JP5322226B2 - Rotary evaporator - Google Patents

Description

  The present invention relates to a rotary evaporator, and more specifically, various types of samples in a sample are heated by rotating an evaporation container into which a sample is rotated, and the vapor evaporated from the sample is introduced into a cooler via a rotary joint and cooled. The present invention relates to a vacuum seal structure in a rotary evaporator used for separating and concentrating components.

  In the rotary evaporator, a rotation drive unit for rotating the evaporation container is provided at the end of the cooler side member, and a rotary joint connected to the evaporation container is provided between the rotation drive unit and the cooler side member. A seal portion for hermetically sealing in a rotatable state is provided (for example, see Patent Document 1). The sealing material provided in this seal part not only has a vacuum holding capacity (vacuum sealability) for partitioning the internal side maintained in a vacuum state from the external side of atmospheric pressure, but also has chemical resistance, heat resistance and durability. Sex is required.

JP 2000-24404 A

  However, since the conventional sealing material is generally manufactured from a rubber-based base material, it cannot be said that the chemical resistance is sufficient, and when it comes into contact with the chemical, it may swell, deform, or harden. The sealing performance was deteriorated. In addition, the sliding portion of the sealing material is heavily worn, and not only deterioration of the sealing performance becomes a problem, but also shavings generated at the time of wear are a serious problem. For this reason, the user not only pays attention to the change in the degree of vacuum due to the deterioration of the sealing performance, but also takes a lot of time and effort for the replacement work and cleaning work of the sealing material.

  In addition, fluororesin is baked on the surface of a sealing material made of a rubber base material to improve chemical resistance and sliding lubrication, but the sliding material of the sealing material makes the glass pipe transparent. The finished rotary joint has a large friction and generates frictional heat. Therefore, there is a problem that the surface portion of the sealing material is easily scraped and the effect of baking the fluororesin does not last long. Conventionally, as a countermeasure, the outer peripheral surface of the rotary joint is processed as smoothly and accurately as possible, which affects the cost of the rotary joint.

  On the other hand, the surface of the rotary joint also wears due to sliding with the sealing material and wear due to the components of the sealing material, and a circumferential groove is generated in the sliding portion with the sealing material. The wear of the sealing material was a factor that further deteriorated the sealing performance. For this reason, it is necessary not only to periodically replace the sealing material but also to periodically replace the rotary joint in which the circumferential groove is generated.

  Accordingly, an object of the present invention is to provide a rotary evaporator having a vacuum seal structure that can suppress deterioration of sealing performance with a simple structure and can extend the life of a sealing material and a rotary joint. .

  In order to achieve the above object, the rotary evaporator according to the present invention penetrates through the inside of the rotation drive unit attached to the end of the cooler side member, the tip extends to the cooler side, and the base end is connected to the evaporation container. In the rotary evaporator provided with a ring-shaped sealing material that hermetically seals the rotary joint for the steam guide to be rotated, the outer peripheral surface of the rotary joint where the sealing material slides is matte finished It is characterized by.

  Furthermore, the rotary evaporator according to the present invention includes a fixed seal portion in which the seal material is mounted in an airtight manner via an elastic body between the end portion of the cooler-side member and the rotation drive portion, and the fixed seal portion A sliding seal portion formed on the inner peripheral side, the sliding seal portion has an annular recess opened on the rotation drive unit side, and the inner peripheral surface of the inner peripheral side piece of the annular recess is the rotary An annular seal surface that slides with the outer peripheral surface of the joint is used, and a pressing member that presses the annular seal surface in the rotary joint direction is inserted into the annular recess.

  Further, the sealing material is characterized in that an annular thin protruding piece whose tip slides on the outer peripheral surface of the rotary joint is provided on the inner peripheral surface of the base portion of the annular recess. It is characterized by being formed of a material in which carbon graphite is blended with a fluorine resin.

