inlet side cap 32 are arranged on the upper side of the reaction column 11. To do. Thereby, the inlet side of the reaction column 11 protrudes into the inner diameter inner peripheral portion 25 c of the cylindrical adapter 25 and is loosely inserted into the circular concave portion 26 c of the inlet side column end 26. Projecting from the lower end of the cylindrical adapter 25 is loosely inserted into the circular recess 27d of the outlet side column end 27.

  At this time, since the holding lid 22 and the link lever 23 are in positions exceeding the top dead center, the holding lid 22 is automatically held in the open position, and is moved downward to the handle portion 24c of the opening / closing operation lever 24 in the column attaching / detaching position. The opening / closing operation lever 24 does not rotate even when a pressing force is applied to the valve, and the components such as the reaction column 11 can be easily set.

  After completing the setting of each component such as the reaction column 11, the handle 24c of the opening / closing operation lever 24 is slightly pulled forward and then rotated downward to rotate the opening / closing operation lever 24 to a predetermined column holding position. Let At this time, the raw material supply pipe 33 and the inlet-side column end 26 protruding above the thermostatic chamber 14 protrude above the restraining lid 22 through the component insertion groove 22b.

  As a result, the holding lid 22 rotates from the open position to the holding position, and the holding lid 22 pushes the inlet side column end 26 toward the reaction column 11 via the inlet side cap 32 and the coil spring 31. The inlet side of the reaction column 11 passes through the inner peripheral surface of the inlet peripheral surface O-ring 36 while sliding, and the end surface is crimped to the inlet end surface O-ring 35, and the inner periphery of the inlet peripheral surface O-ring 36 is in the peripheral groove 11a. The inlet column end 26 and the inlet side of the reaction column 11 are coupled and sealed.

  At the same time, the outlet side of the reaction column 11 is pushed into the outlet side column end 27, the end surface is crimped to the outlet end surface O-ring 30, and the outlet side column end 27 and the outlet side of the reaction column 11 are joined and sealed. become. At the same time, the inner peripheral portions of the outlet-side O-ring mounting groove 27e and the inlet-side O-ring mounting groove 26e support the filters 13 and 13 that are press-fitted into both ends of the reaction column 11, so that pressure is applied during operation. However, the filters 13 and 13 are prevented from coming out of the reaction column 11.

  Further, when the holding lid 22 is rotated to the holding position, the force by which the holding lid 22 presses the handle portion 24c with respect to the force by which the holding lid 22 compresses the coil spring 31 can be reduced due to the lever principle. When the coil spring 31 having a large spring constant is used, the opening / closing operation lever 24 can be operated with a light force to rotate the holding lid 22 to the holding position. Further, since the opening / closing operation lever 24 is rotated to the column holding position beyond the dead point of the link lever 23 and is locked by the restoring force of the coil spring 31, the opening / closing operation lever 24 is Even if a hand touches or some vibration is applied, the open / close operation lever 24 is held in the column holding position, so that the reaction column 11 is held down and the lid 22 is securely sealed in the thermostat 14. Can be retained.

  In the state where the thermostatic chamber 14 holding the reaction column 11 is set in the thermostatic chamber accommodating portion 52 of the thermal insulation case 51, the heater 19 is operated after the outer lid 55 of the thermal insulation case 51 is closed and the reaction column 11 is operated. Start heating. After the reaction column 11 reaches a preset temperature, the supply of the raw material is started from the raw material supply pipe 33 and the reaction product is taken out from the reaction liquid outlet pipe 28.

  At this time, even if the set temperature of the reaction column 11 is high and the partition wall 43b outside the heat insulating material 54 is heated by the heat from the thermostatic chamber 14, the ventilation path 57 provided between the partition wall 43b and the outer wall 56 Due to the effect, the outer wall 56 can be prevented from becoming hot, and accidents such as burns can be avoided. Moreover, since the upper part of the holding lid 22 of the thermostatic chamber 14 is covered with the outer lid 55, the holding lid 22 is not opened during operation, and the reaction column 11 is held in the thermostatic bath 14 in a predetermined state.

