JP5639914B2 - Switching valve - Google Patents

Description

  The present invention is suitable for, for example, a high performance liquid chromatograph (hereinafter referred to as HPLC) having a recycle separation function, and can easily obtain different pressure resistances on the rotor seal surface with a simple configuration, thereby reducing the wear of the rotor. Therefore, the replacement can be performed rationally, the supply and discharge of high-pressure fluid can be performed accurately and smoothly, and the manufacturing can be simplified and reduced, and the size and weight can be reduced. The present invention relates to a switching valve that can easily switch between a phase supply channel and a recycling channel.

  A liquid chromatograph equipped with a recycle separation function (hereinafter referred to as LC) is equipped with a recycle valve and a switching valve. The sample is introduced into the eluent, and when the target component of the sample is eluted, the recycle valve is switched. At the same time, there is one in which the switching valve is switched so that the eluent and the sample are circulated through the recycling flow path for recycling separation (see, for example, Patent Document 1).

  However, the LC requires a recycle valve and a switching valve, which increases the number of parts, makes the configuration complicated and expensive, and requires switching them, resulting in complicated operations.

  As a solution to the above problem, there is one in which the recycling valve and the switching valve are constituted by a single 8-port switching valve, the number of valves is reduced, and the complicated switching operation of the valve is eliminated ( For example, see Patent Document 2).

  However, since the LC has a buffer flow path connected to the 8-port switching valve and a sample injection device is inserted in the recycle flow path, the dead volume of the recycle flow path increases and the sample diffuses. The recycling separation accuracy was not sufficient.

  By the way, in this kind of switching valve, a rotor having an orifice communicating with a port opened to the outside and a rotor having a plurality of rotor grooves communicable with the orifice. The actuator is attached to the back of the rotor in place of the conventional disc spring, and the pressure sensor for detecting the pressure of the flow path and the signal of the amplifier are input to the actuator, There is one in which the axial dimension of the actuator is changed by the pressure of the flow path to generate a seal pressure required for the sliding surface between the rotor and the stator (for example, Patent Document 3). reference).

  However, the dimensional change of the actuator or the urging force of the disc spring acts uniformly on the entire sliding surface of the rotor and the stator via the holding plate, and the orifice and the rotor. -Since the seal pressure is applied uniformly to the groove, there is a problem that the pressure resistance of the rotor seal surface is set uniformly.

  In order to solve such a problem, a rotor seal surface is provided with a plurality of rotor grooves at inner and outer positions on concentric circles, and the sample injection device is switched according to the sample injection amount. is there. (For example, refer to Patent Document 4).

  However, since the switching valve makes the entire area of the rotor seal surface and the sliding surface of the stator contact with a uniform pressure, the inner side of the switching valve is determined based on the pressure resistance of the outer rotor groove. Because the rotor groove pressure is set, the inner rotor groove tends to be set lower than the optimum value, and the rotor seal surface is made of the same member. However, there is a problem in that the outer rotor seal surface having a large peripheral speed is worn faster than the inner side, and the entire rotor must be replaced even though the inner side can be used sufficiently.

Japanese Patent No. 2557384 JP 2006-138699 A JP-A-1-307575 JP 2009-276110 A

  The present invention solves such problems and is suitable for, for example, a high performance liquid chromatograph (hereinafter referred to as HPLC) having a recycle separation function, and easily obtains different pressure resistance on the rotor seal surface with a simple configuration. It is possible to rationally replace the rotor according to the wear of the rotor, to supply and discharge high-pressure fluid accurately and smoothly, and to simplify and reduce the manufacturing cost, as well as to reduce the size and weight. It is an object of the present invention to provide a switching valve that can easily switch between a supply flow path and a recycle flow path of a mobile phase by a single valve operation.

According to the first aspect of the present invention, there is provided a stator having a plurality of orifices communicating with the outside, and a plurality of rotors arranged so as to be slidably contacted and rotatable with the stator and capable of communicating with the orifices. And a rotor formed with a rotor groove, wherein the rotor seal surface of the rotor is urged in a fluid-tight manner to the stator, and the rotor is connected to the outer rotor. Consists of a rotor and an inner rotor arranged inside the rotor, and the outer rotor and the inner rotor can be moved to the stator side. The urging means for urging each rotor toward the stator side is separately provided behind the outer rotor and the inner rotor, and the rotor is configured with a simple structure. -Different pressure resistance can be easily obtained on the tur-seal surface, high pressure fluid can be supplied and discharged smoothly and efficiently, and can be manufactured easily and inexpensively. Unishi to have.
Therefore, by using the switching valve in an HPLC having a recycling separation function, it is possible to easily switch between the supply flow path and the recycling flow path of the mobile phase by a single valve operation, and to make it suitable for use in HPLC. Yes.

According to a second aspect of the present invention, the outer rotor and the inner rotor can be rotated synchronously so that the desired operation of the rotor can be obtained.
According to a third aspect of the present invention, when the outer rotor and the inner rotor are formed of the same or different members, and the same member is used, for example, the configuration is simplified and the manufacture is facilitated. In case of using different materials, rational design is promoted by using different materials with different wear resistance or chemical durability, for example, based on the difference in peripheral speed or wear and pressure resistance. I am doing so.
According to a fourth aspect of the present invention, the outer rotor and the inner rotor are separately detachably provided, and the replacement when the seal action is deteriorated due to wear due to aging is uniquely and uniquely provided. It can be performed separately, and the replacement can be easily performed on a small scale, and the unreasonableness of exchanging the entire rotor can be eliminated like a conventional integrated rotor. .
According to a fifth aspect of the present invention, a valve shaft is rotatably and axially movable in a valve housing that accommodates an outer rotor and an inner rotor, and the end of the valve shaft is provided with the valve shaft. An inner rotor is mounted, and a rotating cylinder is slidably and axially disposed on the end surface of the valve shaft, and the outer rotor is disposed at the end of the rotating cylinder. A rotor is mounted, and the outer rotor and the inner rotor can be rotated synchronously with a simple configuration.

