CN-120268081-B - Preparation device and method of high-purity landiolol hydrochloride

CN120268081BCN 120268081 BCN120268081 BCN 120268081BCN-120268081-B

Abstract

The invention relates to the technical field of medicine preparation, in particular to a preparation device and a preparation method of high-purity landiolol hydrochloride, comprising a water bath heating tank and a filtering structure communicated with the lower part of the water bath heating tank through a valve component, wherein the lower part of the filtering structure is communicated with a cooling liquid storage tank, a semiconductor refrigerating device is arranged on the outer side of the cooling liquid storage tank, a first heat exchange unit is arranged on the outer side of the water bath heating tank, a second heat exchange unit communicated with the first heat exchange unit is arranged on the outer side of the semiconductor refrigerating device, a continuous production flow is formed by adding crude solution, heating, filtering, cooling crystallization and resetting equipment, when one batch of purification is finished, the heating tank is communicated with the cooling liquid storage tank, the filtering component is reset, the next batch of production can be immediately put into without long-time waiting for equipment adjustment, the production period is greatly shortened, the continuous requirement of large-scale industrial production is met, and compared with the traditional intermittent production mode, and the yield is remarkably improved.

Inventors

ZHAO JINLONG
JIANG TINGTING
LIU LEI
CHEN JUNTAO
CHEN SHIXIN
XU LIZHONG

Assignees

连云港众维生物医药有限公司

Dates

Publication Date: 20260508
Application Date: 20250609

Claims (6)

1. The preparation device of the high-purity landiolol hydrochloride is characterized by comprising a water bath heating tank (1) and a filtering structure communicated with the lower part of the water bath heating tank (1) through a valve (14) component, wherein the lower part of the filtering structure is communicated with a cooling liquid storage tank (2), a semiconductor refrigerating device is arranged on the outer side of the cooling liquid storage tank (2), a first heat exchange unit is arranged on the outer side of the water bath heating tank (1), and a second heat exchange unit communicated with the first heat exchange unit is arranged on the outer side of the semiconductor refrigerating device; The filter structure comprises a frame body (3) communicated between a valve (14) assembly and a cooling liquid storage tank (2), wherein both sides of the frame body (3) are communicated with a protective shell (5) through sliding grooves (4), the protective shell (5) is respectively and slidably connected with a filter frame (6) with an upward opening, the bottom of the filter frame (6) is provided with a filter hole (7), the front side and the rear side of the filter frame (6) are slidably connected with the inner wall of the frame body (3) in a sealing way, a spring (8) is connected between one far away side of the two groups of filter frames (6) and the protective shell (5), and the side surface of the filter frame (6) is inserted into a filter plate (9); One side of the filter frame (6) is provided with a mounting groove (10) which is in sliding connection with the filter plate (9), the filter plate (9) is positioned at the bottom of the inner side of the filter frame (6), and the side surface of the protective shell (5) is provided with an opening (11) corresponding to the mounting groove (10); The semiconductor refrigerating device continuously refrigerates the cooling liquid storage tank (2), the temperature in the cooling liquid storage tank (2) is continuously reduced, air in the tank is contracted when being cooled, so that negative pressure is generated, under the action of the negative pressure, components in the filtering structure move, after the filtering structure moves to a certain position, the subsequent filtering operation on the heated saturated solution in the water bath heating tank (1) is facilitated, a valve assembly is opened, the heated saturated solution in the water bath heating tank (1) flows into the filtering structure through the valve assembly under the dual actions of gravity and the negative pressure of the cooling liquid storage tank (2), the filtered saturated solution is filtered by the filtering structure, after the liquid in the heating tank is discharged, the air in the heating tank enters the cooling liquid storage tank (2), the air pressure of the cooling liquid storage tank (2) is rapidly increased, and the filtering structure is automatically reset to an initial state; An embedded groove (12) arranged at the bottom of the inner side of the filter frame (6) is arranged above the filter plate (9), and an expansion pad (13) which is used for extruding the upper edge of the filter plate (9) after expansion is arranged in the embedded groove (12).
2. The device for preparing high-purity landiolol hydrochloride according to claim 1, wherein the valve (14) assembly comprises a valve (14) with the upper end connected with the flange of the water bath heating tank (1), and the lower end of the valve (14) is fixedly connected with the upper surface of the frame body (3) through a flange connector.
3. The device for preparing the high-purity landiolol hydrochloride according to claim 2 is characterized in that the bottom of a cooling liquid storage tank (2) is fixedly connected with a first driving motor (15), a plurality of groups of first-stage stirring paddles (16) distributed circumferentially are arranged on an output shaft of the first driving motor (15), the lower part of the cooling liquid storage tank (2) is communicated with a discharge pipe (17), the semiconductor refrigerating device comprises a plurality of groups of semiconductor refrigerating sheets (18) connected to the outer side of the cooling liquid storage tank (2), and a negative pressure pump (34) is communicated with the cooling liquid storage tank (2).
4. The device for preparing high-purity landiolol hydrochloride according to claim 3, wherein the first heat exchange unit comprises a plurality of groups of arc heat exchange plates (19) arranged outside the water bath heating tank (1), first circulation channels (20) are arranged in the arc heat exchange plates (19), first liquid inlet connectors (21) are communicated with the upper ends of the first circulation channels (20), and first liquid outlet connectors (22) are communicated with the lower ends of the first circulation channels (20); The second heat exchange unit comprises a plurality of groups of plane heat exchange plates (23) arranged on one side of the semiconductor refrigerating sheet (18), the plane heat exchange plates (23) correspond to the arc-shaped heat exchange plates (19), second circulation channels (24) are arranged in the plane heat exchange plates (23), the upper ends of the second circulation channels (24) are communicated with second liquid outlet joints (25), the second liquid outlet joints (25) are communicated with the first liquid inlet joints (21) through pipelines, the lower ends of the second circulation channels (24) are communicated with second liquid inlet joints (26), and the first liquid outlet joints (22) are communicated with the second liquid inlet joints (26) through pipelines.
5. The device for preparing high-purity landiolol hydrochloride according to claim 4, wherein the upper surface of the water bath heating tank (1) is communicated with a first joint (27) and a second joint (28), a second driving motor (29) is arranged on the upper portion of the water bath heating tank (1), a plurality of groups of circumferentially distributed secondary stirring paddles (30) are arranged on an output shaft of the second driving motor (29), and the upper surface of the water bath heating tank (1) is communicated with a pressure relief valve (31).
6. The device for preparing high-purity landiolol hydrochloride according to claim 5, wherein a reinforced supporting structural member (32) is fixedly connected between the upper surfaces of the water bath heating tank (1) and the cooling liquid storage tank (2), and a plurality of groups of supporting legs (33) which are vertically arranged are fixedly connected with the lower end of the cooling liquid storage tank (2).

