Preparation method and equipment of DL-homocysteine thiolactone hydrochloride

Abstract

The invention relates to the field of DL-homocysteine thiolactone hydrochloride preparation, and discloses a DL-homocysteine thiolactone hydrochloride preparation method and equipment, which comprises a cylindrical first tank body, an inverted truncated cone-shaped second tank body arranged in the first tank body, and a liquid outlet formed in the bottom of the second tank body, a circular-truncated-cone-shaped filtering piece is movably arranged on the liquid outlet, a lifting mechanism used for driving the filtering piece to ascend is arranged at the bottom of the first tank body, and a rotating mechanism used for driving the second tank body to rotate is arranged at the top of the first tank body; semicircular bottom plates used for controlling opening and closing of the liquid outlet are symmetrically and movably arranged at the bottom of the second tank body in the horizontal direction, and adjusting mechanisms used for driving the bottom plates to move in the horizontal direction are symmetrically arranged on the first tank body. The method has the effect of improving the yield of finished products.

Description

Technical Field

[0001] The present invention relates to the technical field of preparation of DL-homocysteine ​​thiolactone hydrochloride, in particular to a preparation method and equipment of DL-homocysteine ​​thiolactone hydrochloride. Background Art

[0002] DL-homocysteine ​​thiolactone hydrochloride is an important biochemical reagent and pharmaceutical intermediate. It can be used to produce intermediates for various drugs such as cetirizine and erdosteine ​​for the treatment of respiratory and cardiovascular diseases.

[0003] Currently, electrochemical reduction of DL-homocysteine ​​is generally used to obtain DL-homocysteine ​​thiolactone hydrochloride at home and abroad. During the preparation process, the raw material DL-methionine needs to be hydrolyzed, filtered, the precipitate is dissolved and decolorized, filtered again, and the filtrate is electrolyzed. Therefore, it is necessary to first carry out a hydrolysis reaction in a reaction tank, then transfer the hydrolysis reaction liquid to a filtration device for filtration, and then transfer the filtered precipitate to a reaction tank for dissolution and decolorization, and then transfer it to a filtration device for filtration. In this process, the reaction product needs to be transferred multiple times, resulting in loss of the reaction product and affecting the yield of the final product. Summary of the Invention

[0004] The purpose of the present invention is to provide a method and equipment for preparing DL-homocysteine ​​thiolactone hydrochloride, which has the effect of improving the yield of finished products.

[0005] The above technical objectives of the present invention are achieved through the following technical solutions: it includes a cylindrical first tank body, an inverted truncated cone-shaped second tank body arranged inside the first tank body, and a liquid outlet opened at the bottom of the second tank body, a circular first connecting block is horizontally arranged on the top of the second tank body, the outer side of the first connecting block is engaged with the inner wall of the first tank body, a reaction chamber is formed between the upper side wall of the second tank body and the top of the first tank body, a heating chamber is formed between the lower side wall of the second tank body and the bottom of the first tank body, a first liquid inlet pipe connected to the reaction chamber is provided on the top of the first tank body, and a second liquid inlet pipe connected to the heating chamber is provided on the side wall of the first tank body. Tube, the bottom of the first tank body is provided with a liquid outlet pipe connected to the heating cavity, and a truncated cone-shaped filter element is movably provided on the liquid outlet, the bottom of the first tank body is provided with a lifting mechanism for driving the filter element to rise, and the top of the first tank body is provided with a rotating mechanism for driving the second tank body to rotate, and the bottom of the second tank body is symmetrically provided with a semicircular bottom plate for controlling the opening and closing of the liquid outlet in the horizontal direction, the sum of the cross-sectional areas of the two bottom plates is greater than the cross-sectional area of ​​the liquid outlet, the bottom end of the second tank body and the bottom end of the filter element can be movably fitted to the bottom plate, and the first tank body is symmetrically provided with an adjusting mechanism for driving the bottom plate to move in the horizontal direction.

[0006] By adopting the above technical solution, providing a bottom plate, a filter element, etc., when preparing homocysteine, first, raw materials DL-methionine, concentrated sulfuric acid and 48% hydrobromic acid are introduced into the reaction chamber from the first liquid inlet pipe, and hot water is introduced into the heating chamber from the second liquid inlet pipe, and the rotating mechanism is turned on to drive the second tank body to rotate, so that the raw materials are mixed with the movement of the second tank body after being added to the second tank body, and the bottom of the second tank body is heated more evenly. At this time, the two bottom plates collide with each other to form a disc shape, and the second tank body, the first tank body and the two bottom plates form a closed reaction chamber. The raw materials undergo hydrolysis reaction in the reaction chamber. After a period of reaction, an appropriate amount of alkaline neutralizing agent (such as hydrogen phosphate) is added from the first liquid inlet pipe. Sodium oxide, sodium bicarbonate, etc.), the reaction liquid undergoes precipitation reaction. In this process, the liquid outlet pipe is opened to release the hot water in the heating chamber. After the precipitation reaction is complete, the two regulating mechanisms of the symmetrically arranged buckets are opened to drive the two bottom plates away from each other, so that the liquid outlet at the bottom end of the second tank body is opened. After the reaction liquid passes through the filter element, it flows from between the two bottom plates to the bottom end of the first tank body, and then flows out from the liquid outlet pipe. After the filtration is completed, the regulating mechanism is opened to drive the two bottom plates closer to each other until they conflict with each other, and the liquid outlet is closed. Then, an appropriate amount of hydrochloric acid is added from the first liquid inlet pipe to dissolve the precipitate with hydrochloric acid. In this process, pure water is introduced from the second liquid inlet pipe to rinse the heating chamber, and then an appropriate amount of activated carbon is added to the reaction liquid. The reaction liquid is decolorized, and then the regulating mechanism is opened to drive the two bottom plates away from each other, so that the reaction liquid flows out from the liquid outlet through the liquid outlet pipe, and the collected reaction liquid can be subjected to the next electrolysis reaction. After the production is completed, when the first tank body needs to be cleaned, the lifting mechanism is opened to drive the filter element to rise, and then the cleaning liquid is introduced from the first liquid inlet pipe to clean the first tank body, and at the same time, the activated carbon particles in the reaction cavity are washed away from the gap between the filter element and the second tank body; by setting the second tank body, the filter element, the bottom plate, etc., the first tank body is divided into a reaction cavity and a heating cavity, and the movement of the bottom plate is controlled by the regulating mechanism to control the opening and closing of the liquid outlet, and the filter element is cooperated to clean the sediment in the first tank body. Filtering is performed, and after dissolution and decolorization, filtering is performed again to obtain the required reaction liquid. There is no need to perform operations such as filtering and dissolving on the reaction liquid after transfer, thereby avoiding product loss caused by the transfer process and achieving the effect of improving the yield of the finished product; at the same time, during the process of adding hydrochloric acid, the rotating mechanism drives the second tank body to rotate around the first tank body, so that the hydrochloric acid added from the top of the first tank body can wash down the precipitate attached to the inner wall of the top of the second tank body, thereby facilitating the subsequent hydrochloric acid to completely dissolve the precipitate, avoiding the loss caused by the precipitate attached to the top of the second tank body; the lifting mechanism controls the lifting of the filter element, which can facilitate the cleaning of the activated carbon particles remaining in the second tank body after the reaction, thereby avoiding affecting the progress of the subsequent reaction;In addition, by adding hydrobromic acid to lower the temperature required for the hydrolysis reaction, hot water can be directly introduced through the second liquid inlet pipe for water bath heating. Since the bottom of the second tank is immersed in the hot water in the heating chamber, and the second tank rotates slowly, the heating efficiency of the hot water in the heating chamber on the reaction liquid is improved.