According to a sixth aspect of the present invention, a flange is provided on the rotating cylinder, and an urging means is disposed behind the flange so as to be engageable. A flange is provided on a peripheral surface of the valve shaft, and the flange is attached to the rear of the flange. By arranging the biasing means so as to be engageable and using separate biasing means, each of the outer rotor and the inner rotor is biased independently and as expected. This makes it possible to set the breakdown voltage of the period.
According to the seventh aspect of the present invention, eight or more orifices are formed on the seal surface of the stator, and the number of the orifices formed on the seal surface and the number of orifices formed on the seal surface are determined. Both of them are reduced from the conventional ones, simplifying the structure and facilitating manufacture, reducing the size and weight of the switching valve, and making it compatible with HPLC flow path switching.
According to an eighth aspect of the present invention, four or more rotor grooves capable of communicating with the orifice are formed on a rotor seal surface of the rotor, and the rotor is formed on the seal surface. -The number of grooves is reduced compared to the conventional one, the structure is simplified and the manufacture is facilitated, the switching valve is reduced in size and weight, and it is adapted for switching the flow path of HPLC.

According to the ninth aspect of the present invention, the orifices are formed to have different diameters and are arranged at concentric inner and outer positions, the orifice is rationally arranged on the seal surface of the stator, and the seal is arranged. The surface and the stator are reduced in size and weight.
According to a tenth aspect of the present invention, the rotor grooves are formed to have different widths, and are arranged at concentric inner and outer positions so that the rotor grooves are rationally provided on the rotor seal surface. Therefore, the rotor seal surface or rotor is reduced in size and weight.
According to the eleventh aspect of the present invention, one end of a plurality of conduits is connected to the outside of the stator, and the other end of the conduit is connected to a mobile phase supply channel, a liquid feed pump, a separation column, and a detector. Inserting and connecting the introduced sample to a recycling channel that enables circulation, the supply channel and the recycling channel can be switched, and a single valve configuration allows the mobile phase supply channel and the recycling channel to be switched. Can be easily switched and is suitable for use in HPLC.
According to a twelfth aspect of the present invention, the biasing means is a spring, and can be easily and inexpensively manufactured by a general-purpose configuration such as a disc spring, a coil spring, and a leaf spring.

According to a first aspect of the present invention, a rotor is composed of an outer rotor and an inner rotor disposed inside the rotor, and the outer rotor and the inner rotor are arranged. Rotors are provided so as to be movable toward the stator side, and the rotors are urged toward the stator side behind the outer rotor and the inner rotor. Since the biasing means are separately arranged, different pressure resistances can be easily obtained on the rotor seal surface with a simple configuration, and high-pressure fluid can be supplied smoothly and efficiently, and this can be manufactured easily and inexpensively. be able to.
Therefore, by using the switching valve for HPLC having a recycling separation function, the mobile phase supply channel and the recycling channel can be easily switched by a single valve operation, which is suitable for the use of HPLC. There is.

According to the second aspect of the present invention, since the outer rotor and the inner rotor can be rotated synchronously, the desired operation of the rotor can be obtained.
According to the invention of claim 3, since the outer rotor and the inner rotor are made of the same or different members, when they are made of the same member, for example, the structure is simplified and the manufacture is facilitated. In the case of using different materials, rational design can be achieved by using different materials with different wear resistance or chemical durability, for example, based on differences in peripheral speed or wear and pressure resistance. Can be urged.
According to the invention of claim 4, since the outer rotor and the inner rotor are separately detachably provided, the replacement when the seal action is deteriorated due to wear due to use over time is unique. In addition, they can be performed separately and can be easily exchanged on a small scale, and can eliminate the unreasonableness of exchanging the entire rotor as in a conventional integrated rotor.
According to a fifth aspect of the present invention, a valve shaft is rotatably and axially movable in a valve housing that accommodates an outer rotor and an inner rotor, and the end of the valve shaft is provided with the valve shaft. An inner rotor is mounted, and a rotating cylinder is slidably and axially disposed on the end surface of the valve shaft, and the outer rotor is disposed at the end of the rotating cylinder. Since the rotor is mounted, synchronous rotation of the outer rotor and the inner rotor can be realized with a simple configuration.

According to a sixth aspect of the present invention, a flange is provided on the rotating cylinder, and an urging means is disposed behind the flange so as to be engageable. A flange is provided on a peripheral surface of the valve shaft, and the flange is attached to the rear of the flange. Since the biasing means are arranged to be engageable, by using separate biasing means, the respective biasing of the outer rotor and the inner rotor can be obtained independently and as expected, The desired breakdown voltage can be set.
In the invention of claim 7, since eight or more orifices are formed on the seal surface of the stator, the number of orifices formed on the seal surface and the number of orifices formed on the seal surface is reduced. Both of them are less than the conventional ones, simplifying the structure and facilitating the manufacture, reducing the size and weight of the switching valve, and are effective for switching the flow path of HPLC.
According to the eighth aspect of the present invention, since four or more rotor grooves that can communicate with the orifice are formed on the rotor seal surface of the rotor, the rotor formed on the seal surface. The number of turbine grooves is reduced as compared with the prior art, the structure is simplified and the manufacture is facilitated, the switching valve is reduced in size and weight, and the effect is that it can be used for switching the flow path of HPLC.
According to the ninth aspect of the present invention, since the orifices are formed to have different diameters and are arranged at concentric inner and outer positions, the orifice is rationally arranged on the seal surface of the stator, and -The surface and the stator can be reduced in size and weight.

