L-p-hydroxyphenylglycine centrifugal mother liquor concentration device

By introducing an external reboiler, adding a damper and a vacuum buffer head in the production process of L-hydroxyphenylglycine, the problems of low efficiency and gas-liquid entrainment in the evaporation unit were solved, achieving efficient evaporation and safe production.

CN223760427UActive Publication Date: 2026-01-06HENAN NEWLAND PHARMACEUTICAL CO LTD
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Patent Information

Application Number
CN202520072769.8
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-01-13
Publication Date
2026-01-06
Estimated Expiration
2035-01-13

AI Technical Summary

Technical Problem

In the existing L-hydroxyphenylglycine production process, the evaporation device is inefficient and the COD and ammonia nitrogen content of the distillate water exceeds the standard due to gas-liquid entrainment, and there are also material loss and safety risks.

Method used

An externally heated reboiler and a steam-heated reboiler are introduced into the evaporation unit. A damper is installed on the evaporation pipeline, and a superheated feed tube is inserted under the liquid in the distillation kettle. A vacuum buffer head is installed on the upper part of the distillation water receiving tank.

Benefits of technology

It improves evaporation efficiency, reduces COD and ammonia nitrogen content in the distillate, prevents gas-liquid entrainment and material loss, and ensures safe production.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses an L-p-hydroxyphenylglycine centrifugal mother liquor concentration device, and belongs to the technical field of chemical production equipment and evaporation concentration. The device mainly comprises a distillation kettle, a reboiler, an overheating material pipe, a circulating pump, a damper, a condenser, a distilled water receiving tank, a vacuum buffer head, a vacuum port and the like, according to the L-p-hydroxyphenylglycine centrifugal mother liquor concentration device disclosed by the technical scheme of the utility model, the defects of low efficiency and high COD (Chemical Oxygen Demand) of distilled water of a previous evaporation boiler are effectively overcome, and the problems that gas-liquid entrainment or material flushing and the like are easy to occur in a common distillation mode and are unfavorable for safe production are solved; the L-p-hydroxyphenylglycine centrifugal mother liquor concentration device disclosed by the technical scheme of the utility model also has the characteristics of reasonable layout, easiness in installation, convenience in operation and high evaporation efficiency.
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Description

Technical Field

[0001] This utility model relates to the field of chemical production equipment and evaporation and concentration technology, and specifically to a centrifugal mother liquor concentration device for L-hydroxyphenylglycine. Background Technology

[0002] Dp-hydroxyphenyl glycine (DHPG), with a molecular weight of 167.16, is a white crystalline powder. It is slightly soluble in ethanol and water, readily soluble in acids or alkalis to form salts, has a melting point of 225℃~227℃, a purity of >98.5%, and a specific rotation of -155~-161°. Dp-hydroxyphenyl glycine is not only an important fine chemical product and a crucial pharmaceutical intermediate, but also an indispensable side-chain acid in the synthesis of broad-spectrum antibiotics such as amoxicillin, cefadroxil, cefoperazone, cefuroxime, and cefhydroxylamine.

[0003] The production process of L-hydroxyphenylglycine involves the evaporation and concentration of centrifugal mother liquor. The distillate is then transferred to a biochemical workshop for further treatment, and the concentrated mother liquor is transferred to the next process for deep extraction. Previously, the evaporation unit was inefficient due to equipment limitations, and gas-liquid entrainment during the evaporation process frequently resulted in excessive COD and ammonia nitrogen levels in the distillate. This not only hindered the biochemical treatment of the distillate but also caused material loss and safety risks due to gas-liquid entrainment. Therefore, innovative improvements to the existing centrifugal mother liquor evaporation and concentration unit are essential. Summary of the Invention

[0004] To address the aforementioned problems, this utility model discloses a centrifugal mother liquor concentration device for L-para-hydroxyphenylglycine. Its innovations include: 1) introducing an externally heated reboiler based on conventional evaporation equipment; 2) adding a damper to the evaporation pipeline; 3) inserting the superheated feed tube under the liquid in the distillation kettle; and 4) installing a vacuum buffer head on the upper part of the distilled water receiving tank. This L-para-hydroxyphenylglycine centrifugal mother liquor concentration device effectively solves the shortcomings of previous evaporation kettles, such as low efficiency and high COD in the distilled water, and addresses the problems of gas-liquid entrainment or material overflow that easily occur in ordinary distillation modes, which are detrimental to safe production. Furthermore, this L-para-hydroxyphenylglycine centrifugal mother liquor concentration device features a reasonable layout, easy installation, convenient operation, and high evaporation efficiency.