[0007] The present invention is further configured as follows: the adjustment mechanism includes an adjustment screw rod that is arranged on the first tank body and rotates in a horizontal direction, and an adjustment block that is cooperated with the adjustment screw rod, the bottom of the base plate is fixedly connected to the adjacent adjustment block, and a first motor for driving the adjustment screw rod to rotate is provided on the outer wall of the first tank body.

[0008] By adopting the above technical solution, the equipment includes adjusting the screw rod and the adjusting block, etc., and when the liquid outlet needs to be opened, the two first motors are turned on to drive the bottom plate close to the inner wall of the first tank body, and the two bottom plates are moved away from each other, so that the liquid outlet is opened, and the reaction liquid in the second tank body is filtered through the filter element. When the liquid outlet needs to be closed, the two first motors are turned on to drive the two bottom plates close to each other until the bottom plates collide with each other; therefore, the movement of the bottom plates is driven by adjusting the screw rod, the structure is simple, and the operation is convenient.

[0009] The present invention is further configured as follows: a long first fixing plate is horizontally arranged inside the first tank body, the central axis of the first fixing plate is perpendicular to the central axis of the adjusting screw, a circular second fixing plate is horizontally arranged on the first fixing plate, the bottom ends of the second tank body and the filter element are movably fitted to the second fixing plate, and the top end of the bottom plate can be movably fitted to the bottom ends of the first fixing plate and the second fixing plate.

[0010] By adopting the above technical solution, a first fixing plate and a second fixing plate are provided. On the one hand, the first fixing plate is provided between the bottom end of the second tank body and the bottom plate, so that the gravity of the reaction liquid in the second tank body can directly act on the first fixing plate, thereby preventing the gravity of the reaction liquid from directly acting between the two bottom plates, thereby preventing the reaction liquid from leaking from between the two bottom plates. On the other hand, the bottom end of the second tank body acts on the annular second fixing plate. When the second tank body rotates, the second fixing plate always remains stationary. The first fixing plate and the second fixing plate form support for the second tank body, thereby improving the stability of the second tank body during rotation.

[0011] The present invention is further configured as follows: the filter element includes a first filter plate with a circular cross-section and a second filter plate with a truncated cone shape arranged at the bottom of the first filter plate, the lifting mechanism includes a rotating screw arranged at the bottom of the first tank body and rotating in a vertical direction, and a lifting cylinder cooperated with the rotating screw, the bottom end of the first tank body is provided with a second motor for driving the rotating screw to rotate, the top of the lifting cylinder movably fits the first filter plate, the top end of the rotating screw moves through the first filter plate, the rotating screw moves through the first fixed plate, and the bottom plate is provided with a positioning groove with a semicircular cross-section that cooperates with the rotating screw on one side close to the rotating screw.

[0012] By adopting the above technical solution, a rotating screw, a lifting cylinder, etc. are provided. After the reaction is completed, when the activated carbon particles in the second tank need to be cleaned, the liquid outlet is in an open state at this time, the second motor is turned on to drive the rotating screw to rotate, driving the lifting cylinder to rise, and the lifting cylinder pushes the first filter plate to rise, so that the filter element is separated from the second tank. Then, a cleaning liquid is introduced from the first liquid inlet pipe to flush out the activated carbon particles in the second tank. The activated carbon particles flow out from the liquid outlet pipe with the cleaning liquid. During the process of introducing the cleaning liquid, the rotating mechanism is turned on to drive the second tank to rotate, so that the cleaning liquid can fully rinse the top of the second tank, preventing the activated carbon particles from adhering to the bottom of the second tank and affecting the subsequent reaction. After the cleaning is completed, the second motor is turned on to drive the lifting cylinder to descend. The first filter plate descends with the lifting cylinder under the action of gravity until the bottom end of the second filter plate contacts the second fixed plate. At this time, the bottom of the second filter plate is movably attached to the inner wall of the bottom of the second tank. Therefore, by providing the rotating screw, etc., the first filter plate can be lifted and lowered, which is convenient for cleaning the activated carbon particles in the second tank and avoiding affecting the normal progress of the subsequent reaction.

[0013] The present invention is further configured as follows: the rotating mechanism includes a first rotating shaft arranged on the top of the first tank body and rotating in a vertical direction, and a rotating disk arranged horizontally on the first rotating shaft, a plurality of first rotating rods are evenly arranged on the rotating disk in an oblique downward direction, the bottom end of the first rotating rod is fixedly connected to the upper side wall of the second tank body, a third motor for driving the first rotating shaft to rotate is provided at the top of the first tank body, a set distance is provided between the bottom end of the first rotating shaft and the top end of the rotating screw screw, a plurality of second rotating rods are vertically arranged on the rotating disk, and the bottom end of the second rotating rod moves through the first filter plate.