In the tenth aspect of the present invention, the rotor grooves are formed to have different widths, and are arranged at concentric inner and outer positions, so that the rotor groove is formed on the rotor seal surface. The rotor seal surface or rotor can be reduced in size and weight by rational arrangement.
According to the eleventh aspect of the present invention, one end of a plurality of conduits is connected to the outside of the stator, and the other end of the conduit is connected to a mobile phase supply channel, a liquid feed pump, a separation column, and a detector. Inserted and connected to the recycle flow path that allows the introduced sample to be circulated, and the supply flow path and the recycle flow path can be switched. The flow path can be easily switched, and there is an effect suitable for the use of HPLC.
According to a twelfth aspect of the present invention, the biasing means is a spring, and can be easily and inexpensively manufactured by a general-purpose configuration such as a disc spring, a coil spring, and a leaf spring.

It is a front view which shows the outer surface of the valve head of the switching valve applied to this invention. It is an expanded sectional view which follows the AA line of FIG. It is a front view which shows the rotor of the switching valve applied to this invention, and the inner rotor is mounted | worn with the outer rotor. FIG. 2 is an exploded front view showing a rotor of a switching valve applied to the present invention, wherein (a) shows an outer rotor and (b) shows an inner rotor. It is explanatory drawing which shows the time of normal use at the time of applying the switching valve of this invention for the flow path switching of HPLC.

It is explanatory drawing which shows the time of recycling at the time of applying the switching valve of this invention for the flow path switching of HPLC. It is an expanded sectional view showing an important section of a 2nd embodiment of the present invention. It is a front view of the rotor which shows the principal part of the 3rd Embodiment of this invention, and the inner rotor is mounted | worn with the outer rotor. FIG. 7 is an exploded front view showing a rotor of a switching valve applied to the third embodiment, wherein (a) shows an outer rotor and (b) shows an inner rotor. Yes.

  DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention applied to an HPLC switching valve having a recycle separation function will be described below. In FIG. 1 to FIG. A switching valve having a switching function. The switching valve 1 is a multi-port valve of 8 ports or more, and in the embodiment, a 10-port switching valve is used.

In order to reduce the internal dead volume, the switching valve 1 has a stator 2 having a function of a valve head, and has a flat seal surface 2a inside the stator 2. The stator 2 is connected to a cylindrical valve housing 4 via a bolt 3.
The outside of the stator 2 is formed in a substantially truncated cone shape, and a plurality of ports 5 and 6 are arranged concentrically at the inner and outer positions of the outer surface thereof, and fittings 7 and 8 are provided on the ports 5 and 6. Are connected, and the conduits 9a to 9d and the conduits 9b, 9c and 10a are connected to the fittings 7 and 8, respectively.

  In this case, the inner diameter of the conduit 9c on the suction side of the liquid feeding pump, which will be described later, is formed to the maximum diameter among the respective conduits so that the suction operation by the liquid feeding pump can be performed smoothly and efficiently. The inner diameter of the conduit 9b on the introduction side to the switching valve 1 is formed to be an intermediate diameter so as to prevent a high-pressure load on the cell of the detector to prevent the destruction of the cell. It is desirable to form the inner diameter of the discharge-side conduit 9c to the minimum diameter.

Slanted passages 11 and 12 communicating with the ports 5 and 6 are formed inside the stator-2. The inclination angles of the passages 11 and 12 are different from each other. It is formed at an acute angle with respect to the oblique passage 12 arranged on the inner side, and the inner end thereof opens to the inner and outer positions of the seal surface 2a of the stator-2.
Large and small diameter orifices 13 to 16 and 17 to 22 are formed at inner end portions of the oblique passages 11 and 12, and the orifices 13 to 16 and 17 to 22 can communicate with a rotor groove described later. Is arranged.
In the embodiment, ten orifices are formed, but it is sufficient to form eight or more orifices for switching the supply flow path of the HPLC mobile phase and the recycle flow path.

A stepped valve chamber 4 a having a large and small diameter is formed inside the valve housing 4, and a valve shaft 23 is disposed in the valve chamber 4 a so as to be rotatable and slidable in the axial direction. Projecting outward, the projecting portion is linked to a rotor driving motor (not shown).
The other end portion of the valve shaft 23 is enlarged in diameter, a rotating cylinder 24 is disposed around the enlarged diameter portion 23a, and a plurality of guide grooves 25 are formed on the inner surface of the cylinder 24 in the axial direction. A plurality of dogs 26 project from the other end of the shaft 23, and the dogs 26 are slidably fitted into the guide grooves 25.

A flange 27 is formed at the end of the rotating cylinder 24. A spring 28 is provided between the flange 27 and the large-diameter step 4b of the valve chamber 4a as a biasing means for an outer rotor described later. In the embodiment, a plurality of disc springs and a bearing 29 are arranged.
A convex portion such as a flange 30 protrudes from an intermediate portion of the valve shaft 23, and a spring 31 is provided between the flange 30 and the small-diameter step portion 4c as an urging means for an inner rotor described later. Then, the some disc spring and the bearing 32 are arrange | positioned.
In this case, it is also possible to use a coil spring or a leaf spring instead of the disc spring.

  The disc spring 28 is formed to have a larger diameter than the disc spring 31, and the spring strength of the disc springs 28, 31 is the pressure resistance or seal pressure of the corresponding outer rotor or inner rotor. And the spring strength of the disc spring 31 is set to be stronger than that of the disc spring 28.

