CN114917614A

CN114917614A - Sublimation purification device for pharmaceutical intermediate preparation and purification method thereof

Info

Publication number: CN114917614A
Application number: CN202210678339.1A
Authority: CN
Inventors: 丁正兵
Original assignee: Individual
Current assignee: Individual
Priority date: 2022-06-16
Filing date: 2022-06-16
Publication date: 2022-08-19

Abstract

The invention belongs to the technical field of pharmacy, and discloses a sublimation purification device for pharmaceutical intermediate preparation, which comprises a hot bath component, wherein the hot bath component comprises a hot bath box, a water outlet pipe, a water inlet pipe, a heating pipe and a container, the container is arranged in the hot bath box, the heating pipe is fixed at the bottom end in the hot bath box, and the water outlet pipe and the water inlet pipe are both connected with the hot bath box; the collecting assembly comprises a top cover, a collecting frame and a guide pipe, wherein the top cover is arranged on the hot bath box, the collecting frame is connected to the top cover, and the guide pipe is arranged between the top cover and the collecting frame.

Description

Sublimation purification device for drug intermediate preparation and purification method thereof

Technical Field

The invention belongs to the technical field of pharmacy, and particularly relates to a sublimation purification device for pharmaceutical intermediate preparation and a purification method thereof.

Background

The intermediate is also called organic intermediate, coal tar or petroleum product is used as raw material to produce intermediate products of dye, pesticide, medicine, resin, auxiliary agent, plasticizer, etc., while the medical intermediate is some chemical raw material or chemical product used in the process of synthesizing medicine, and the chemical product can be produced in ordinary chemical plant without production license of medicine, and can be used for synthesizing medicine as long as reaching some grades.

But there are more defects in the sublimation purification device that current is used for medicine midbody to prepare when using, for example, hold the container of medicine midbody and set up in a fixed box usually, heat the container through the heating structure in the fixed box to make heat transfer heat sublimation to medicine midbody, nevertheless use the container for a long time and damage easily, and inside is dirty, and the inconvenient quick dismantlement separation of container, thereby be difficult to in time change or clearance, influenced the result of use of device greatly.

Disclosure of Invention

The invention aims to provide a sublimation purification device for preparing a drug intermediate and a purification method thereof, and aims to solve the problem that the use effect of the device is greatly influenced because a container for containing the drug intermediate provided in the background technology is not convenient to rapidly disassemble and assemble.

In order to achieve the purpose, the invention provides the following technical scheme: a sublimation purification device for preparing a drug intermediate comprises a hot bath component, wherein the hot bath component comprises a hot bath box, a water outlet pipe, a water inlet pipe, a heating pipe and a container, the container is arranged in the hot bath box, the heating pipe is fixed at the bottom end inside the hot bath box, and the water outlet pipe and the water inlet pipe are both connected with the hot bath box; the collecting assembly comprises a top cover, a collecting frame and a guide pipe, wherein the top cover is arranged on the hot bath box, the collecting frame is connected to the top cover, and the guide pipe is arranged between the top cover and the collecting frame; the supporting component, the supporting component includes that the symmetry runs through in the clamp ring, fixed block, locating piece and the constant head tank of hot bath case top both sides that first spring, symmetric connection on the dead lever are located to dead lever, cover, wherein the dead lever extends to the outside one end of hot bath case and is connected with the fixed block, the locating piece is installed in the inboard of clamp ring, the constant head tank is seted up in the outside of container, and constant head tank and locating piece phase-match.

Preferably, a connection assembly is included; the connecting assembly comprises connecting rings symmetrically arranged on two sides of the bottom of the top cover, limiting grooves symmetrically arranged on two sides of the top of the hot bath box and limiting blocks, wherein the limiting blocks are fixed on the connecting rings and are matched with the limiting grooves.

Preferably, the device comprises a limiting component; the limiting assembly comprises clamping plates, second springs and pressing blocks, the clamping plates are symmetrically hinged to two sides of the hot bath box, the second springs are mounted on the inner sides of the top ends of the clamping plates, and the pressing blocks are fixed on the second springs.

Preferably, the stirring device further comprises a stirring component; the stirring assembly comprises rotating rods, helical blades and a motor which are symmetrically arranged at two ends inside the hot bath box, wherein the helical blades are fixed on the rotating rods, and one end of each rotating rod extending to the outside of the hot bath box is connected with the motor.

Preferably, a telescopic cylinder is installed between the clamping plate and the pressing block and is located inside the second spring.