  According to the rotary evaporator of the present invention, the outer peripheral surface of the rotary joint where the sealing material slides is matte finished, for example, the matte finish having a surface roughness of about 3 to 10 μm is used. The initial wear powder of the seal material that has worn due to movement is entangled with the irregularities on the mat surface, and the coating film in which the wear powder of the seal material hardens is formed on the sliding part with the seal material based on the entangled initial wear powder. As the sealing material slides on the surface of the coating film, sliding resistance and frictional force are reduced. Therefore, when the initial wear stage is passed, the amount of wear of the sealing material is reduced, and the outer peripheral surface of the rotary joint is also protected by the coating film, and generation of circumferential grooves can be suppressed.

  In addition, an annular recess is formed in the sliding seal portion on the inner circumferential side of the seal material, and a pressure member is inserted into the annular recess to press the annular seal surface in the direction of the rotary joint, thereby making the annular seal surface of the rotary joint The mat finish portion can be reliably pressed, and a sufficient sealing property can be secured. Furthermore, by providing the annular thin protruding piece, it is possible to more reliably prevent the shavings from entering the inside. Further, by forming a sealing material with a material in which carbon graphite is blended with fluorine resin, lubricity by the fluorine resin and carbon graphite can be imparted to the coating film.

It is a partial cross section front view which shows the principal part of the rotary evaporator which shows one example of this invention. It is sectional drawing which shows one shape example of a sealing material. It is sectional drawing which shows the other example of a shape of a sealing material. It is sectional drawing which shows the sliding part of a sealing material and a rotary joint.

  In FIG. 1, the rotary evaporator has a rotary drive unit 13 held by a connection member (connection adapter) 11 fixed by a fixing means (not shown) and an evaporation container connection port 12 projecting obliquely downward from the connection member 11. The evaporation container 15 connected via the rotary joint 14, the cooler (not shown) connected above the connecting member 11, and the distilling receiver (not shown) connected below the connecting member 11. And is composed of.

  The rotation drive unit 13 holds and rotates the rotary joint 14 made of a glass pipe for steam guide that is detachably connected to the mouth of the evaporation container 15, and inside the rotation drive unit 13, A rotating member 17 having a holding hole 16 for inserting the rotary joint 14 is provided via a bearing 18. The rotating member 18 is driven by a driving device (not shown) to rotate at a predetermined rotation number, and rotates the evaporation container 15 through the rotary joint 14.

  Further, a male screw member 19 is provided on the evaporation container connection port 12 side of the rotation drive unit 13, and the male screw member 19 and a nut member 20 engaged with the outer periphery of the end of the evaporation container connection port 12 are screwed together. The connecting member 11 and the rotation drive unit 13 are coupled by tightening the screw. Between the opening end surface of the evaporation container connection port 12 and the end surface of the rotation driving unit 13 facing the opening end surface of the evaporation container connection port 12, the inside of the connection member 11, the rotary joint 14, the evaporation container 15, etc. 4 is provided on the outer peripheral surface of the rotary joint 14 that slides on the annular seal surface 22 on the inner periphery of the seal material 21. Is provided.

  The sealing material 21 shown in FIG. 2 has a fixed seal portion 23 on the outer peripheral side and a sliding seal portion 24 on the inner peripheral side, and the inner peripheral portion on the evaporation container connection port 12 side in the fixed seal portion 23. Is provided with a circular fitting portion 25 that is fitted into the opening of the evaporation container connection port 12, and an annular convex portion 26 that protrudes from the opening end surface of the evaporation container connection port 12 is provided on the outer peripheral side. In addition, an O-ring mounting groove 28 for mounting an O-ring 27 that is an annular elastic body is provided on the outer peripheral side surface of the fixed seal portion 23 on the rotation drive unit 13 side so as to open the rotation drive unit 13 side. .

  3 has a fixed seal portion 23 on the outer peripheral side and a sliding seal portion 24 on the inner peripheral side as described above, and an O-ring 27 is provided on the outer periphery of the fixed seal portion 23. The O-ring mounting groove 28a for mounting the outer ring is provided with an opening in the outer peripheral direction, and the same annular protrusion as described above that is in pressure contact with the opening end surface of the evaporation container connection port 12 is provided on the outer surface of both sides of the O-ring mounting groove 28a. The part 26 and the annular convex part 26a which press-contacts to the end surface of the rotational drive part 13 are each provided. In FIG. 3, the shape of the sliding seal portion 24 and the like excluding the O-ring mounting groove 28a can be formed in the same manner as the sealing material shown in FIG.