  An elastic force of the disc spring 28 urges an outer rotor, which will be described later, to move toward the stator 2 side, and the elastic force of the disc spring 31 causes the valve shaft 23 to move toward the stator. The inner rotor, which will be described later, is urged so as to be movable toward the second side, and is urged so as to be movable toward the stator-2 side separately from the outer rotor. In the figure, reference numeral 33 denotes a bearing disposed on one end side of the valve shaft 23.

  The end face of the flange 27 is arranged on the same plane as the end face of the valve shaft 23, and an annular holding plate 34 is arranged on the end face of the flange 27. A disc-shaped holding plate 35 is arranged inside the holding plate 34 so as to be movable with the valve shaft 23, and a rotor 36 is arranged on the other side of the holding plates 34, 35.

The rotor 36 includes a ring-shaped outer rotor 37 made of a synthetic resin such as PEEK (registered trademark) material, and a disk-shaped made of a synthetic resin of the same quality as the outer rotor 37. The inner rotor 38 is fitted in the through hole 37b of the outer rotor 37 so as to be slidable in the axial direction.
In this case, the outer rotor 37 is made of PEEK material, and the inner rotor 38 is made of graphite Bespel (registered trademark), Delrin (registered trademark) material, etc., which are different from the outer rotor 37. It is also possible to configure.
Further, although the outer rotor 37 is formed in an annular truncated cone shape, it can be formed in an annular disk shape.

The outer rotor 37 is fixed to the holding plate 34 and the end face of the flange 27 via a pin 39, and the inner rotor 38 is fixed to the holding plate 35 and a valve via a pin 40. It is fixed to the end face of the shaft 23.
In this case, in the rotor 36 of the embodiment, the valve shaft 23 is linked to a rotor driving motor (not shown) as rotating means, but manually instead of the motor. It is also possible to rotate.

The turning force of the valve shaft 23 is transmitted to the rotating cylinder 24 via the dog 26, and the turning force of the cylinder 24 can be transmitted to the outer rotor 37 via the pin 39 and the holding plate 34. Has been.
On the other hand, the rotational force of the valve shaft 23 can be transmitted to the inner rotor 38 via the pin 40 and the holding plate 35, and can be rotated synchronously with the outer rotor 37. Yes.

On the rotor seal surface 37a of the outer rotor 37, two large and small arc-shaped rotor grooves 41, 42 are formed at inner and outer positions on concentric circles. , 42 are arranged at substantially point-symmetrical positions as shown in the figure. Among these, the rotor groove 41 is formed to be approximately half the length of the rotor groove 42, and the groove width is the same. Has been.
In the normal time when the mobile phase is supplied and the target component is separated, the orifices 13 and 14 are arranged in the rotor groove 41 so as to communicate with each other, and the orifices 15 and 14 are arranged in the rotor groove 42. 16 is arrange | positioned so that communication is possible.

One end of a conduit 9a communicates with the orifice 13 and the other end is connected to a sorting device 43. One end of a conduit 9b communicates with the orifice 14 and the other end is connected to the orifice 18. The conduit 9b A detector 45 having a cell 44 and a separation column 46 are interposed.
One end of a conduit 9c communicates with the orifice 15, the other end communicates with the orifice 19, and a liquid feed pump 47 is inserted into the conduit 9c.
One end of a conduit 9 d communicates with the orifice 16 and the other end is connected to a container 49 containing an eluent 48.

Three similar arc-shaped rotor grooves 50 to 52 are arranged concentrically on the rotor seal surface 38a of the inner rotor 38 at equiangular positions.
The length of the rotor grooves 50 to 52 is formed to be approximately ¼ of the rotor groove 42, and the groove width is formed to be approximately ½ of the rotor groove 42. .
Among these, the rotor groove 51 is positioned on the radiation at the substantially center of the length of the rotor groove 42, and the other rotor grooves 50, based on the rotor groove 51. 52 is arranged.

In a normal state, the orifices 17 and 18 are arranged to communicate with the rotor groove 50, and the orifices 19 and 20 are arranged to communicate with the rotor groove 51. The orifices 21 and 22 are arranged in the turbine groove 52 so as to communicate with each other.
One end of a conduit 10a communicates with the orifice 20, the other end communicates with the orifice 22, and a preheat tube 53 and an autosampler 54 are inserted into the conduit 10a. One end of a conduit or passage 10 b communicates with the orifice 17 and the other end communicates with the orifice 21.

The preheat tube 53 is supplied with the eluent 48 until the recycle target component is eluted, and the eluent 48 can be heated by a heater (not shown) attached to the tube 53. Yes.
In the embodiment, the autosampler 54 is disposed in the conduit 10a. However, it is also possible to dispose the autosampler 54 on the upstream side of the separation column 46. It is also possible to arrange in an oven (not shown).

  In general, the switching valve configured as described above is a stateer 2 having a function of a valve head, a valve housing 4 to which the stater-2 is attached, and the valve housing 4 can be rotated and moved in the axial direction. A valve shaft 23 provided on the rotating shaft 24, a rotating cylinder 24 that can rotate synchronously with the valve shaft 23, a holding plate 34 that can move with the rotating cylinder 24, and a holding plate 35 that can move with the valve shaft 23 The outer rotor 37 that can move with the holding plate 34, the inner rotor 37 that can move with the holding plate 35, the outer rotor 37, and the inner rotor The disc springs 28 and 31 are biasing means of −37.