Preferably, a rubber pad is installed on the inner side of the clamping ring, and an anti-skid convex pattern is arranged on the outer wall of the rubber pad.

Preferably, a support is installed at the bottom of the hot bath box, and a foot pad is arranged at the bottom of the support.

Preferably, one end of the first spring is fixedly connected with the clamping ring, and the other end of the first spring is fixedly connected with the hot bath box.

Preferably, the limiting groove is of an arc-shaped structure, and the outer wall of the limiting block is provided with an anti-slip groove.

Compared with the prior art, the invention has the beneficial effects that:

(1) according to the invention, through the matching of the structures such as the fixing block, the fixing rod, the clamping ring and the positioning block, the container can be fastened in the hot bath box, and meanwhile, the fixing block is pulled to release the fixing so as to take out the container, so that the container can be quickly disassembled and assembled so as to be replaced or cleaned in time, the operation is simple and quick, and the using effect of the device is greatly improved.

(2) The top cover is tightly limited on the hot bath box, so that the top cover is effectively prevented from being separated, and the connection strength is greatly improved.

(3) According to the invention, through the matching of the clamping plate, the second spring and the pressing block, the pressing block can downwards press the top cover, so that the top cover can be tightly propped against the hot bath box, the gap between the top cover and the hot bath box is greatly reduced, the leakage of sublimed gas is prevented, and the sealing effect is greatly improved.

(4) According to the invention, through the matching of the motor, the rotating rod and the helical blade, the helical blade can rotate at a high speed, so that water in the hot bath box can be continuously stirred and mixed, further, the heat transfer can be accelerated, the water temperature is more uniform, and the heating effect is greatly improved.

Drawings

FIG. 1 is a schematic view of the structure of the present invention;

FIG. 2 is a schematic view of the container of the present invention in a configuration in which it is connected to a clamp ring;

FIG. 3 is an enlarged view of portion A of FIG. 1;

FIG. 4 is an enlarged view of portion B of FIG. 1;

in the figure: 1. a hot bath tank; 2. a top cover; 31. a water outlet pipe; 32. a water inlet pipe; 33. heating a tube; 34. a container; 41. a collection frame; 42. a conduit; 51. fixing the rod; 52. a first spring; 53. a clamping ring; 54. a fixed block; 55. positioning blocks; 56. positioning a groove; 61. a connecting ring; 62. a limiting groove; 63. a limiting block; 71. clamping a plate; 72. a second spring; 73. pressing into blocks; 81. a rotating rod; 82. a helical blade; 83. a motor; 9. a telescopic cylinder.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.

Referring to fig. 1-4, the present invention provides the following technical solutions: a sublimation purification device for preparing a drug intermediate comprises a hot bath component, wherein the hot bath component comprises a hot bath box 1, a water outlet pipe 31, a water inlet pipe 32, a heating pipe 33 and a container 34, the container 34 is arranged in the hot bath box 1, the heating pipe 33 is fixed at the bottom end of the interior of the hot bath box 1, and the water outlet pipe 31 and the water inlet pipe 32 are both connected with the hot bath box 1; a collecting assembly including a top cover 2 mounted on the hot bath box 1, a collecting frame 41 and a duct 42, wherein the collecting frame 41 is connected to the top cover 2, and the duct 42 is mounted between the top cover 2 and the collecting frame 41; the supporting component comprises fixing rods 51 symmetrically penetrating through two sides of the top end of the hot bath box 1, first springs 52 sleeved on the fixing rods 51, clamping rings 53 symmetrically connected to two sides of the container 34, fixing blocks 54, positioning blocks 55 and positioning grooves 56, wherein one ends of the fixing rods 51 extending to the outside of the hot bath box 1 are connected with the fixing blocks 54, the positioning blocks 55 are installed on the inner sides of the clamping rings 53, the positioning grooves 56 are arranged on the outer sides of the container 34, and the positioning grooves 56 are matched with the positioning blocks 55.