[0005] The present invention relates to a centrifugal mother liquor concentration device for L-hydroxyphenylglycine, comprising: a distillation kettle, a circulating pump, a reboiler, a superheated feed tube, a damper, an evaporation tube, a condenser, a distilled water receiving tank, a vacuum buffer head, a vacuum port, and a distilled water sampling port. The device is characterized in that the bottom of the distillation kettle is connected to the bottom of the reboiler via a pipe and the circulating pump; the reboiler is connected to the distillation kettle via the superheated feed tube at its upper part; the distillation kettle is connected upwards to the damper via the evaporation tube; the damper is then connected to the condenser via the evaporation tube; the condenser outlet is connected downwards to the distilled water receiving tank; a vacuum buffer head is installed at the top of the distilled water receiving tank; and the vacuum buffer head is connected upwards to the vacuum port.

[0006] Preferably, the L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this utility model is characterized in that the reboiler is made of 904 stainless steel or titanium alloy, and is equipped with a steam coil with a heat exchange area of ​​80-120 m². This design aims to increase the heat exchange area during the distillation process; the coordinated evaporation of the distillation vessel and reboiler will increase the evaporation efficiency by 2-3 times.

[0007] Preferably, the L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this utility model is characterized in that the superheated feed tube is made of glass-lined, 904 stainless steel, PTFE-lined, or titanium alloy material, with a diameter of 125-150 mm, and a sight glass for observing the flow state of the feed liquid is provided on the superheated feed tube.

[0008] Preferably, the L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this utility model is characterized in that the superheated feed tube is inserted to 2 / 3 of the depth of the distillation vessel, and the outlet of the superheated feed tube has a bevel of 15-45°. This design aims to ensure that the superheated feed tube remains continuously submerged during evaporation, preventing splashing of the superheated liquid and effectively preventing the splashed liquid from escaping due to negative pressure or gas-liquid entrainment.

[0009] Preferably, the centrifugal mother liquor concentration device for L-hydroxyphenylglycine described in this utility model is characterized in that the damper has conical ends and a cylindrical middle section, the diameter of which is 2-4 times the diameter of the evaporation tube. The purpose of adding the damper is to effectively prevent gas-liquid entrainment caused by high-speed evaporation and negative pressure flow, thus ensuring the quality of the distilled water and preventing material loss.

[0010] Preferably, the L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this utility model is characterized in that the damper is internally equipped with a 304 stainless steel wire mesh or titanium wire mesh, and the mass transfer area of ​​the wire mesh is 400-600 m². 2The purpose of this design is to intercept some of the material that may be entrained in the airflow passing through the damper, ensuring that no material is entrained in the airflow, which is beneficial to the quality of the distilled water and the control of material loss.

[0011] Preferably, the L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this utility model is characterized in that the condenser is a shell-and-tube type, a spiral plate type, or a graphite condenser, with a heat exchange area of ​​100-150 m². 2 .

[0012] The L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this utility model has four significant beneficial effects: 1. The addition of an external reboiler can increase the evaporation efficiency by 2-3 times, which is very beneficial to production organization and cost reduction; 2. The insertion of the superheated feed tube into the liquid can effectively prevent material splashing, thereby preventing the splashed liquid from escaping due to negative pressure or gas-liquid entrainment; 3. The addition of a damper on the evaporation tube can effectively prevent gas-liquid entrainment caused by high-speed evaporation and negative pressure, thereby ensuring the quality of the distilled water and preventing material loss; 4. The addition of a vacuum buffer head on the upper part of the distilled water receiving tank can effectively prevent some of the splashed distilled water from being drawn into the vacuum pump system under high vacuum.

[0013] The L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this utility model also has the advantages of reasonable layout, easy installation, and convenient operation. Attached Figure Description

[0014] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings.