[0014] By adopting the above technical solution, a first rotating shaft, a first rotating rod, etc. are set. During the process of adding raw materials or conducting the reaction, the third motor can be turned on to drive the first rotating shaft to rotate slowly. The first rotating shaft drives the second tank body and the filter element to rotate respectively through the first rotating rod and the second rotating rod, so that during the rotation of the second tank body, the added raw materials can flush the top and side walls of the second tank body, preventing the solids produced by the reaction or the added activated carbon particles from adhering to the top of the second tank body, making the reaction more complete; at the same time, during the rotation of the second tank body, the reaction liquid can be driven to flow to a certain extent, thereby accelerating the reaction.

[0015] The present invention is further configured as follows: a return spring is provided between the rotating disc and the first filter plate, and the central axes of the first rotating shaft and the rotating screw coincide with the central axis of the return spring.

[0016] By adopting the above technical solution, in the process of rotating the screw rod to drive the lifting cylinder to rise, the return spring is pushed to be compressed, driving the first filter plate to rise. After completing the cleaning of the activated carbon, the second motor is turned on to drive the rotating screw rod to rotate, driving the lifting cylinder to descend. In the process of descending the lifting cylinder, the elastic force of the return spring acts on the first filter plate, causing the filter element to descend with the lifting cylinder until the filter element hits the second fixed plate. Therefore, by setting the return spring, the filter element can be synchronously lowered with the lifting cylinder under the action of the return spring until it hits the second fixed plate, and at the same time ensure that the filter element can always hit the second fixed plate during the process of rotating with the first rotating shaft, avoiding the gap between the filter element and the second tank body during the reaction process, affecting the filtering effect of the reaction product.

[0017] The present invention is further configured as follows: a cylindrical second rotating shaft is provided on the first tank body to rotate in a direction coinciding with the central axis of the first rotating shaft, the inner wall of the second rotating shaft is movably fitted to the inner wall of the first rotating shaft, a stirring shaft is symmetrically provided on the second rotating shaft, a first rotating wheel is provided at the top end of the second rotating shaft, a second rotating wheel is provided at the top end of the first tank body to rotate, a synchronous belt is provided between the first rotating wheel and the second rotating wheel, and a fourth motor for driving the second rotating wheel to rotate is provided at the top end of the first tank body.

[0018] By adopting the above technical solution, during the reaction process, the fourth motor is turned on, and the second rotating shaft is driven by the synchronous belt to rotate in the opposite direction of the first rotating shaft, so that the stirring shaft stirs the reaction liquid in the second tank body. At the same time, the second tank body rotates slowly under the drive of the first rotating shaft, thereby generating convection between the middle part of the reaction liquid and the reaction liquid near the side wall of the second tank body, thereby making the reaction liquid mixed more evenly and improving the reaction rate.

[0019] The present invention is further configured as follows: a third long fixed plate is arranged in the horizontal direction in the first tank body, the central axis of the third fixed plate is in the same horizontal plane as the central axis of the first fixed plate, the bottom end of the third fixed plate is provided with a guide block in a direction parallel to the central axis of the adjusting screw rod, and the top end of the bottom plate is provided with a guide groove matching the guide block.

[0020] By adopting the above technical solution, on the one hand, a cross-shaped support structure is formed between the third fixed plate and the first fixed plate, which can provide more effective support for the second tank body, making the second tank body more stable; on the other hand, the guide block at the bottom of the third fixed plate can guide the two bottom plates, and also increase the connection between the bottom plate and the third fixed plate, making the movement process of the two bottom plates more stable.

[0021] The present invention is further configured as follows: a cleaning plate with a trapezoidal longitudinal cross-section is fixedly provided on the rotating screw in the vertical direction, the end of the cleaning plate can be movably fitted to the second filter plate, and the bottom end of the cleaning plate can be movably fitted to the top ends of the first fixed plate and the third fixed plate.

[0022] By adopting the above technical solution, a cleaning plate is provided. On the one hand, during the reaction process, the second tank body and the filter element rotate slowly with the first rotating shaft, and the cleaning plate remains stationary, so that the cleaning plate can generate relative movement with the second filter plate. The cleaning plate cleans the bottom of the second filter plate, which can avoid the generated sediment from clogging the second filter plate to a certain extent; on the other hand, when the rotating screw rotates and drives the lifting cylinder to rise and fall, it also drives the cleaning plate to rotate. The cleaning plate can clean the activated carbon particles that may remain on the top of the first fixed plate and the second fixed plate, avoiding the activated carbon particles from staying on the first fixed plate and the third fixed plate and affecting the subsequent reaction.

[0023] The beneficial effects of the present invention are:

[0024] 1. By setting a second tank body, a filter element, a bottom plate, etc., the first tank body is divided into a reaction chamber and a heating chamber. The bottom plate is controlled to move by an adjusting mechanism, thereby controlling the opening and closing of the liquid outlet. In conjunction with the filter element, the precipitate is filtered in the first tank body, and after dissolution and decolorization, it is filtered again to obtain the required reaction liquid. There is no need to filter and dissolve the reaction liquid after transfer, thereby avoiding product loss caused by the transfer process and achieving the effect of improving the yield of the finished product. At the same time, during the addition of hydrochloric acid, the rotating mechanism drives the second tank body to rotate around the first tank body, so that the hydrochloric acid added from the top of the first tank body can remove the hydrochloric acid attached to the second tank body. The precipitates on the inner wall of the top of the tank body are washed down, making it easier for the subsequent hydrochloric acid to completely dissolve the precipitates, thereby avoiding losses caused by the precipitates adhering to the top of the second tank body; by controlling the lifting and lowering of the filter element through the lifting mechanism, it is easy to clean the activated carbon particles remaining in the second tank body after the reaction, thereby avoiding affecting the progress of subsequent reactions; in addition, by adding hydrobromic acid to lower the temperature required for the hydrolysis reaction, hot water can be directly introduced from the second liquid inlet pipe for water bath heating. Since the bottom of the second tank body is immersed in the hot water in the heating chamber and the second tank body rotates slowly, the heating efficiency of the hot water in the heating chamber on the reaction liquid is improved.