  The sliding seal portion 24 has an annular recess 29 that is open on the rotational drive portion 13 side that is the atmospheric pressure side, and an inner peripheral surface of an inner peripheral piece 29a of the annular recess 29 is the mat finish portion. It becomes the said annular seal surface 22 which slides to 14a. Further, a pressing member 30 made of a U-shaped elastic member acting in a direction to press the annular sealing surface 22 against the outer peripheral surface of the mat finishing portion 14 a is inserted into the annular recess 29, and the opening of the pressing member 30 is Both side tips are respectively engaged with stepped portions 29b provided on the groove wall facing surface of the annular recess 29 to be prevented from coming off.

  Furthermore, an annular thin protruding piece 31 whose tip slides on the outer peripheral surface of the mat finishing portion 14a is provided on the inner peripheral surface of the annular recess 29 in the sliding seal portion 24. The annular thin projecting piece 31 hardly contributes to the vacuum sealability and is provided to prevent the shavings generated by the wear of the sliding seal portion 24 from entering the inside.

  In such a vacuum seal structure, the mat finish of the mat finish portion 14a can be selected with an appropriate surface roughness depending on conditions such as the material of the annular seal surface 22 and the sliding state of the seal material 21. Is preferably mat-finished with a surface roughness of about 3 to 10 μm. If the surface roughness of the mat finish portion 14a is too small or too large, the effect of applying the mat finish cannot be sufficiently obtained, and the durability of the sealing material 21 is adversely affected, or the vacuum sealing property is obtained. May be adversely affected.

  The sealing material 21 can be formed of any material as long as it has vacuum sealing properties, chemical resistance, heat resistance, and durability. However, the sealing material 21 is made of a material in which carbon graphite is blended with a fluorine-based resin. By forming 21, the vacuum sealability and durability can be greatly improved by a synergistic effect with the mat finish 15 a of the rotary joint 14 described above.

  When the new rotary joint 14 and the new seal material 21 are used, the vacuum seal structure formed in this way is formed with fine concave and convex recesses formed in the mat finishing portion 14a of the rotary joint 14 as shown in FIG. The inside is a space, and the tip of the uneven convex portion is in contact with the annular sealing surface 22 of the sealing material 21. When the rotary drive unit 13 is operated and the rotary joint 14 is rotated in this state, initial wear occurs in which the surface portion of the annular seal surface 22 is slightly scraped by the tip of the convex portion of the mat finish portion 14a. The fine shavings (initial wear powder) peeled off from 22 are pressed into the annular sealing surface 22 to enter the concave portion of the mat finishing portion 14a and become entangled with the concave and convex portions of the mat finishing portion 14a. This process reaches a level where there is no problem in actual use in only a few minutes in the normal use rotation range from the initial start.

  At this time, even if the concave portion of the mat finishing portion 14a is a gap, the pressing member 30 inserted into the annular concave portion 29 presses the annular sealing surface 22 toward the mat finishing portion 14a. The sealing property between 22 and the mat finish portion 14a can be obtained with certainty. Further, by providing the annular thin protruding piece 31 on the vacuum side of the annular seal surface 22, it is possible to reliably prevent the shavings from entering the connection member 11 and the like. Further, the sealing material 21 is hermetically fitted to the opening of the evaporation container connection port 12 by the circular fitting portion 25, and the fixed seal portion 23 is securely sealed by the annular convex portion 26 and the O-ring 27. It has become.