Specifically, when the device is used, the drug intermediate can be placed into the container 34, the top cover 2 is buckled on the hot bath box 1, the hot bath box 1 can be filled with water through the water inlet pipe 32, the water is heated through the heating pipe 33 to reach a preset temperature, the container 34 is heated through the hot water, so that the drug intermediate can be heated and sublimated, then the gas enters the collecting frame 41 through the guide pipe 42, the temperature is reduced in the collecting frame 41, the solid drug intermediate is formed again, and finally sublimation and purification of the drug intermediate are completed;

in addition, the fixing blocks 54 at the two sides of the hot bath box 1 are pulled, so that the fixing blocks 54 drive the fixing rod 51 to move, the rear fixing rod 51 pulls the clamping ring 53 to move, the clamping ring 53 extrudes the first spring 52, and the positioning block 55 exits from the positioning groove 56, so that the fixing can be released, and the container 34 can be taken out;

on the contrary, under the elastic action of the first spring 52, the two clamping rings 53 can clamp the container 34, and the positioning block 55 is inserted into the positioning slot 56, so that the container 34 can be fastened in the hot bath box 1, and the container 34 can be quickly disassembled and assembled so as to be replaced or cleaned in time, the operation is simple and quick, and the using effect of the device is greatly improved.

Comprises a connecting component; the connecting assembly comprises connecting rings 61 symmetrically arranged on two sides of the bottom of the top cover 2, limiting grooves 62 symmetrically arranged on two sides of the top of the hot bath box 1 and limiting blocks 63, wherein the limiting blocks 63 are fixed on the connecting rings 61, and the limiting blocks 63 are matched with the limiting grooves 62.

Specifically, when top cap 2 is connected with hot bath case 1, can insert the spacing groove 62 with the stopper 63 earlier, then rotate top cap 2, make top cap 2 drive go-between 61 and remove, go-between 61 can drive stopper 63 in spacing groove 62 afterwards, make stopper 63 and the locking of spacing groove 62 block to can be with the restriction that top cap 2 is tight on hot bath case 1, the effectual top cap 2 that has prevented breaks away from, improved joint strength greatly.

Comprises a limiting component; the limiting component comprises a clamping plate 71, a second spring 72 and a pressing block 73, wherein the clamping plate 71, the second spring 72 and the pressing block 73 are symmetrically hinged to two sides of the hot bath box 1, the second spring 72 is installed on the inner side of the top end of the clamping plate 71, and the pressing block 73 is fixed on the second spring 72.

Specifically, the back is connected with hot bath case 1 to top cap 2, rotatable cardboard 71 makes the tip card of cardboard 71 in top cap 2's top, simultaneously under the spring action of second spring 72, can make briquetting 73 compress tightly top cap 2 downwards to can tightly support top cap 2 tightly on hot bath case 1, and then reduced the clearance between top cap 2 and the hot bath case 1 greatly, prevent sublimed gas leakage, improve sealed effect greatly.

The stirring device also comprises a stirring component; the stirring assembly comprises a rotating rod 81, a helical blade 82 and a motor 83 which are symmetrically arranged at two ends inside the hot bath box 1, wherein the helical blade 82 is fixed on the rotating rod 81, and one end of the rotating rod 81 extending to the outside of the hot bath box 1 is connected with the motor 83.

Specifically, drive bull stick 81 through the work of motor 83 and rotate, make bull stick 81 drive helical blade 82 and rotate, under helical blade 82's high-speed rotation, can constantly stir the mixture to the water in the hot bath case 1 to can accelerate heat transfer, and make more even of temperature, improve the heating effect greatly.

Install telescopic tube 9 between cardboard 71 and the briquetting 73, and telescopic tube 9 is located the inside of second spring 72, and the rubber pad is installed to the inboard of clamp ring 53, and the outer wall of rubber pad is provided with anti-skidding burr, and the pillar is installed to the bottom of hot-water bath case 1, and the bottom of pillar is provided with the callus on the sole, the one end and the clamp ring 53 fixed connection of first spring 52, and the other end and the hot-water bath case 1 fixed connection of first spring 52, spacing groove 62 is the arc structure, the antiskid groove has been seted up to the outer wall of stopper 63.

Specifically, through addding telescopic cylinder 9, can strengthen the stability when second spring 72 elasticity is flexible greatly, and the rubber pad has skid-proof effect, and the fastening nature when can further improve the clamp ring 53 centre gripping can be supported fixedly to the device through the pillar simultaneously, and the callus on the sole can increase frictional force.

A purification method of a sublimation purification apparatus for pharmaceutical intermediate preparation, comprising the steps of:

s1, putting the medicine intermediate into a container 34, and then covering a top cover 2;

s2, injecting water into the hot bath box 1 through a water inlet pipe 32, and heating the water through a heating pipe 33 to enable the water to reach a preset temperature;

s3, uniformly transferring heat to the container 34 through hot water, so that the medicine in the container 34 is sublimated;

s4, gas generated by sublimation enters the collecting frame 41 through the guide pipe 42, and is cooled in the collecting frame 41 to form a solid drug intermediate again, and finally sublimation and purification of the drug intermediate are completed.