[0025] 2. By arranging the first fixing plate and the second fixing plate, on the one hand, the first fixing plate is arranged between the bottom end of the second tank body and the bottom plate, so that the gravity of the reaction liquid in the second tank body can directly act on the first fixing plate, thereby preventing the gravity of the reaction liquid from directly acting between the two bottom plates, thereby preventing the reaction liquid from leaking from between the two bottom plates. On the other hand, the bottom end of the second tank body acts on the annular second fixing plate. When the second tank body rotates, the second fixing plate always remains stationary. The first fixing plate and the second fixing plate form support for the second tank body, thereby improving the stability of the second tank body during rotation.

[0026] 3. By setting a first rotating shaft, a first rotating rod, etc., during the process of adding raw materials or conducting a reaction, the third motor can be turned on to drive the first rotating shaft to rotate slowly. The first rotating shaft drives the second tank body and the filter element to rotate respectively through the first rotating rod and the second rotating rod, so that during the rotation of the second tank body, the added raw materials can flush the top and side walls of the second tank body, preventing the solids produced by the reaction or the added activated carbon particles from adhering to the top of the second tank body, making the reaction more complete; at the same time, the second tank body can drive the reaction liquid to flow to a certain extent during the rotation, thereby accelerating the reaction.

[0027] 4. By setting up a cleaning plate, on the one hand, during the reaction process, the second tank body and the filter element rotate slowly with the first rotating shaft, and the cleaning plate remains stationary, so that the cleaning plate can generate relative movement with the second filter plate, and the cleaning plate cleans the bottom of the second filter plate, which can avoid the generated sediment from clogging the second filter plate to a certain extent; on the other hand, when the rotating screw rotates and drives the lifting cylinder to rise and fall, it also drives the cleaning plate to rotate, and the cleaning plate can clean the activated carbon particles that may remain on the top of the first fixed plate and the second fixed plate, avoiding the activated carbon particles from staying on the first fixed plate and the third fixed plate and affecting the subsequent reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0029] Figure 1 This is a schematic structural diagram of an embodiment of an apparatus for preparing DL-homocysteine ​​thiolactone hydrochloride according to the present invention;

[0030] Figure 2 It is a partial cross-sectional structural diagram of an embodiment of an apparatus for preparing DL-homocysteine ​​thiolactone hydrochloride of the present invention;

[0031] Figure 3 yes Figure 2 A is an enlarged schematic diagram;

[0032] Figure 4 yes Figure 2 A magnified schematic diagram of middle B;

[0033] Figure 5 yes Figure 2 A magnified schematic diagram of middle C;

[0034] Figure 6 It is a partial cross-sectional structural diagram of an embodiment of an apparatus for preparing DL-homocysteine ​​thiolactone hydrochloride of the present invention;

[0035] Figure 7 yes Figure 6 A magnified schematic diagram of D in the middle;

[0036] Figure 8 yes Figure 6 Enlarged schematic diagram of E;

[0037] Figure 9 yes Figure 6 A magnified schematic diagram of F in the middle.

[0038] In the figure, 1, first tank body; 2, second tank body; 3, liquid outlet; 4, first connecting block; 5, reaction chamber; 6, heating chamber; 7, first liquid inlet pipe; 8, second liquid inlet pipe; 9, liquid outlet pipe; 10, filter element; 10a, first filter plate; 10b, second filter plate; 11, lifting mechanism; 11a, rotating screw rod; 11b, lifting cylinder; 12, rotating mechanism; 12a, first rotating shaft; 12b, rotating disk; 13, bottom plate; 14, adjusting mechanism; 14a, adjusting Screw rod; 14b, adjusting block; 15, first motor; 16, first fixed plate; 17, second fixed plate; 18, second motor; 19, positioning groove; 20, first rotating rod; 21, third motor; 22, second rotating rod; 23, return spring; 24, second rotating shaft; 25, stirring shaft; 26, first rotating wheel; 27, second rotating wheel; 28, synchronous belt; 29, fourth motor; 30, third fixed plate; 31, guide block; 32, guide groove; 33, cleaning plate. DETAILED DESCRIPTION

[0039] The technical solutions of the present invention will be described clearly and completely below with reference to specific embodiments. Obviously, the embodiments described are only some of the embodiments of the present invention, not all of them. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without inventive effort are also within the scope of protection of the present invention.

[0040] The present invention provides a method and equipment for preparing DL-homocysteine ​​thiolactone hydrochloride, such as Figures 1 to 9As shown, it includes a cylindrical first tank body 1, an inverted truncated cone-shaped second tank body 2 arranged inside the first tank body 1, and a liquid outlet 3 opened at the bottom of the second tank body 2, a circular first connecting block 4 is horizontally arranged on the top of the second tank body 2, the outer side of the first connecting block 4 is engaged with the inner wall of the first tank body 1, a reaction chamber 5 is formed between the upper side wall of the second tank body 2 and the top of the first tank body 1, a heating chamber 6 is formed between the lower side wall of the second tank body 2 and the bottom of the first tank body 1, a first liquid inlet pipe 7 connected to the reaction chamber 5 is provided on the top of the first tank body 1, a second liquid inlet pipe 8 connected to the heating chamber 6 is provided on the side wall of the first tank body 1, and a liquid inlet pipe 9 connected to the heating chamber 6 is provided at the bottom of the first tank body 1. The heating cavity 6 is connected to a liquid outlet pipe 9, and a truncated cone-shaped filter element 10 is movably provided on the liquid outlet 3. The bottom of the first tank body 1 is provided with a lifting mechanism 11 for driving the filter element 10 to rise, and the top of the first tank body 1 is provided with a rotating mechanism 12 for driving the second tank body 2 to rotate. The bottom of the second tank body 2 is symmetrically provided with a semicircular bottom plate 13 for controlling the opening and closing of the liquid outlet 3 in the horizontal direction. The sum of the cross-sectional areas of the two bottom plates 13 is greater than the cross-sectional area of ​​the liquid outlet 3. The bottom end of the second tank body 2 and the bottom end of the filter element 10 can be movably fitted on the bottom plate 13, and the first tank body 1 is symmetrically provided with an adjusting mechanism 14 for driving the bottom plate 13 to move in the horizontal direction.