The stator-2 is formed in a deformed disk shape, four ports 5 and six ports 6 are formed on the outer surface thereof, and a smooth seal surface 2a is formed on the inner side. The orifices 13 to 16 and 17 to 22 having different diameters communicating with the ports 5 and 6 are formed in the inner and outer positions on the concentric circles.
The valve housing 4 is formed in a substantially cylindrical shape, a stepped valve chamber 4a is formed therein, a large-diameter step portion 4b and a small-diameter step portion 4c having large and small different diameters are formed at front and rear positions thereof, The valve shaft 23 is accommodated so as to be rotatable and movable in the axial direction.

The valve shaft 23 is formed in a stepped shaft shape, a flange 30 is projected in the middle of the valve shaft 23, a plurality of dogs 26 are projected on the outer periphery of the shaft end, and the other end is reduced in diameter. Extend.
The rotating cylinder 24 is formed in a hollow cylindrical shape, a flange 27 is provided at the end thereof, and a guide groove 25 that can be engaged with the dog 26 is formed in the axial direction on the inner surface of the hollow portion.
The holding plate 34 is formed in an annular disk shape, and the inner holding plate 35 is formed in a disk shape that can be inserted into the holding plate 34.

The rotor 36 is composed of two members of the same or different quality, an outer rotor 37 and an inner rotor 38. In the embodiment, these are made of PEEK (registered trademark) material, graphite vespel (registered trademark) material, delrin (registered trademark), or the like.
Further, the outer rotor 37 is formed in an annular truncated cone shape or a disk shape, and is formed in a disk shape that can be fitted into the through hole 37b of the inner rotor 38.
Two large and small arc-shaped rotor grooves 41 and 42 are arranged concentrically on the rotor seal surface 37a of the outer rotor 37 so that the rotor of the inner rotor 38 is rotated. Three similar arc-shaped rotor grooves 50 to 52 are arranged at equiangular positions on a concentric circle on the rotor seal surface 38a.

  The spring strength of the disc springs 28 and 31 is set in accordance with the pressure resistance or seal pressure of the corresponding outer rotor 37 or inner rotor 38. In the embodiment, the outer rotor is used. The spring strength of the disc spring 31 with respect to the inner rotor 38 is set stronger than the disc spring 28 with respect to -37.

When assembling the switching valve using such main components, for example, one end of the valve shaft 23 is inserted into the rotating cylinder 24, the dog 26 is engaged with the guide groove 25, and the valve shaft 23 The shaft end and the end face of the flange 27 are positioned on the same plane.
Thereafter, the holding plate 34 is superposed on the end face of the flange 27, the holding plate 35 is inserted inside thereof, and the holding plate 35 is superposed on the shaft end portion of the valve shaft 23. Then, the pin 39 is press-fitted into the holding plate 34 and the end surface of the flange 27, the pin 40 is press-fitted into the holding plate 35 and the shaft end surface of the valve shaft 23, and the holding plates 34 and 35 are pressed into the shaft end surface of the flange 27 and the valve shaft 23. Secure to

Next, the outer rotor 37 is superposed on the other end surface of the holding plate 34, the outer rotor 37 is press-fitted into the protruding portion of the pin 39, and the outer rotor 37 is also pressed. An inner rotor 38 is inserted inside the inner rotor 38, and the inner rotor 38 is press-fitted into the projecting portion of the pin 40 to hold the outer rotor 37 and the inner rotor 38. Secure to plates 34 and 35.
Thus, the valve shaft assembly in which the outer rotor 37 and the inner rotor 38 are assembled to the shaft end portion of the valve shaft 23 via the pins 39 and 40 and the holding plates 34 and 35 is provided. To manufacture.

Before and after manufacturing the assembly, the bearing 29 and the large-diameter disc spring 28 are accommodated in the large-diameter step portion 4b of the valve housing 4a, and the bearing 32 and the small-diameter disc spring 31 are accommodated in the small-diameter step portion 4c of the valve housing 4. And the bearings 32 and 32 are arranged to be engageable with the stepped portions 4b and 4c.
Thereafter, the valve shaft assembly is inserted into the valve chamber 4a, the flange 30 is positioned so as to be engageable with the disc spring 31, the flange 27 of the rotating cylinder 24 is positioned so as to be engageable with the disc spring 28, and The other end protrudes outside the valve housing 4 and the protrusion is linked to a rotor driving motor (not shown).

  The stator 2 is joined to one end of the valve housing 4, and the seal surface 2a is connected to the other end surfaces of the outer rotor 37 and the inner rotor 38, that is, each rotor. -Join the seals 37a and 38a, screw the bolt 3 into the valve housing 4 from the outside of the stator-2, and tighten the bolt 3 to connect the stator-2 to the valve housing 4.

This situation is as shown in FIGS. 2 and 3. The rotor grooves 41 and 42 of the outer rotor 37 are connected to the orifices 13 to 16 of the stator 2 so that the inner rotor 38 The rotor grooves 50 to 52 are connected to the orifices 17 to 22 of the stator 2.
Thereafter, the fittings 7 and 8 are screwed into the respective ports 5 and 6, and one ends of the conduits 9a to 9d, 9b, 9c and 10a are piped to the fittings 7 and 8, respectively.

The other end of the conduit 9a is connected to the sorting device 43, the other end of the conduit 9b communicates with the orifice 18, and the detector 45 and the separation column 46 are inserted into the conduit 9b.
Further, the other end of the conduit 9 c communicates with the orifice 19, a liquid feed pump 47 is inserted into the conduit 9 c, and the other end of the conduit 9 d is connected to the container 49. Further, the other end of the conduit 10a is communicated with the orifice 22, and a preheat tube 53 and an autosampler 54 are inserted into the conduit 10a. This situation is as shown in FIG.