[0015] Figure 1 This is a schematic diagram of the structure of a centrifugal mother liquor concentration device for levorotatory p-hydroxyphenylglycine as described in the embodiment of the present invention.

[0016] Figure 1 In the middle: Distillation kettle 01, Distillation kettle steam inlet 02, Distillation kettle steam trap 03, Circulation pump 04, Reboiler 05, Reboiler steam inlet 06, Distillation coil 07, Reboiler steam trap 08, Superheated feed tube 09, Pipe sight glass 10, Damper 11, Evaporator tube 12, Condenser 13, Cooling water inlet 14, Cooling water outlet 15, Distilled water receiving tank 16, Vacuum buffer head 17, Vacuum port 18, Distilled water sampling port 19, Distilled water outlet 20. Detailed Implementation

[0017] To make the objectives, technical solutions, and advantages of this utility model clearer, the following description is provided in conjunction with... Figure 1 The specific embodiments of this implementation will be further described.

[0018] The L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this specific embodiment includes: a distillation kettle 01, a distillation kettle steam inlet 02, a distillation kettle steam trap 03, a circulating pump 04, a reboiler 05, a reboiler steam inlet 06, a distillation coil 07, a reboiler steam trap 08, a superheated feed tube 09, a pipe sight glass 10, a damper 11, an evaporator tube 12, a condenser 13, a cooling water inlet 14, a cooling water outlet 15, a distilled water receiving tank 16, a vacuum buffer head 17, a vacuum port 18, a distilled water sampling port 19, and a distilled water outlet 20.

[0019] Furthermore, in the embodiment of this specific implementation, the centrifugal mother liquor concentration device for L-hydroxyphenylglycine is characterized in that the bottom of the distillation kettle 01 is connected to the bottom of the reboiler 05 via a pipe and a circulating pump 04. The reboiler 05 is connected to the distillation kettle 01 via a superheated feed pipe 09 at its upper part. The distillation kettle 01 is connected upward to the damper 11 via an evaporation pipe 12. The damper 11 is then connected to the condenser 13 via an evaporation pipe. The outlet of the condenser 13 is connected downward to the distilled water receiving tank 16. A vacuum buffer head 17 is provided on the top of the distilled water receiving tank 16. The vacuum buffer head 17 is connected upward to the vacuum port 18.

[0020] Furthermore, the L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this specific embodiment is characterized in that the reboiler is made of 904 stainless steel or titanium alloy, and is equipped with a steam coil with a heat exchange area of ​​80-120 m². This design aims to increase the heat exchange area during the distillation process; the coordinated evaporation of the distillation vessel and reboiler will increase the evaporation efficiency by 2-3 times.

[0021] Furthermore, the L-para-hydroxyphenylglycine centrifugal mother liquor concentration device described in this specific embodiment is characterized in that the superheated feed tube is made of glass-lined, 904 stainless steel, PTFE-lined, or titanium alloy material, with a diameter of 125-150 mm, and a sight glass for observing the flow state of the feed liquid is provided on the superheated feed tube.

[0022] Furthermore, in the specific embodiment of this invention, the centrifugal mother liquor concentration device for L-para-hydroxyphenylglycine is characterized in that the superheated feed tube is inserted to 2 / 3 of the depth of the distillation vessel, and the outlet of the superheated feed tube has a bevel of 15-45°. This design aims to ensure that the superheated feed tube remains continuously submerged during evaporation, preventing splashing of the superheated liquid and effectively preventing the splashed liquid from escaping due to negative pressure or gas-liquid entrainment.

[0023] Furthermore, in this specific embodiment, the centrifugal mother liquor concentration device for L-hydroxyphenylglycine is characterized in that the damper has conical ends and a cylindrical middle section, the diameter of which is 2-4 times the diameter of the evaporation tube. The purpose of adding the damper is to effectively prevent gas-liquid entrainment caused by high-speed evaporation and negative pressure flow, thus ensuring the quality of the distilled water and preventing material loss.