[0041] Furthermore, the adjustment mechanism 14 includes an adjustment screw 14a that is arranged on the first tank body 1 and rotates in the horizontal direction, and an adjustment block 14b that is cooperated with the adjustment screw 14a. The bottom of the base plate 13 is fixedly connected to the adjacent adjustment block 14b, and a first motor 15 for driving the adjustment screw 14a to rotate is provided on the outer wall of the first tank body 1.

[0042] Furthermore, a long first fixing plate 16 is horizontally arranged inside the first tank body 1, and the central axis of the first fixing plate 16 is perpendicular to the central axis of the adjusting screw 14a. A circular second fixing plate 17 is horizontally arranged on the first fixing plate 16, and the bottom ends of the second tank body 2 and the filter element 10 are movably fitted to the second fixing plate 17, and the top end of the bottom plate 13 can be movably fitted to the bottom ends of the first fixing plate 16 and the second fixing plate 17.

[0043] Furthermore, the filter element 10 includes a first filter plate 10a with a circular cross-section and a second filter plate 10b with a truncated cone shape arranged at the bottom of the first filter plate 10a. The lifting mechanism 11 includes a rotating screw 11a arranged at the bottom of the first tank body 1 and rotating in a vertical direction, and a lifting cylinder 11b cooperated with the rotating screw 11a. The bottom end of the first tank body 1 is provided with a second motor 18 for driving the rotating screw 11a to rotate. The top of the lifting cylinder 11b is movably fitted to the first filter plate 10a, the top of the rotating screw 11a moves through the first filter plate 10a, and the rotating screw 11a moves through the first fixed plate 16. The bottom plate 13 is provided with a positioning groove 19 with a semicircular cross-section that cooperates with the rotating screw 11a on one side close to the rotating screw 11a.

[0044] Furthermore, the rotating mechanism 12 includes a first rotating shaft 12a vertically arranged on the top of the first tank body 1 and a rotating disc 12b horizontally arranged on the first rotating shaft 12a, and a plurality of first rotating rods 20 are evenly arranged on the rotating disc 12b in an oblique downward direction, and the bottom end of the first rotating rod 20 is fixedly connected to the upper side wall of the second tank body 2, and a third motor 21 for driving the first rotating shaft 12a to rotate is provided at the top of the first tank body 1, and a set distance is provided between the bottom end of the first rotating shaft 12a and the top end of the rotating screw 11a, and a plurality of second rotating rods 22 are vertically arranged on the rotating disc 12b, and the bottom end of the second rotating rod 22 moves through the first filter plate 10a.

[0045] Furthermore, a return spring 23 is provided between the rotating disc 12 b and the first filter plate 10 a , and the central axes of the first rotating shaft 12 a and the rotating screw 11 a coincide with the central axis of the return spring 23 .

[0046] Furthermore, a cylindrical second rotating shaft 24 is provided on the first tank body 1 to rotate in a direction coinciding with the central axis of the first rotating shaft 12a, and the inner wall of the second rotating shaft 24 is movably fitted to the inner wall of the first rotating shaft 12a. A stirring shaft 25 is symmetrically provided on the second rotating shaft 24, and a first rotating wheel 26 is provided at the top of the second rotating shaft 24. A second rotating wheel 27 is rotatably provided at the top of the first tank body 1, and a synchronous belt 28 is provided between the first rotating wheel 26 and the second rotating wheel 27. A fourth motor 29 for driving the second rotating wheel 27 to rotate is provided at the top of the first tank body 1.

[0047] Furthermore, a third long fixed plate 30 is horizontally arranged in the first tank body 1, and the central axis of the third fixed plate 30 is in the same horizontal plane as the central axis of the first fixed plate 16. The bottom end of the third fixed plate 30 is provided with a guide block 31 in a direction parallel to the central axis of the adjusting screw rod 14a, and the top end of the bottom plate 13 is provided with a guide groove 32 that cooperates with the guide block 31.

[0048] Furthermore, a cleaning plate 33 with a trapezoidal longitudinal cross-section is fixedly provided on the rotating screw 11a in the vertical direction, and the end of the cleaning plate 33 can be movably fitted to the second filter plate 10b, and the bottom end of the cleaning plate 33 can be movably fitted to the top of the first fixed plate 16 and the third fixed plate 30.