  Each component on the inlet side including the reaction column 11 and the cylindrical adapter 25 can be assembled in a state where the thermostatic chamber 14 is accommodated in the thermostatic chamber accommodating portion 52, and the opening / closing operation lever 24 is finally connected to the handle portion 58. And the handle portion 24c can be easily and reliably rotated to the column holding position.

  Further, since the reaction column 11 is pushed and pressed by the coil spring 31, even if the thermal expansion coefficients of the reaction column 11, the main body 15 of the thermostatic chamber 14, and the cylindrical adapter 25 are different, both ends of the reaction column 11 are used. On the other hand, when the pressure in the reaction column 11 rises abnormally, the internal pressure can be released by slightly raising the inlet-side column end 26 while compressing the coil spring 31. It is also possible to ensure safety in the event of an emergency.

  Furthermore, since the inlet side of the reaction column 11 is inserted with sufficient depth into the inner diameter inner peripheral portion 25c of the cylindrical adapter 25 together with the inlet side column end 26, the heat from the thermostatic chamber 14 is transferred from the reaction column 11 to the reaction column 11. Can be reliably transmitted to the inlet side, and heat radiation from the inlet side of the reaction column 11 can also be suppressed. Thereby, the reaction from the inlet side in the reaction column 11 can be reliably advanced.

  In addition, although the exit side of the reaction column 11 protrudes from the lower end of the cylindrical adapter 25, since the reaction is completed at the exit side portion of the reaction column 11 in a normal reaction, a slight temperature decrease becomes a problem. There is nothing. Further, even when a large-diameter reaction column that does not use the cylindrical adapter 25 is used, it is housed in the large-diameter insertion portion 16a at the upper part of the column insertion hole 16, so that the reaction column inlet side is the same as described above. It is possible to sufficiently heat by suppressing the heat radiation from.

  In addition, the toggle link structure in the column pushing means 18 is formed by the rotating shafts 22a and 23a fixed to the main body part of the four-node toggle link structure. The rigidity can be increased, and the holding lid 22 can be reliably held in the holding position.

  After the predetermined processing is completed and the temperature is lowered, the outer lid 55 is opened and the open / close operation lever 24 is rotated upward to the column attaching / detaching position, whereby the holding lid 22 can be rotated to the open position. it can. When the reaction column 11 is taken out, the reaction column 11 is easily taken out by integrating the reaction column 11, the inlet side column end 26, the coil spring 31, and the inlet side cap 32 as described above. In addition, each part after taking out does not fall apart, and the handleability can be improved.

  Further, when the reaction column 11, the cylindrical adapter 25, and the column insertion hole 16 are fixed due to crystals generated by leakage of a highly crystalline raw material liquid during operation, the outlet side holding member 17 is removed from the main body 15. By removing the reaction column 11 protruding from the lower end of the cylindrical adapter 25 and applying an impact from below, the reaction column 11 and the cylindrical adapter 25 can be easily removed from the column insertion hole 16.

  When another reaction column 11 is used to perform the treatment under different reaction conditions, after removing the used reaction column 11, a new reaction column 11 is installed in the cylindrical adapter 25 as described above. By inserting and turning the restraining lid 22 to the restraining position, preparation for the next processing is completed. Therefore, it is possible to easily attach and detach the reaction column 11 when performing a process by exchanging a plurality of reaction columns 11, greatly reducing the time required for the process, and easily searching for the optimum reaction conditions. Can be done.

  The reaction column 11 can be easily prepared in a state where a hydrogenation catalyst 12 is filled in a straight tube made of metal or glass and a filter 13 is press-fitted at both ends. Furthermore, since the connection and sealing to both column ends are performed by crimping to the O-ring, the work before and after the treatment can be simplified and the replacement of the reaction column is extremely easy compared to the case where both column ends are screwed together. . Therefore, the cost required for the reaction column and the running cost can be reduced, and the hydrogenation catalyst in the reaction column can be easily replaced.