[0024] Furthermore, the L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this specific embodiment is characterized in that the damper is internally equipped with a 304 stainless steel wire mesh or titanium wire mesh, and the mass transfer area of ​​the wire mesh is 400-600 m². 2 The purpose of this design is to intercept some of the material that may be entrained in the airflow passing through the damper, ensuring that no material is entrained in the airflow, which is beneficial to the quality of the distilled water and the control of material loss.

[0025] Furthermore, the L-hydroxyphenylglycine centrifugal mother liquor concentration device described in this specific embodiment is characterized in that the condenser is a shell-and-tube type, a spiral plate type, or a graphite condenser, with a heat exchange area of ​​100-150 m². 2 .

[0026] This device, a centrifugal mother liquor concentration device for L-hydroxyphenylglycine described in this utility model, has four significant beneficial effects: 1. Adding an external reboiler can increase evaporation efficiency by 2-3 times, which is very beneficial for production organization and cost reduction; 2. Inserting the superheated feed tube into the liquid can effectively prevent material splashing, thereby preventing the splashed liquid from escaping due to negative pressure or gas-liquid entrainment; 3. Adding a damper to the evaporation tube can effectively prevent gas-liquid entrainment caused by high-speed evaporation and negative pressure, thereby ensuring the quality of the distilled water and preventing material loss; 4. Adding a vacuum buffer head to the upper part of the distilled water receiving tank can effectively prevent some of the splashed distilled water from being drawn into the vacuum pump system under high vacuum.

[0027] This device, a centrifugal mother liquor concentration device for L-hydroxyphenylglycine described in this utility model, also has the advantages of reasonable layout, easy installation, and convenient operation. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of this utility model should be included within the protection scope of this utility model. The protection scope of this utility model is to conform to the widest range consistent with the principles and novel features described herein.

Claims

1. A device for concentrating a centrifugate of levorotatory p-hydroxyphenylglycine, comprising: The distillation kettle, circulating pump, reboiler, superheated material pipe, damper, evaporation pipe, condenser, distilled water receiving tank, vacuum buffer head, vacuum port and distilled water sampling port are characterized in that the bottom of the distillation kettle is connected with the bottom of the reboiler through a pipeline and a circulating pump, the reboiler is connected with the distillation kettle through a superheated material pipe at the upper portion of the reboiler, the distillation kettle is connected with the damper through an evaporation pipe upward, the damper is connected with the condenser through an evaporation pipe, the outlet of the condenser is connected with the distilled water receiving tank downward, the top of the distilled water receiving tank is provided with the vacuum buffer head, and the vacuum buffer head is connected with the vacuum port upward.

2. The device for concentrating the centrifugal mother liquor of levorotatory p-hydroxyphenylglycine according to claim 1, characterized in that, The reboiler is made of 904 stainless steel, and is internally provided with a steam coil pipe. The heat exchange area of the steam coil pipe is 80-120m 2 .

3. The device for concentrating the centrifugal mother liquor of levorotatory p-hydroxyphenylglycine according to claim 1, characterized in that, The superheated material pipe is made of glass lining, 904 stainless steel, tetrafluoroethylene lining or titanium alloy, has a diameter of 125-150 mm, and is provided with a pipeline sight glass.

4. The device for concentrating the centrifugal mother liquor of levorotatory p-hydroxyphenylglycine according to claim 1, characterized in that, The superheated material pipe is inserted into the distillation kettle to a depth of 2 / 3 of the distillation kettle, and the outlet of the superheated material pipe is provided with a bevel of 15-45°.

5. The device for concentrating the centrifugal mother liquor of levopropoxyphen glycin according to claim 1, characterized in that, The damper has a conical shape at both ends and a cylindrical body in the middle, and the diameter of the cylindrical body of the damper is 2-4 times the diameter of the evaporation pipe.

6. The device for concentrating the centrifugal mother liquor of levovisual hydroxyphenylglycine according to claim 1, characterized in that, The damper is internally equipped with 304 stainless steel wire mesh or titanium wire mesh, and the mass transfer area of the wire mesh is 400-600 m 2 .

7. The device for concentrating the centrifugal mother liquor of levopropoxyphen glycin according to claim 1, characterized in that, The condenser is shell-and-tube or spiral-plate or graphite condenser, heat exchange area 100-150m 2 .