[0049] When preparing homocysteine, first, the raw materials DL-methionine, concentrated sulfuric acid and 48% hydrobromic acid are introduced into the reaction chamber 5 from the first liquid inlet pipe 7, and hot water is introduced into the heating chamber 6 from the second liquid inlet pipe 8, and the third motor 21 and the fourth motor 29 are turned on, and the second tank body 2 and the filter element 10 are driven to rotate by the first rotating shaft 12a, the first rotating rod 20 and the second rotating rod 22, so that the raw materials are mixed with the movement of the second tank body 2 after being added to the second tank body 2, and the bottom of the second tank body 2 is heated more evenly. The stirring shaft 25 is driven to rotate by the second rotating shaft 24 to mix the reaction liquid. At this time, the two bottom plates 13 conflict with each other to form a disc shape, and the second tank body 2. The first tank body 1 and the two bottom plates 13 form a closed reaction chamber 5. The raw materials undergo a hydrolysis reaction in the reaction chamber 5. After a period of reaction, an appropriate amount of alkaline neutralizing agent (such as sodium hydroxide, sodium bicarbonate, etc.) is added from the first liquid inlet pipe 7, and the reaction liquid undergoes a precipitation reaction. In this process, the liquid outlet pipe 9 is opened to release the hot water in the heating chamber 6. After the precipitation reaction is complete, the two symmetrically arranged first motors 15 are turned on to drive the two bottom plates 13 away from each other, so that the liquid outlet 3 at the bottom end of the second tank body 2 is opened. After the reaction liquid passes through the second filter plate 10b and is filtered, it flows from between the two bottom plates 13 to the bottom end of the first tank body 1, and then flows out from the liquid outlet pipe 9. After the filtration is completed, the reaction liquid is opened. Turn on the first motor 15 to drive the two bottom plates 13 closer to each other until they collide with each other, and the liquid outlet 3 is closed. Then, an appropriate amount of hydrochloric acid is added from the first liquid inlet pipe 7 to dissolve the precipitate. In this process, pure water is introduced from the second liquid inlet pipe 8 to rinse the heating chamber 6. Then, an appropriate amount of activated carbon is added from the first liquid inlet pipe 7 to decolorize the reaction liquid. Then, turn on the first motor 15 to drive the two bottom plates 13 away from each other, so that the reaction liquid flows out from the liquid outlet 3 through the liquid outlet pipe 9 after filtration. The collected reaction liquid can then be subjected to the next electrolysis reaction. After production is completed, when the first tank body 1 needs to be cleaned, turn on the second motor 18, and the lifting cylinder 11b pushes the filter element 10 up. , then a cleaning liquid is introduced from the first liquid inlet pipe 7 to clean the first tank body 1, and at the same time, the activated carbon particles in the reaction chamber 5 are flushed out from the gap between the filter element 10 and the second tank body 2; by arranging the second tank body 2, the filter element, the bottom plate 13, etc., the first tank body 1 is divided into a reaction chamber 5 and a heating chamber 6, and the movement of the bottom plate 13 is controlled by the adjustment mechanism 14, thereby controlling the opening and closing of the liquid outlet 3, and cooperating with the filter element 10, the precipitate is filtered in the first tank body 1, and after dissolution and decolorization, it is filtered again to obtain the required reaction liquid. There is no need to perform filtering and dissolving operations on the reaction liquid after transfer, thereby avoiding product loss caused by the transfer process, thereby achieving the effect of improving the yield of the finished product;During the addition of hydrochloric acid, the rotating mechanism 12 drives the second tank body 2 to rotate about the first tank body 1, allowing the hydrochloric acid added from the top of the first tank body 1 to flush out the precipitate attached to the inner wall of the top of the second tank body 2, thereby facilitating the subsequent complete dissolution of the precipitate by the hydrochloric acid and preventing loss caused by the precipitate adhering to the top of the second tank body 2. The lifting mechanism 11 controls the lifting and lowering of the filter element 10, facilitating the removal of activated carbon particles remaining in the second tank body 2 after the reaction, thereby preventing interference with subsequent reactions. Furthermore, by adding hydrobromic acid to lower the temperature required for the hydrolysis reaction, hot water can be directly introduced from the second liquid inlet pipe 8 for water bath heating. Since the bottom of the second tank body 2 is immersed in the hot water in the heating chamber 6 and the second tank body 2 rotates slowly, the heating efficiency of the hot water in the heating chamber 6 on the reaction liquid is improved.

[0050] By providing the adjusting screw rod 14a and the adjusting block 14b, etc., when the liquid outlet 3 needs to be opened, the two first motors 15 are turned on to drive the bottom plate 13 to approach the inner wall of the first tank body 1, and the two bottom plates 13 are moved away from each other, so that the liquid outlet 3 is opened and the reaction liquid in the second tank body 2 is filtered through the filter element 10. When the liquid outlet 3 needs to be closed, the two first motors 15 are turned on to drive the two bottom plates 13 to approach each other until the bottom plates 13 collide with each other; therefore, the bottom plates 13 are driven to move by the adjusting screw rod 14a, which has a simple structure and is easy to operate.

[0051] By arranging the first fixing plate 16 and the second fixing plate 17, on the one hand, the first fixing plate 16 is arranged between the bottom end of the second tank body 2 and the bottom plate 13, so that the gravity of the reaction liquid in the second tank body 2 can directly act on the first fixing plate 16, thereby preventing the gravity of the reaction liquid from directly acting between the two bottom plates 13, thereby preventing the reaction liquid from leaking from between the two bottom plates 13. On the other hand, the bottom end of the second tank body 2 acts on the annular second fixing plate 17. When the second tank body 2 rotates, the second fixing plate 17 always remains stationary. The first fixing plate 16 and the second fixing plate 17 support the second tank body 2, thereby improving the stability of the second tank body 2 during rotation.

[0052] By setting the rotating screw rod 11a, the lifting cylinder 11b, etc., after the reaction is completed, when the activated carbon particles in the second tank body 2 need to be cleaned, the liquid outlet 3 is in the open state, the second motor 18 is turned on, the rotating screw rod 11a is driven to rotate, and the lifting cylinder 11b is driven to rise. The lifting cylinder 11b pushes the first filter plate 10a to rise, so that the filter element 10 is separated from the second tank body 2, and then the cleaning liquid is introduced from the first liquid inlet pipe 7 to flush out the activated carbon particles in the second tank body 2. The activated carbon particles flow out from the liquid outlet pipe 9 with the cleaning liquid. In the process of introducing the cleaning liquid, the rotating mechanism 12 is turned on to drive the second tank body 2 to rotate, so that the cleaning liquid can It is enough to fully rinse the top of the second tank body 2 to prevent the activated carbon particles from adhering to the bottom of the second tank body 2 and affecting the subsequent reaction. After cleaning is completed, the second motor 18 is turned on to drive the lifting cylinder 11b to descend, and the first filter plate 10a descends with the lifting cylinder 11b under the action of gravity until the bottom end of the second filter plate 10b hits the second fixed plate 17. At this time, the bottom of the second filter plate 10b is movably fitted to the inner wall of the bottom of the second tank body 2; therefore, by setting the rotating screw 11a, etc., the first filter plate 10a can be lifted and lowered, which is convenient for cleaning the activated carbon particles in the second tank body 2 and avoiding affecting the normal progress of the subsequent reaction.

