Free device for phenylethylamine salt compound
By improving the phenylethylamine salt compound release device, using a diaphragm pump and precision filter to remove impurities, combined with airfoil axial flow agitation and nitrogen protection, the problems of large material loss, product inhomogeneity and difficult operation in the production of phenylethylamine salt compounds in the prior art have been solved, and a highly efficient and safe release process has been achieved.
Patent Information
- Application Number
- CN202422911493.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-28
- Publication Date
- 2025-11-07
- Estimated Expiration
- 2034-11-28
AI Technical Summary
The existing production process of phenethylamine salt compounds has problems such as large material loss, high cost, product inhomogeneity, easy adhesion and blockage due to multiple refining processes. In particular, the free process has problems such as excessive foaming and unclear liquid level, which makes operation difficult.
The freeing device, which connects the reaction vessel and the dropping tank, ensures the purity of the solution through a diaphragm pump and a precision filter. It uses an airfoil-type axial flow agitator to improve stirring efficiency and avoids foaming through a cross-shaped four-way connector and nitrogen protection before directly entering the centrifuge for processing.
It improves product yield and quality, reduces costs and labor intensity, avoids adhesion and blockage inside the vessel, and ensures product uniformity and safety.
Smart Images
Figure CN223517471U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model belongs to the technical field of medicine processing, and particularly relates to a free device for phenethylamine salt compound. BACKGROUND
[0002] The current production process of phenethylamine salt compound is generally as follows: optical pure alpha-phenethylamine obtained by resolving racemic alpha-phenethylamine with tartaric acid is used as basic resolving agent in the reaction, and then is reacted with a carboxylic acid intermediate material which needs to be resolved or purified to form a salt, and finally, the product is prepared through selective refining crystallization, filtration, free, concentration, beating, centrifugation and vacuum drying.
[0003] I. The product needs selective crystallization and multiple refining and beating, which increases the material loss in the centrifugation process, and because the multiple mother liquor is difficult to be recovered batch by batch, the solvent consumption is large, the cost is high, and the workload is large if mass production is carried out.
[0004] II. The free process will produce substances with uneven properties, which will have the following effects: (1) a large amount of foam is easily produced, the liquid level and solution condition in the kettle cannot be observed, the material is adhered everywhere, which often causes the bottom valve to be blocked in the subsequent centrifugation process, not only the centrifugation efficiency is low, but also the workload of the operator is increased; (2) the solid purity of the final product is not uniform, which easily leads to quality deviation; (3) a large amount of solid is often adhered to the inner wall of the free kettle, which is difficult to fall off, causing large product loss. SUMMARY
[0005] The utility model discloses a kind of free devices for phenethylamine salt compound, can obviously improve the property of phenethylamine salt compound free crystal, obtain the crystal with uniform property, reduce cost and work intensity simultaneously, improve product quality and yield.
[0006] The utility model discloses the technical scheme for solving above-mentioned problem is as follows: a kind of free device for phenethylamine salt compound, the free device includes reaction kettle, the reaction kettle is connected with the drip tank above the reaction kettle by adjusting valve, the reaction kettle is also connected with the drip tank by balance pipe, it is guaranteed that the reaction kettle and the drip tank pressure balance by balance pipe, avoid the violent analysis, agglomerate produced by uneven drop speed.
[0007] The upper interface of the cross four-way joint connected with the reaction kettle, the lower interface of the cross four-way joint is connected with centrifuge, the left interface of the cross four-way joint is connected with nitrogen storage tank, the right interface of the cross four-way joint is connected with diaphragm pump, the diaphragm pump is also sequentially connected with reaction kettle feed port by precision filter and adjusting valve;Adjusting valve is arranged at the four interfaces of the cross four-way joint.
[0008] Preferably, the left interface of the cross four-way joint is connected with a nitrogen tank through a nitrogen pipeline.
[0009] Preferably, the reaction kettle is provided with a stirring mechanism and a heating device; the wing type axial flow stirring is adopted, so that the rotating speed is greater than or equal to 100 revolutions per minute, and the free speed of the reaction liquid is increased.
[0010] More preferably, the stirring mechanism comprises a stirring shaft and a plurality of layers of stirring paddles arranged on the stirring shaft, and the plurality of layers of stirring paddles are wing type axial flow stirring paddles.
[0011] Preferably, the reaction kettle is connected with a dropping tank above the reaction kettle through a regulating valve and a dropping pipeline.
[0012] Preferably, the lower interface of the cross four-way joint is connected with a centrifuge through a discharging pipeline.
[0013] Compared with the prior art, the utility model has the advantages that:
[0014] The diaphragm pump in the utility model is sequentially connected with the feeding port of the reaction kettle through the precision filter and the regulating valve, so that the phenethylamine salt compound in the solution state is added into the reaction kettle through the precision filter, mechanical impurities and other foreign matters are removed, and the content, property, color and other indexes of the product after final crystallization are ensured to reach the standard.