  Further, when using reaction columns having different sizes, a cylindrical adapter corresponding to the reaction column is used. For example, as shown in FIG. 9, when using reaction columns 61 having the same length and different diameters, the outer diameter is the same as that of the cylindrical adapter 25, and the inner diameter corresponds to the outer diameter of the reaction column 61. The cylindrical adapter 62 is used, and the inlet side column end 63 and the outlet side column end 64 formed with circular recesses 63a and 64a corresponding to the end face shape of the reaction column 61 are used. An inlet peripheral surface O-ring 65 and an inlet end surface O-ring 66 corresponding to the diameter of the reaction column 61 are mounted in advance in the circular recess 63a of the inlet-side column end 63. The outlet end face O-ring 67 is mounted in advance. When the diameter of the coil spring 68 is large, the coil spring 68 can be directly pushed by the restraining lid 22 without using the inlet side cap.

  Therefore, by simply replacing the parts around the reaction column with parts corresponding to the diameter of each reaction column, reaction columns of various sizes can be easily and reliably set in the thermostat 14 by the above-described operation. Experiments with varying amounts of hydrogenation catalyst, space velocity, and linear velocity can be easily performed. Further, when a reaction column having an outer diameter corresponding to the inner diameter of the column insertion hole 16 is used without using a cylindrical adapter, the inlet side column end 26 is accommodated in the large diameter insertion portion 16 a of the column insertion hole 16. Therefore, the sealing at the inlet side of the reaction column can be performed by the inlet end face O-ring and the inlet peripheral face O-ring as described above.

  FIG. 10 is a cross-sectional side view of the main part showing another embodiment of the thermostatic chamber in the reaction apparatus of the present invention. In addition, in the following description, the same code | symbol is attached | subjected to the component same as the component of the thermostat shown to the said example, and detailed description is abbreviate | omitted.

  In this embodiment, a plurality of disc springs 71 are stacked in series instead of the coil spring 31 as urging means for pushing the inlet side column end in the reaction column direction. By using such a disc spring 71, desired pressing force and pressing force can be obtained in a small space. A cap 72 corresponding to the shape of the disc spring 71 is used, and an O-ring 73 for preventing the cap 72 is disposed on the inner periphery of the upper portion of the cap 72.

  The reaction column and the inlet side column end can be integrated by providing a circumferential groove on the inlet side of the reaction column into which the inlet peripheral surface O-ring fits, and the reaction column can be kept at a constant temperature together with the inlet side column end. While being able to extract from a tank, it can utilize also for identification of the inlet side of a reaction column. However, the circumferential groove may be omitted when it is difficult to accurately form the circumferential groove, for example, when the reaction column is made of glass instead of metal. In addition, the flange on the outlet side column end is formed using two chamfers that engage the tool when screwing the reaction solution pipe, but it is formed in a flange shape on the upper outer periphery of the outlet side column end. You can also