[0053] By setting the first rotating shaft 12a, the first rotating rod 20, etc., during the process of adding raw materials or conducting the reaction, the third motor 21 can be turned on to drive the first rotating shaft 12a to rotate slowly. The first rotating shaft 12a drives the second tank body 2 and the filter element 10 to rotate respectively through the first rotating rod 20 and the second rotating rod 22, so that during the rotation of the second tank body 2, the added raw materials can flush the top and side walls of the second tank body 2, preventing the solids produced by the reaction or the added activated carbon particles from adhering to the top of the second tank body 2, making the reaction more complete; at the same time, during the rotation of the second tank body 2, the second tank body 2 can drive the reaction liquid to flow to a certain extent, thereby accelerating the reaction.

[0054] By providing a return spring 23, when the rotating screw rod 11a drives the lifting cylinder 11b to rise, the return spring 23 is pushed to be compressed, driving the first filter plate 10a to rise. After the activated carbon is cleaned, the second motor 18 is turned on to drive the rotating screw rod 11a to rotate, driving the lifting cylinder 11b to descend. During the descending process of the lifting cylinder 11b, the elastic force of the return spring 23 acts on the first filter plate 10a, causing the filter element 10 to descend with the lifting cylinder 11b until the filter element 10 hits the second fixed plate 17. Therefore, by providing a return spring 23, the filter element 10 can be synchronously lowered with the lifting cylinder 11b under the action of the return spring 23 until it hits the second fixed plate 17, and at the same time ensure that the filter element 10 can always hit the second fixed plate 17 during the rotation process of the first rotating shaft 12a, thereby avoiding a gap between the filter element 10 and the second tank body 2 during the reaction process, which affects the filtering effect of the reaction product.

[0055] By providing a second rotating shaft 24, a stirring shaft 25, etc., during the reaction process, the fourth motor 29 is turned on, and the second rotating shaft 24 is driven by the synchronous belt 28 to rotate in the opposite direction of the first rotating shaft 12a, so that the stirring shaft 25 stirs the reaction liquid in the second tank body 2. At the same time, the second tank body 2 rotates slowly under the drive of the first rotating shaft 12a, thereby generating convection between the middle of the reaction liquid and the reaction liquid near the side wall of the second tank body 2, thereby making the reaction liquid mixed more evenly and improving the reaction rate.

[0056] By providing the third fixing plate 30, the guide block 31, etc., on the one hand, a cross-shaped support structure is formed between the third fixing plate 30 and the first fixing plate 16, which can provide more effective support for the second tank body 2, making the second tank body 2 more stable; on the other hand, the guide block 31 at the bottom of the third fixing plate 30 can guide the two bottom plates 13, and also increase the connection between the bottom plate 13 and the third fixing plate 30, so that the movement process of the two bottom plates 13 is more stable.

[0057] By providing the cleaning plate 33, on the one hand, during the reaction process, the second tank body 2 and the filter element 10 slowly rotate along with the first rotating shaft 12a, and the cleaning plate 33 remains stationary, so that the cleaning plate 33 can generate relative movement with the second filter plate 10b, and the cleaning plate 33 cleans the bottom of the second filter plate 10b, which can avoid the generated sediment from clogging the second filter plate 10b to a certain extent; on the other hand, when the rotating screw 11a rotates and drives the lifting cylinder 11b to rise and fall, it also drives the cleaning plate 33 to rotate, and the cleaning plate 33 can clean the activated carbon particles that may remain on the top of the first fixed plate 16 and the second fixed plate 17, thereby preventing the activated carbon particles from staying on the first fixed plate 16 and the third fixed plate 30 and affecting the subsequent reaction.

[0058] It should be noted that the various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same and similar parts between the various embodiments can be referenced to each other.

[0059] The above description is only a description of the preferred embodiments of the present invention and does not limit the scope of the present invention. Any changes and modifications made by ordinary technicians in the field of the present invention based on the above disclosure shall fall within the scope of protection of the claims.

Claims

1. A DL-homocysteine ​​thiolactone hydrochloride preparation device, characterized in that: The invention comprises a cylindrical first tank body (1), an inverted truncated cone-shaped second tank body (2) arranged inside the first tank body (1), and a liquid outlet (3) opened at the bottom of the second tank body (2); a first annular connecting block (4) is horizontally arranged on the top of the second tank body (2); the outer side of the first connecting block (4) is engaged with the inner wall of the first tank body (1); a reaction chamber (5) is formed between the upper side wall of the second tank body (2) and the top of the first tank body (1); a heating chamber (6) is formed between the lower side wall of the second tank body (2) and the bottom of the first tank body (1); a first liquid inlet pipe (7) connected to the reaction chamber (5) is arranged on the top of the first tank body (1); a second liquid inlet pipe (8) connected to the heating chamber (6) is arranged on the side wall of the first tank body (1); and a liquid inlet pipe (9) connected to the heating chamber (6) is arranged at the bottom of the first tank body (1). The heating chamber (6) is connected to a liquid outlet pipe (9), a truncated cone-shaped filter element (10) is movably arranged on the liquid outlet (3), a lifting mechanism (11) for driving the filter element (10) to rise is arranged at the bottom of the first tank body (1), a rotating mechanism (12) for driving the second tank body (2) to rotate is arranged at the top of the first tank body (1), a semicircular bottom plate (13) for controlling the opening and closing of the liquid outlet (3) is symmetrically arranged at the bottom of the second tank body (2) in a horizontal direction, the sum of the cross-sectional areas of the two bottom plates (13) is greater than the cross-sectional area of ​​the liquid outlet (3), the bottom end of the second tank body (2) and the bottom end of the filter element (10) can both be movably fitted on the bottom plate (13), and the first tank body (1) is symmetrically arranged with an adjusting mechanism (14) for driving the bottom plate (13) to move in a horizontal direction.