Description

Preparation device and method of high-purity landiolol hydrochloride Technical Field The invention relates to the technical field of medicine preparation, in particular to a device and a method for preparing high-purity landiolol hydrochloride. Background Landil hydrochloride is an ultra-short-acting beta 1-receptor blocker, is mainly used for treating tachyarrhythmia, can effectively reduce heart rate and relieve heart load, and plays a key role in emergency treatment of cardiovascular diseases such as acute myocardial infarction, unstable angina and the like; at present, in the preparation process of the landiolol hydrochloride, the purification stage is a key link for determining the quality and the production efficiency of the product, the traditional purification process usually adopts a recrystallization method, the method usually comprises the steps of preparing a hot saturated solution, filtering while the solution is hot and cooling and crystallizing, the traditional purification method is low in efficiency, and occupies a large amount of operation time of production equipment in the purification process, so that the production efficiency is difficult to improve, and urgent requirements of large-scale industrial production on efficient and continuous preparation of the high-purity landiolol hydrochloride cannot be met, so that the preparation device and the method for the high-purity landiolol hydrochloride are provided to improve the purification efficiency of the landiolol hydrochloride and realize continuous production. Disclosure of Invention Aiming at the problems in the prior art, the invention provides a preparation device and a preparation method of high-purity landiolol hydrochloride, which improve the purification efficiency of the landiolol hydrochloride and realize continuous production. The invention solves the technical problems by adopting the technical scheme that the device and the method for preparing the high-purity landiolol hydrochloride comprise a water bath heating tank and a filtering structure communicated with the lower part of the water bath heating tank through a valve component, wherein the lower part of the filtering structure is communicated with a cooling liquid storage tank, a semiconductor refrigerating device is arranged on the outer side of the cooling liquid storage tank, a first heat exchange unit is arranged on the outer side of the water bath heating tank, and a second heat exchange unit communicated with the first heat exchange unit is arranged on the outer side of the semiconductor refrigerating device. Specifically, the filter assembly comprises a frame body communicated between the valve assembly and the cooling liquid storage tank, two sides of the frame body are communicated with the protective shell through sliding grooves, filter frames with upward openings are respectively and hermetically connected in the protective shell, filter holes are formed in the bottoms of the filter frames, the front side and the rear side of the filter frames are hermetically and slidably connected with the inner wall of the frame body, springs are connected between the side, away from the two groups of filter frames, of the filter frames and the protective shell, and the side surfaces of the filter frames are inserted into the filter plates. Specifically, the filter frame one side is equipped with the mounting groove with filter plate sliding connection, and the filter plate is located the inboard bottom of filter frame, and the protecting crust side is equipped with the opening that corresponds the mounting groove. Specifically, an embedded groove arranged at the bottom of the inner side of the filter frame is arranged above the filter plate, and an expansion pad which is expanded and then extruded on the upper edge of the filter plate is arranged in the embedded groove. Specifically, the valve assembly comprises a valve with the upper end connected with the flange of the water bath heating tank, and the lower end of the valve is fixedly connected with the upper surface of the frame body through a flange connecting piece. Specifically, the bottom of the cooling liquid storage tank is fixedly connected with a first driving motor, a plurality of groups of first-stage stirring paddles distributed circumferentially are arranged on an output shaft of the first driving motor, the lower part of the cooling liquid storage tank is communicated with a discharge pipe, the semiconductor refrigerating device comprises a plurality of groups of semiconductor refrigerating sheets connected to the outer side of the cooling liquid storage tank, and the cooling liquid storage tank is communicated with a negative pressure pump. Specifically, the first heat exchange unit comprises a plurality of groups of arc heat exchange plates arranged on the outer side of the water bath heating tank, first circulating channels are arranged in the arc heat exchange plates, the upper ends of the first circ