DESCRIPTION OF SYMBOLS 11 ... Reaction column, 11a ... Circumferential groove, 12 ... Hydrogenation catalyst, 13 ... Filter, 14 ... Constant temperature bath, 15 ... Main part, 16 ... Column insertion hole, 16a ... Large diameter insertion part, 16b ... Positioning step part, 17 DESCRIPTION OF SYMBOLS ... Outlet side holding member, 17a ... Fitting recessed part, 18 ... Column pushing means, 19 ... Heater, 20 ... Thermal fuse, 21 ... Temperature sensor, 22 ... Holding lid, 22a ... Rotating shaft, 22b ... Component insertion groove, 23 ... Link lever, 23a ... Rotating shaft, 24 ... Opening / closing operation lever, 24a, 24b ... Rotating shaft, 24c ... Handle part, 25 ... Cylindrical adapter, 25a ... Large diameter outer peripheral portion, 25b ... Circumferential groove, 25c ... Medium diameter inner circumference, 25d ... large diameter inner circumference, 26 ... inlet side column end, 26a ... raw material introduction hole, 26b ... small diameter part, 26c ... circular recess, 26d ... internal thread hole, 26e ... inlet side O-ring mounting groove , 26f ... Circumferential O-ring mounting groove 26g ... Coil spring engaging part, 27 ... Outlet side column end, 27a ... Reactant outlet hole, 27b ... Gutter part, 27c ... Female thread hole, 27d ... Circular recess, 27e ... Outlet side O-ring mounting groove, 28 ... Reaction liquid Derived piping, 29 ... exit side connector, 30 ... exit end face O-ring, 31 ... coil spring, 32 ... inlet side cap, 32a ... through hole, 32b ... coil spring engaging portion, 33 ... raw material supply piping, 34 ... inlet Side connector, 35 ... inlet end face O-ring, 36 ... inlet peripheral face O-ring, 51 ... heat insulation case, 51a ... opening, 51b ... slit, 52 ... constant temperature bath accommodating part, 53a, 53b ... partition wall, 54 ... heat insulating material, 55 DESCRIPTION OF SYMBOLS ... Outer cover, 55a ... Pipe insertion part, 56 ... Outer wall, 57 ... Ventilation path, 57a ... Ventilation port, 58 ... Hand part, 59 ... Fixing pole, 60 ... Lead wire, 61 ... Reaction column, 6 ... cylindrical adapter, 63 ... inlet side column end, 63a ... circular recess, 64 ... outlet side column end, 64a ... circular recess, 65 ... inlet peripheral surface O-ring, 66 ... inlet end surface O-ring, 67 ... outlet end surface O-ring 68 ... Coil spring, 71 ... Disc spring, 72 ... Cap, 73 ... O-ring

Claims (3)

In a reaction apparatus for introducing a stock solution and hydrogen gas into a reaction column packed with a hydrogenation catalyst and performing a hydrogenation reaction, the reaction apparatus includes a thermostat holding the reaction column and a heat insulating case containing the thermostat, and the reaction The column is preliminarily filled with a hydrogenation catalyst in a straight pipe having a preset length, and filters for holding the hydrogenation catalyst in the column are press-fitted at both ends, respectively.
The thermostatic chamber includes a metal main body, a column insertion hole formed through the main body in the vertical direction, an outlet-side holding member provided on a lower outlet side of the column insertion hole, and a reaction column at a lower part. Column pushing means for pushing toward the outlet side, and heating means inserted into the main body,
In the reaction column, an outlet side column end provided on the lower outlet side is held by the outlet side holding member, and an inlet side column end provided on the upper inlet side is pushed by the column pushing means,
The column pushing means includes a restraining lid that can be rotated between a restraining position and an open position that cover the upper part of the column insertion hole, an opening / closing operation lever that opens and closes the restraining lid, and when the restraining lid is in the restraining position. Urging means for pushing the inlet side column end toward the reaction column,
The outlet-side column end includes a circular recess into which the lower end of the reaction column is inserted, and an outlet end surface O-ring that is provided on the bottom outer periphery of the circular recess and is in close contact with the lower end of the reaction column,
The inlet column end includes a circular recess into which the upper end of the reaction column is inserted, and an inlet end surface O-ring that is provided on the outer periphery of the bottom surface of the circular recess and is in close contact with the upper end of the reaction column. Characteristic reactor.   The reaction column has an outer diameter corresponding to the inner diameter of the column insertion hole, and the inner diameter is inserted into the column insertion hole via a cylindrical adapter having a shape corresponding to the outer diameter of the reaction column. The reaction apparatus according to claim 1, wherein the reaction apparatus is formed to have a length that is flush with a lower end of the column insertion hole when inserted into the column insertion hole.   The reaction column is made of metal, and a circumferential groove is provided in a circumferential direction on the outer circumference of the inlet side of the column, and an inlet circumference that fits into the circumferential groove on an inner circumferential surface of a circular recess of the inlet side column end. The reactor according to claim 1 or 2, wherein a surface O-ring is provided.

Images