2. A DL-homocysteine ​​thiolactone hydrochloride preparation device according to claim 1, characterized in that: The adjusting mechanism (14) comprises an adjusting screw (14a) rotatably arranged on the first tank body (1) in a horizontal direction and an adjusting block (14b) cooperating with the adjusting screw (14a); the bottom of the bottom plate (13) is fixedly connected to the adjacent adjusting block (14b); and a first motor (15) for driving the adjusting screw (14a) to rotate is arranged on the outer wall of the first tank body (1).

3. A DL-homocysteine ​​thiolactone hydrochloride preparation device according to claim 2, characterized in that: A first strip-shaped fixing plate (16) is horizontally arranged inside the first tank body (1), the central axis of the first fixing plate (16) is perpendicular to the central axis of the adjusting screw rod (14a), a second ring-shaped fixing plate (17) is horizontally arranged on the first fixing plate (16), the bottom ends of the second tank body (2) and the filter element (10) are movably fitted to the second fixing plate (17), and the top end of the bottom plate (13) is movably fitted to the bottom ends of the first fixing plate (16) and the second fixing plate (17).

4. The DL-homocysteine ​​thiolactone hydrochloride preparation device according to claim 3, characterized in that: The filter element (10) comprises a first filter plate (10a) with a circular cross section and a second filter plate (10b) with a truncated cone shape arranged at the bottom of the first filter plate (10a); the lifting mechanism (11) comprises a rotating screw (11a) arranged at the bottom of the first tank body (1) and rotating in a vertical direction, and a lifting cylinder (11b) arranged in cooperation with the rotating screw (11a); a second motor (18) for driving the rotating screw (11a) to rotate is arranged at the bottom of the first tank body (1); the top of the lifting cylinder (11b) is movably fitted to the first filter plate (10a); the top of the rotating screw (11a) movably passes through the first filter plate (10a); the rotating screw (11a) movably passes through the first fixing plate (16); and a positioning groove (19) with a semicircular cross section and matching with the rotating screw (11a) is provided on a side of the bottom plate (13) close to the rotating screw (11a).

5. The DL-homocysteine ​​thiolactone hydrochloride preparation device according to claim 4, characterized in that: The rotating mechanism (12) comprises a first rotating shaft (12a) arranged vertically and rotatably on the top of the first tank body (1) and a rotating disc (12b) arranged horizontally on the first rotating shaft (12a); a plurality of first rotating rods (20) are evenly arranged on the rotating disc (12b) in an oblique downward direction; the bottom ends of the first rotating rods (20) are fixedly connected to the upper side wall of the second tank body (2); a third motor (21) for driving the first rotating shaft (12a) to rotate is arranged at the top of the first tank body (1); a set distance is provided between the bottom end of the first rotating shaft (12a) and the top end of the rotating screw (11a); a plurality of second rotating rods (22) are vertically arranged on the rotating disc (12b); the bottom ends of the second rotating rods (22) moveably pass through the first filter plate (10a).

6. The DL-homocysteine ​​thiolactone hydrochloride preparation device according to claim 5, characterized in that: A return spring (23) is provided between the rotating disc (12b) and the first filter plate (10a), and the central axes of the first rotating shaft (12a) and the rotating screw rod (11a) coincide with the central axis of the return spring (23).

7. The DL-homocysteine ​​thiolactone hydrochloride preparation device according to claim 5, characterized in that: A cylindrical second rotating shaft (24) is rotatably arranged on the first tank body (1) in a direction coincident with the central axis of the first rotating shaft (12a); the inner wall of the second rotating shaft (24) is movably fitted to the inner wall of the first rotating shaft (12a); a stirring shaft (25) is symmetrically arranged on the second rotating shaft (24); a first rotating wheel (26) is arranged at the top end of the second rotating shaft (24); a second rotating wheel (27) is rotatably arranged at the top end of the first tank body (1); a synchronous belt (28) is arranged between the first rotating wheel (26) and the second rotating wheel (27); and a fourth motor (29) for driving the second rotating wheel (27) to rotate is arranged at the top end of the first tank body (1).

8. The DL-homocysteine ​​thiolactone hydrochloride preparation device according to claim 5, characterized in that: A third strip-shaped fixing plate (30) is arranged in the first tank body (1) along the horizontal direction, the central axis of the third fixing plate (30) and the central axis of the first fixing plate (16) are in the same horizontal plane, the bottom end of the third fixing plate (30) is provided with a guide block (31) in a direction parallel to the central axis of the adjusting screw rod (14a), and the top end of the bottom plate (13) is provided with a guide groove (32) matched with the guide block (31).

9. The DL-homocysteine ​​thiolactone hydrochloride preparation device according to claim 8, characterized in that: A cleaning plate (33) having a trapezoidal longitudinal section is fixedly arranged on the rotating screw rod (11a) in the vertical direction, and the end of the cleaning plate (33) can be movably fitted to the second filter plate (10b), and the bottom end of the cleaning plate (33) can be movably fitted to the top ends of the first fixed plate (16) and the third fixed plate (30).

10. The DL-homocysteine ​​thiolactone hydrochloride preparation device according to claim 1, characterized in that: The method for preparing homocysteine ​​using a homocysteine ​​preparation device specifically comprises the following steps: (a) DL-methionine, concentrated sulfuric acid and 48% hydrobromic acid are introduced into a first tank (1) at a mass ratio of 1:2:1 through a first liquid inlet pipe (7) for hydrolysis, hot water is introduced through a second liquid inlet pipe (8), the reaction temperature is controlled at 90-100° C., and the temperature is kept at 90-10 hours; (b) adding alkaline liquid from the first liquid inlet pipe (7) to neutralize the hydrolyzate of step (a) to a pH of 6-7; (c) opening the liquid outlet (3) and the liquid outlet pipe (9), filtering and separating the crude DL-homocysteine ​​produced in step (b); (d) closing the liquid outlet (3), adding hydrochloric acid from the first liquid inlet pipe (7), stirring until the crude DL-homocysteine ​​is completely dissolved, adding activated carbon for decolorization, then opening the bottom plate (13) and the liquid outlet pipe (9), filtering to obtain a clarified liquid; (e) electrolyzing the liquid obtained in step (d); (f) concentrating the crystals, filtering, and drying to collect the desired product.

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