In the assembled switching valve 1, the valve shaft 23 is biased toward the stator 2 side by the elasticity of the disc spring 31, and the rotor seal surface 38 a of the inner rotor 38 is interposed via the holding plate 35. However, it is in close contact with the seal surface 2a of the stator 2 and slidably contacted.
The rotating cylinder 24 is slidably engaged with the dog 26 and is connected to the valve shaft 23 so as to be able to rotate synchronously. The rotating cylinder 24 is attached to the stator-2 side by the elasticity of the disc spring 28. The rotor seal surface 37a of the outer rotor 37 is slidably brought into close contact with the seal surface 2a of the stator 2 via the holding plate 34 so as to be rotatable.

At this time, the seal pressure or pressure resistance of the rotor seal surface 37a of the outer rotor 37 with respect to the seal surface 2a of the stator 2 is set by the elasticity of the disc spring 28, and The seal pressure or pressure resistance of the rotor seal surface 38 a of the inner rotor 38 with respect to the seal surface 2 a is set by the elasticity of the disc spring 31.
Thus, since the pressure acting on the rotor seal surfaces 37a and 38a is uniquely and separately set by the two urging means, compared with the conventional one set by the single urging means. Thus, the strength of the urging means such as individual disc springs can be reduced, and the pressure resistance against the rotor seal surfaces 37a and 38a can be set precisely.

Therefore, by selecting the spring strength of the disc springs 28 and 31, the optimum shearing surface 37a and 38a for the outer rotor 37 and the inner rotor 38 can be obtained. -The pressure or pressure can be set individually and individually, and with a degree of freedom.
In the embodiment, the spring strength of the disc spring 31 is set stronger than that of the disc spring 28, the pressure resistance of the rotor seal surface 38a of the inner rotor 38 is 33 MPa, and the outer rotor. The pressure resistance of the 37 rotor seal surfaces 37a is set to 4 MPa.

Therefore, it is possible to accurately set the seal pressure or pressure resistance according to the pressure of the fluid guided to the rotor grooves 41, 42, 50 to 52, and to cause liquid leakage when supplying or discharging the high or low pressure fluid. It can be done safely and smoothly.
Therefore, the rotor is integrally formed as in the prior art, or a plurality of constituent members are integrally connected, and the entire area of the rotor is uniformly and uniformly distributed from the rear by a single biasing means. The rotor seal pressure or pressure resistance is set uniformly with reference to the outer rotor groove as in the case of energizing the motor, eliminating the problem that the correct pressure resistance cannot be obtained. Can do.

Under such circumstances, for example, when the valve shaft 23 is rotated by a drive motor (not shown), the rotational force is transferred to the inner rotor 38 via the holding plate 35 fixed to the shaft end. Then, the inner rotor 38 rotates in synchronism with the valve shaft 23.
On the other hand, the rotational force of the valve shaft 23 is transmitted to the rotary cylinder 24 via the dog 26, and the rotary cylinder 24 rotates synchronously with the valve shaft 23 and via the holding plate 34 fixed to the flange 27. The outer rotor 37 is transmitted to the outer rotor 37, and the outer rotor 37 rotates in synchronization with the valve shaft 23.

In the normal state, as shown in FIG. 5, the eluent 48 discharged from the liquid feed pump 47 is sent to the conduit 9c and moved to the orifice 19, and is sent from the rotor groove 51 to the conduit 10a. -Moves to the orifice 22 through the tube 53 and the autosampler 54, and is sent out from the rotor groove 52 to the passage 10b and from the rotor groove 50 to the conduit 9b.
After that, it moves to the orifice 14 through the separation column 46 and the detector 45, and is sent from the rotor groove 41 to the conduit 9 a to move to the sorting device 43.

At this time, the eluent 48 containing the sample is guided to the rotor grooves 50 to 52, and the fluid pressure is applied to the rotor seal surface 38a of the inner rotor 38, and the rotor is rotated. The elution solution 48 or the like guided to the grooves 41 and 42 applies the fluid pressure to the rotor seal surface 37a of the outer rotor 37.
The rotors 38 and 37 are supported by the holding plates 34 and 35, the flange 27, and the valve shaft 23, respectively, and the disc springs 31 and 28 support them separately.

Therefore, the rotor rotor 37 and the inner rotor 38 can be compared with the conventional rotor rotor 37 and the inner rotor 38, as compared with the conventional case where the entire rotor is supported by a single biasing means. The lube surfaces 37a and 38a are accurately and reliably sealed by the elasticity of the disc springs 31 and 28 to prevent liquid leakage.
Therefore, for example, the moving fluid is pulsated by the liquid feed pump 47, and the rotor seal surface 37a of the outer rotor 37 on the seal surface 2a and the rotor of the inner rotor 38 are rotated. Even if the pressure fluctuation of the turbine seal surface 38a is frequently performed, the rotor seal surfaces 37a and 38a can be sealed accurately and reliably.

  On the other hand, at the time of recycling, as shown in FIG. 6, the eluent 48 and the like discharged from the liquid feed pump 47 is sent to the conduit 9c and moved to the orifice 19, and sent from the rotor groove 50 to the conduit 9b. It moves to the orifice 14 through the separation column 46 and the detector 45, and is sent out from the rotor groove 42 through the orifice 15 to the conduit 9 c and returned to the liquid feed pump 47.

At this time, the eluent 48 and the like are guided to the rotor groove 50, and the fluid pressure acts on the rotor seal surface 38a of the inner rotor 38, and the rotor groove 42. The eluent 48 and the like led to the above acts on the rotor seal surface 37a of the outer rotor 37 with its fluid pressure.
The rotors 38 and 37 are supported by the holding plates 34 and 35, the flange 27, and the valve shaft 23, respectively, and the disc springs 31 and 28 support them separately.