[0015] (2) The reaction kettle in the utility model is connected with the dropping tank above the reaction kettle through the regulating valve, the upper interface of the cross four-way joint is connected with the reaction kettle, the lower interface of the cross four-way joint is connected with the centrifuge, the left interface of the cross four-way joint is connected with the nitrogen tank, and the regulating valve is arranged at the four interfaces of the cross four-way joint; in this way, the solvent in the dropping tank is uniformly added into the reaction kettle containing the phenethylamine salt reaction liquid, nitrogen gas is supplied into the reaction kettle to protect the positive pressure, the problems in the prior art, such as the generation of a large amount of foam in the free separation of the phenethylamine salt compound reaction liquid, unclear liquid level in the kettle, wall sticking, more block-shaped matters, easy clogging, difficult discharging, poor product stability and the like are avoided, the product yield and quality are improved, the cost is saved, the labor intensity is reduced, and after the free separation is completed, the regulating valves at the interfaces of the upper interface and the lower interface of the cross four-way joint are directly opened, so that the materials in the free separation reaction kettle are directly fed into the centrifuge, manual intermittent discharging is not needed, the safety risk in the centrifugal operation and the possibility of foreign matters are reduced. BRIEF DESCRIPTION OF DRAWINGS
[0016] Figure 1 It is a structure schematic view of the free separation device for the phenethylamine salt compound in the utility model embodiment.
[0017] Wherein: 1 is a reaction kettle, 2 is a dropping tank, 3 is a balance pipe, 4 is a cross four-way joint, 5 is a centrifuge, 6 is a nitrogen storage tank, 7 is a diaphragm pump, 8 is a precision filter, 9 is a nitrogen pipeline, 10 is a stirring mechanism, 11 is a dropping pipeline, 12 is a discharge pipeline. DETAILED DESCRIPTION
[0018] The utility model will be described in further detail below with the embodiments combined with the drawings.
[0019] As Figure 1 shown, the structure diagram of the free device of the phenethylamine salt compound in the embodiment.
[0020] A free device of phenethylamine salt compound, the free device includes reaction kettle 1, be provided with stirring mechanism 10 and heating device in reaction kettle 1, stirring mechanism 10 includes stirring shaft and the multilayer stirring paddle of setting on stirring shaft, the multilayer stirring paddle is wing type axial flow stirring paddle, reaction kettle 1 is connected the dropping tank 2 above reaction kettle 1 through adjusting valve, dropping pipeline 11, reaction kettle 1 is also connected dropping tank 2 through balance pipe 3, reaction kettle 1 connects the upper interface of cross four-way joint 4, the lower interface of cross four-way joint 4 is connected centrifuge 5 through discharge pipeline 12, the left interface of cross four-way joint 4 is connected nitrogen storage tank 6 through nitrogen pipeline 9, the right interface of cross four-way joint 4 connects diaphragm pump 7, diaphragm pump 7 is also connected reaction kettle 1 feed inlet in sequence through precision filter 8, adjusting valve, the adjusting valve is arranged in the four interfaces of cross four-way joint 4.
[0021] The working process of the embodiment will be described in detail below with the drawings:
[0022] The phenethylamine salt compound reaction solution to be freed is entered into reaction kettle 1 through diaphragm pump 7 and precision filter 8, and is stirred by stirring mechanism 10, the solvent in dropping tank 2 is added into reaction kettle 1 at a constant speed through adjusting valve through dropping pipeline 11, the left interface and the upper interface of cross four-way joint 4 are opened during the adding process, nitrogen in nitrogen storage tank 6 is entered into reaction kettle 1 through nitrogen pipeline 9 to perform positive pressure protection, to ensure that the foam generated in reaction kettle 1 is blown away by nitrogen, until the solvent is added completely, at the same time, the pressure balance between reaction kettle 1 and dropping tank 2 is ensured through balance pipe 3, to avoid the violent precipitation and caking caused by the uneven adding speed, and the temperature is heated to 50-55 DEG C through the heating device, after the crystallization is completed, the heating is stopped, the free operation process is completed, and the free material in reaction kettle 1 is entered into centrifuge 5 through the upper interface, the lower interface and discharge pipeline 12 of cross four-way joint 4.
[0023] In addition to the above embodiments, the utility model also includes other implementation manners, and the technical solutions formed by equivalent transformation or equivalent replacement shall fall within the protection scope of the utility model claims.
Claims
1. A device for liberating a phenethylamine salt compound, characterized by: The free device includes a reaction kettle (1), the reaction kettle (1) is connected with the dropping tank (2) above the reaction kettle (1) through a regulating valve, the reaction kettle (1) is also connected with the dropping tank (2) through a balance pipe (3), the upper interface of the cross four-way joint (4) is connected with the reaction kettle (1), the lower interface of the cross four-way joint (4) is connected with the centrifuge (5), the left interface of the cross four-way joint (4) is connected with the nitrogen storage tank (6), the right interface of the cross four-way joint (4) is connected with the diaphragm pump (7), the diaphragm pump (7) is also connected with the feed inlet of the reaction kettle (1) through a precision filter (8) and a regulating valve in sequence; the four interfaces of the cross four-way joint (4) are all provided with regulating valves.
2. The free device of phenethylamine salt compounds according to claim 1, characterized by: The left interface of the cross four-way joint (4) is connected with the nitrogen storage tank (6) through a nitrogen pipeline (9).
3. The free device of phenethylamine salt compounds according to claim 1, characterized in that: A stirring mechanism (10) and a heating device are arranged in the reaction kettle (1).
4. The free device of phenethylamine salt compounds according to claim 3, characterized in that: The stirring mechanism (10) includes a stirring shaft and a plurality of layers of stirring paddles arranged on the stirring shaft, and the plurality of layers of stirring paddles are wing-shaped axial flow stirring paddles.
5. The free form device of claim 1, wherein: The reaction kettle (1) is connected with the dropping tank (2) above the reaction kettle (1) through a regulating valve and a dropping pipeline (11).
6. The free form device of claim 1, wherein: The lower interface of the cross four-way joint (4) is connected with the centrifuge (5) through a discharging pipeline (12).