It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims

1. A sublimation purification apparatus for pharmaceutical intermediate preparation, comprising:

the heating bath assembly comprises a heating bath box (1), a water outlet pipe (31), a water inlet pipe (32), a heating pipe (33) and a container (34), wherein the container (34) is installed in the heating bath box (1), the heating pipe (33) is fixed at the bottom end of the interior of the heating bath box (1), and the water outlet pipe (31) and the water inlet pipe (32) are both connected with the heating bath box (1);

the collecting assembly comprises a top cover (2) arranged on the hot bath box (1), a collecting frame (41) and a guide pipe (42), wherein the collecting frame (41) is connected to the top cover (2), and the guide pipe (42) is arranged between the top cover (2) and the collecting frame (41);

the supporting component comprises a fixing rod (51) symmetrically penetrating through two sides of the top end of the hot bath box (1), a first spring (52) sleeved on the fixing rod (51), and a clamp ring (53), a fixing block (54), a positioning block (55) and a positioning groove (56) symmetrically connected to two sides of the container (34), wherein the fixing rod (51) extends to one end of the outside of the hot bath box (1) to be connected with the fixing block (54), the positioning block (55) is installed on the inner side of the clamp ring (53), the positioning groove (56) is arranged on the outer side of the container (34), and the positioning groove (56) is matched with the positioning block (55).

2. A sublimation purification apparatus for pharmaceutical intermediate preparation according to claim 1, wherein: comprises a connecting component;

the connecting assembly comprises connecting rings (61) symmetrically arranged on two sides of the bottom of the top cover (2), limiting grooves (62) symmetrically arranged on two sides of the top of the hot bath box (1) and limiting blocks (63), wherein the limiting blocks (63) are fixed on the connecting rings (61), and the limiting blocks (63) are matched with the limiting grooves (62).

3. The sublimation purification apparatus for preparation of pharmaceutical intermediates of claim 2, wherein: comprises a limiting component;

the limiting assembly comprises clamping plates (71), second springs (72) and pressing blocks (73), wherein the clamping plates (71), the second springs (72) and the pressing blocks (73) are symmetrically hinged to two sides of the hot bath box (1), the second springs (72) are installed on the inner sides of the top ends of the clamping plates (71), and the pressing blocks (73) are fixed on the second springs (72).

4. A sublimation purification apparatus for pharmaceutical intermediate preparation according to claim 3, wherein: the stirring device also comprises a stirring component;

stirring assembly is including symmetry install in bull stick (81), helical blade (82) and motor (83) of hot bath (1) inside both ends, wherein helical blade (82) are fixed in on bull stick (81), and bull stick (81) extend to the outside one end of hot bath (1) and are connected with motor (83).

5. A sublimation purification apparatus for pharmaceutical intermediate preparation according to claim 4, wherein: a telescopic cylinder (9) is installed between the clamping plate (71) and the pressing block (73), and the telescopic cylinder (9) is located inside the second spring (72).

6. A sublimation purification apparatus for pharmaceutical intermediate preparation according to claim 5, wherein: the inner side of the clamping ring (53) is provided with a rubber pad, and the outer wall of the rubber pad is provided with anti-skid convex lines.

7. A sublimation purification apparatus for pharmaceutical intermediate preparation according to claim 6, wherein: the bottom of hot-bath box (1) is installed the pillar, and the bottom of pillar is provided with the callus on the sole.

8. A sublimation purification apparatus for pharmaceutical intermediate preparation according to claim 7, wherein: one end of the first spring (52) is fixedly connected with the clamping ring (53), and the other end of the first spring (52) is fixedly connected with the hot bath box (1).

9. A sublimation purification apparatus for pharmaceutical intermediate preparation according to claim 8, wherein: the limiting groove (62) is of an arc-shaped structure, and the outer wall of the limiting block (63) is provided with an anti-skidding groove.

10. A purification method of a sublimation purification device for preparing a pharmaceutical intermediate is characterized by comprising the following steps:

s1, putting the drug intermediate into a container (34), and then covering a top cover (2);

s2, injecting water into the hot bath box (1) through a water inlet pipe (32), and heating the water through a heating pipe (33) to enable the water to reach a preset temperature;

s3, uniformly transferring heat to the container (34) through hot water so as to sublimate the medicine in the container (34);

s4, gas generated by sublimation enters the collecting frame (41) through the guide pipe (42), and is cooled in the collecting frame (41) to form a solid drug intermediate again, and finally sublimation and purification of the drug intermediate are completed.