Therefore, the rotor seal surfaces 37a and 398a are more reliably and reliably provided by the elasticity of the disc springs 31 and 28, compared to the conventional case where the entire rotor is supported by a single biasing means. Sealed precisely to prevent leakage.
For this reason, for example, the moving fluid is pulsated by the liquid feed pump 47, and the pressure fluctuations of the rotor seal surface 37a and the rotor seal surface 38a on the seal surface 2a are frequently performed. In addition, the seals of the rotor seal surfaces 37a and 38a can be precisely and reliably performed.

Thus, when the switching valve 1 is used over time, the rotor seal surfaces 37a and 38a of the outer rotor 37 and the inner rotor 38 are connected to the shaft of the stator 2. The seal surface 2a is slidably contacted and worn, and the seal action is lowered and needs to be replaced.
In this case, since the outer rotor 37 has a higher peripheral speed than the inner rotor 38, the outer rotor 37 tends to wear quickly and the sealing action tends to decrease, while the inner rotor 38 tends to decrease. Since the peripheral speed is lower than that of the outer rotor 37, the wear is slow and the seal function is often exhibited sufficiently. In such a case, if only the outer rotor 37 is replaced, It will be good.

Therefore, when replacing the outer rotor 37, the bolt 3 is removed, the stator 2 is removed, the valve shaft assembly is removed from the valve housing 4, and only the outer rotor 37 is removed as appropriate. A new outer rotor 37 may be replaced.
Therefore, there is no unreasonable or troublesome replacement of the entire rotor as in the case of a conventional integrated rotor, and the replacement of the inner rotor 38 is avoided, so that a small-scale replacement operation is sufficient. This work can be done easily and quickly.

Next, separation by HPLC equipped with the switching valve 1 will be described.
That is, at the normal time of sample introduction and fractionation, the switching valve 1 is set to the normal operation mode, the ports 5 and 6 and the orifices 13 to 22 are communicated, and the liquid feed pump 47 is connected. To drive.
In this way, the eluent 48 in the container 49 is guided to the conduit 9 d and moves to the orifice 16, is sent from the rotor groove 42 to the conduit 9 c through the orifice 15, and is sucked into the liquid feed pump 47. .
In this case, if the inner diameter of the conduit 9c on the suction side from the switching valve 1 of the liquid feed pump 47 is formed to the maximum diameter in each conduit, the suction operation by the liquid feed pump 47 can be performed smoothly and efficiently.

Thereafter, the eluent 48 is discharged from the liquid feed pump 47, sent to the conduit 9c, moved to the orifice 19, sent from the rotor groove 51 to the conduit 10a, and led to the preheat tube 53. A sample is introduced when the autosampler 54 is moved, and is sent out from the rotor groove 52 to the passage 10b through the orifice 22.

  The eluent 48 containing the sample is sent out from the rotor groove 50 to the conduit 9b, moves to the separation column 46, where the target component is separated, and is guided to the detector 45 to detect the target component, to the orifice 14. Moving. After that, it is sent out from the rotor groove 41 to the conduit 9a, moves to the sorting device 43, and is sorted by the sorting device 43 for each target component.

At that time, the separation column 46 is heated by an oven (not shown), and the eluent 48 heated by the preheat tube 53 is moved, so that the temperature difference between the inside and outside is eliminated, and the separation accuracy is improved. .
In this case, if the inner diameter of the conduit 9b is formed to be an intermediate diameter in each conduit, the pressure increase of the conduits 9a and 9b can be suppressed, the high pressure load on the cell 44 caused by them can be avoided, and the failure of the cell 44 can be prevented. .

Thus, when the target component of the sample is eluted and confirmed by the detector 45, the motor for driving the rotor (not shown) is driven, and the motor is rotated by a predetermined angle (about 45 °). To do.
In this way, the valve shaft 23 linked to the motor moves, and the inner rotor 38 rotates synchronously via the holding plate 35 fixed to the shaft end.
Further, the rotating cylinder 24 is synchronously rotated through the dog 26 protruding from the shaft end portion, and the holding plate 34 fixed to the flange 27 is moved together, and the outer roller fixed to the holding plate 34 is moved. The counter 37 rotates synchronously.

In this way, the inner rotor 38 and the outer rotor 37 rotate synchronously, and the rotor grooves 41, 42, and 50 to 52 are moved in synchronism, so that the switching valves 1 to Switch rotor 36 to recycle mode.
This situation is as shown in FIG. 6. The orifices 18 and 19 communicate with the rotor groove 50, the orifices 20 and 21 communicate with the rotor groove 51, and the orifices 22 and 17 communicate with the rotor groove 49. Communicate with.
Further, the orifice 13 communicates with the rotor groove 41, and the orifices 14 to 16 communicate with the rotor groove 42.

That is, both ends of the conduit 9b communicate with the orifices 14 and 18, both ends of the conduit 9c communicate with the orifices 15 and 19, and the rotor grooves 42 and 51 communicate with the conduits 9b and 9c. Form a recycling path for
At that time, the conduit 9 a communicating with the orifice 13, the conduit 9 d communicating with the orifice 16, and the conduit 10 a communicating with the orifices 20 and 22 are disconnected from the recycling flow path, and the supply of the eluent 48 to the switching valve 1 is performed. Sample introduction is stopped.

  Then, the eluent 48 containing the sample is circulated through the recycling channel via the liquid feed pump 47, and the target component in the sample is separated by the separation column 46, and this is detected by the detector 45.