  Then, when the initial wear progresses to some extent, a new initial wear powder grows into a film shape based on the initial wear powder that enters the concave portion of the mat finish portion 14a and gets entangled with the unevenness, and the annular seal surface 22 slides. A coating film of initial wear powder is formed on the mat finishing portion 14a, and the sliding between the mat finishing portion 14a and the annular seal surface 22 is performed through the coating film. At this time, by forming the sealing material 21 with a material in which carbon graphite is mixed with a fluorine resin, extremely good lubricity due to the fluorine resin and carbon graphite can be imparted to the coating film.

  After the initial wear stage until the coating film is formed on the mat finish portion 14a, the wear amount of the annular seal surface 22 is reduced by the action of the coating film, and the outer peripheral surface of the mat finish portion 14a is also protected by the coating film. Therefore, even if the annular seal surface 22 slides on the outer peripheral surface of the rotary joint 14, the occurrence of circumferential grooves as in the conventional case can be suppressed. Furthermore, by forming the sealing material 21 with a fluorine-based resin, the coating film is also formed with a fluorine-based resin, so that the chemical resistance and heat resistance can be improved.

  Therefore, the life of the sealing material 21 can be extended by reducing the amount of wear on the annular seal surface 22 and the life of the rotary joint 14 can be extended by suppressing the generation of circumferential grooves. Since the protruding pieces 31 prevent the shavings from entering the inside, contamination due to the shavings can also be avoided.

  As a result, maintenance work such as replacement and cleaning of the sealing material 21 and replacement of the rotary joint 14 can be reduced, and shavings can be prevented from being mixed into the sample during the concentration work using the rotary evaporator. A stable concentration operation can be performed. In addition, since it is not necessary to smooth the outer peripheral surface of the rotary joint 14 with high accuracy, the manufacturing cost of the rotary joint can be reduced.

  In addition, the structure and rotation mechanism of the rotary drive in the rotary evaporator, the holding structure of the rotary joint, and the like are arbitrary, and the cooler and the distiller are in accordance with the concentration work conditions such as the sample and the target component. Appropriate coolers and distillation receivers can be used, and the present invention can be applied to both vertical and horizontal coolers.

  DESCRIPTION OF SYMBOLS 11 ... Connection member (adapter for connection), 12 ... Evaporation container connection port, 13 ... Rotation drive part, 14 ... Rotary joint, 14a ... Matt finishing part, 15 ... Evaporation container, 16 ... Holding hole, 17 ... Rotation member, 18 ... Bearing, 19 ... Male thread member, 20 ... Nut member, 21,21a ... Seal material, 22 ... Ring seal surface, 23 ... Fixed seal part, 24 ... Sliding seal part, 25 ... Circular fitting part, 26, 26a ... An annular convex part, 27 ... O-ring, 28, 28a ... O-ring mounting groove, 29 ... annular concave part, 29a ... inner peripheral side piece, 29b ... step part, 30 ... pressing member, 31 ... annular thin protruding piece

Claims (4)

  In a state where the rotary joint for the steam guide, which penetrates the inside of the rotation drive unit attached to the end of the cooler side member and extends to the cooler side and the base end is connected to the evaporation container, is rotatable. A rotary evaporator provided with a ring-shaped sealing material that hermetically seals, wherein the outer peripheral surface of the rotary joint at which the sealing material slides has a mat finish.   The seal material includes a fixed seal portion that is hermetically mounted via an elastic body between an end portion of the cooler side member and the rotation drive portion, and a slide formed on an inner peripheral side of the fixed seal portion. A seal portion, and the sliding seal portion has an annular recess that is open on the rotation drive portion side, and an annular slide that slides the inner peripheral surface of the inner peripheral piece of the annular recess with the outer peripheral surface of the rotary joint. The rotary evaporator according to claim 1, wherein a pressing member that presses the annular seal surface in the direction of the rotary joint is inserted into the annular recess as a seal surface.   3. The rotary evaporator according to claim 2, wherein the seal material is provided with an annular thin protruding piece whose tip slides on the outer peripheral surface of the rotary joint on the inner peripheral surface of the base of the annular recess.   4. The rotary evaporator according to claim 2, wherein the sealing material is made of a material in which carbon graphite is blended with a fluorine resin.

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