In such recycle separation, the eluent 48 containing the sample is sucked smoothly and efficiently from the rotor groove 42 by the liquid feed pump 47 through the conduit 9c having the maximum inner diameter.
In this case, if the conduit 9c on the discharge side of the liquid feed pump 47 has a minimum inner diameter and the length thereof is made as short as possible, the dead volume of the flow path is reduced, and the diffusion of the sample is suppressed and separated. Separation accuracy by the column 46 is improved.
Moreover, if the conduit 9b on the outlet side of the detector 45 is made to have an intermediate diameter, the pressure rise in the relevant part is suppressed to avoid a high-pressure load on the cell 44 and to prevent a failure of the cell 44.

As described above, the switching valve 1 of the embodiment is inserted in the recycling flow path, and the recycling valve and the switching of the flow path can be configured by a single valve. The number of parts is reduced and the configuration is simplified, so that the HPLC can be reduced in size and weight and can be manufactured at low cost.
In addition, since it is sufficient to switch the single switching valve 1 at the normal time of sample introduction or sorting and at the time of recycling, the trouble of switching between the two valves as in the prior art can be eliminated.

7 to 9 show other embodiments of the present invention, and the same reference numerals are used for portions corresponding to the above-described configuration.
Of these, FIG. 7 shows a second embodiment of the present invention. In this embodiment, the above-described outer rotor 37 and holding plate 34 are integrally formed by the same member, and the inner rotor is also formed. -38 and the holding plate 35 are integrally formed of the same member to reduce the number of parts, simplify the structure, and reduce the thickness to reduce the size and weight so that they can be manufactured easily and inexpensively. ing.
In this case, the outer rotor 37 and the inner rotor 38 can be made of the same or different members as described above.

FIGS. 8 and 9 show a third embodiment of the present invention. This embodiment has three outer and outer arc-shaped rotor grooves 55 to 57 at equiangular positions. Of these, the lengths of the rotor grooves 55 and 56 are the same, and the length of the rotor groove 57 is slightly longer than the rotor grooves 55 and 56.
Further, the inner rotor 38 is configured in substantially the same manner as in the above-described embodiment, and the rotor grooves 50 to 52 are positioned 60 degrees out of phase with the rotor grooves 55 to 57. It is arranged.

  The switching valve of the present invention can easily obtain different pressure resistances on the rotor seal surface with a simple structure, and can be rationally replaced according to the wear of the rotor, and can supply and discharge high-pressure fluid. It can be performed accurately and smoothly, and can be easily and inexpensively manufactured, and can be reduced in size and weight. In addition, since the mobile phase supply channel and the recycling channel can be easily switched by a single valve operation, it is suitable for, for example, HPLC having a recycling separation function.

1 Switching valve 2 Starter
2a Seal surface 4 Valve housing 9a to 9d Conduit
10a conduit

13-22 Orifice 23 Valve shaft 24 Rotating cylinder 27 Flange 28 Biasing means (spring)
30 Flange

31 Biasing means (spring)
36 rotor
37 Outer rotor
37a Rotor sealing surface 38 Inner rotor
38a Rotor seal surface 41, 42 Rotor groove

45 Detector 46 Separation column 47 Liquid feed pump 50 to 52 Rotor groove

Claims (12)

  A stator having a plurality of orifices communicating with the outside, and a rotor having a plurality of rotor grooves that are slidably contacted and rotatable with the stator and that communicate with the orifices. A switching valve in which the rotor seal surface of the rotor is urged in a fluid-tight manner to the stator, and the rotor is connected to the outer rotor and the rotor. An inner rotor disposed on the inner side of the rotor, the outer rotor and the inner rotor being provided movably toward the stator side, and the outer rotor A switching valve characterized in that urging means for urging each rotor toward the stator side is separately arranged behind the rotor and the inner rotor.   2. The switching valve according to claim 1, wherein the outer rotor and the inner rotor can be rotated synchronously. 2. The outer rotor and the inner rotor are made of the same or different members.
The switching valve described.   2. The switching valve according to claim 1, wherein the outer rotor and the inner rotor are detachably provided separately.   A valve shaft is provided in the valve housing for accommodating the outer rotor and the inner rotor so as to be rotatable and movable in the axial direction, and the inner rotor is provided at the end of the valve shaft. A rotary cylinder is disposed on the peripheral surface of the end portion of the valve shaft so as to be slidable and engageable in the axial direction, and the outer rotor is mounted on an end portion of the rotary cylinder. The switching valve according to any one of claims 1 to 4.   The rotating cylinder is provided with a flange, and an urging means is disposed behind the flange so as to be engageable. A flange is provided on the peripheral surface of the valve shaft, and the urging means can be engaged with the rear of the flange. 6. The switching valve according to claim 5, which is arranged.   2. The switching valve according to claim 1, wherein eight or more orifices are formed on the seal surface of the stator.   2. The switching valve according to claim 1, wherein four or more rotor grooves capable of communicating with the orifice are formed on a rotor seal surface of the rotor.   The switching valve according to claim 7, wherein the orifices are formed to have different diameters and are arranged at concentric inner and outer positions.   9. The switching valve according to claim 8, wherein the rotor grooves are formed to have different widths and are arranged at concentric inner and outer positions.   One end of a plurality of conduits is connected to the outside of the stator, the other end of the conduit is inserted through a mobile phase supply flow path, a liquid feed pump, a separation column, and a detector, and an introduced sample is inserted. The switching valve according to claim 1, wherein the switching valve is connected to a recycling flow path that can be circulated so that the supply flow path and the recycling flow path can be switched.   The switching valve according to claim 1, wherein the biasing means is a spring.

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