Device for recovering p-hydroxyphenylglycine from centrifugal mother liquor

By using a mud pump and jet nozzle combined with baffles in the mother liquor sedimentation tank, effective separation of p-hydroxyphenylglycine and ammonium sulfate was achieved, solving the problems of low separation efficiency and safety risks in the existing technology, and realizing an efficient and safe recovery process.

CN223970140UActive Publication Date: 2026-03-06HENAN NEWLAND PHARMACEUTICAL CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-02-09
Publication Date
2026-03-06

AI Technical Summary

Technical Problem

In the centrifuged mother liquor of p-hydroxyphenylglycine, ammonium sulfate and p-hydroxyphenylglycine are difficult to separate, resulting in quality degradation and economic waste. Existing stirring methods are inefficient and pose safety risks.

Method used

A mud pump is used to drive high and low staggered jet nozzles to promote material rotation in the mother liquor sedimentation tank. Combined with the baffle plate design, uniform mixing of the mixture is achieved. Then, p-hydroxyphenylglycine crystals are separated and recovered by centrifuge.

Benefits of technology

It improves the recovery purity and efficiency of p-hydroxyphenylglycine, reduces safety risks, and is simple to operate with low investment, making it highly efficient and convenient.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses a device for recovering p-hydroxyphenylglycine from centrifugal mother liquor, and belongs to the technical field of chemical production devices and mother liquor recovery. The device is formed by combining a mother liquor deposition tank, a slurry pump, an upper rotary control valve, a lower rotary control valve, a baffle plate, a jet flow nozzle, a centrifugal machine and the like, the innovation point of the technical scheme of the utility model is as follows: by utilizing the power generated by the slurry pump, materials in the mother liquor deposition tank are pushed to rotate and turn over by mother liquor sprayed by the high-low staggered jet nozzles, so that deposited p-hydroxyphenylglycine crystals float upwards; then feeding the para-hydroxyphenylglycine centrifugal mother liquor with suspended crystals into a centrifugal machine by virtue of a slurry pump for centrifugal separation, so as to achieve the purpose of efficiently recovering the para-hydroxyphenylglycine crystals; according to the technical scheme, the problem that crystals are not easy to turn up after standing and depositing is solved, and the problem that mechanical stirring is not easy to add due to large span of a mother liquor depositing tank is solved; the device also has the characteristics of convenience in operation, simplicity and high efficiency.
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Description

Technical Field

[0001] This utility model belongs to the field of chemical production equipment and mother liquor recovery technology, and specifically relates to an apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor. Background Technology

[0002] p-Hydroxyphenylglycine, abbreviated as HPG, is a white needle-like crystal with a molecular weight of 167.16. It is an important pharmaceutical synthesis and fine organic intermediate. The levorotatory p-hydroxyphenylglycine obtained from its separation is not only an important synthetic pharmaceutical chemical product, but also an indispensable side chain acid in the synthesis of broad-spectrum antibiotics such as amoxicillin, cefadroxil, cefoperazone, cefuroxime, and cefhydroxylamine.

[0003] The initial centrifugation mother liquor in the synthesis process of p-hydroxyphenylglycine racem contains approximately 4.5–5.0% p-hydroxyphenylglycine and 20–25% ammonium sulfate. During the previous processing of these mother liquors, it is easy to mix ammonium sulfate with p-hydroxyphenylglycine and extract them together. The high-value p-hydroxyphenylglycine is difficult to separate from the inexpensive ammonium sulfate solid material, which not only affects the quality of p-hydroxyphenylglycine but also has a significant negative impact on the purity of ammonium sulfate, resulting in considerable economic waste.

[0004] The key to treating the p-hydroxyphenylglycine centrifugal mother liquor is preventing excessive deposition and precipitation of ammonium sulfate and p-hydroxyphenylglycine, which would result in them becoming highly bound together. Therefore, the p-hydroxyphenylglycine centrifugal mother liquor in the sedimentation tank needs continuous agitation to suspend the precipitated p-hydroxyphenylglycine crystals and allow the ammonium sulfate to settle. However, due to the large span of the sedimentation tank, installing mechanical agitators poses significant safety risks. Furthermore, the strong agitation force of mechanical agitation often causes the precipitated ammonium sulfate crystals to float in the mother liquor, which is detrimental to the purity of the recovered p-hydroxyphenylglycine. On the other hand, bubbling and manual stirring methods do not achieve satisfactory results. Summary of the Invention

[0005] To address the aforementioned problems, this invention discloses a device for recovering p-hydroxyphenylglycine from centrifugal mother liquor. Its main innovation lies in utilizing the power generated by a mud pump to propel the material in the mother liquor sedimentation tank through a staggered jet nozzle, causing the deposited p-hydroxyphenylglycine crystals to float to the surface. The mud pump then pumps the mother liquor containing the suspended p-hydroxyphenylglycine crystals into a centrifuge for centrifugal separation, thereby achieving efficient recovery of the p-hydroxyphenylglycine crystals. This invention solves the problem of crystals being difficult to agitate after static sedimentation and the difficulty of installing mechanical agitators in large-span mother liquor sedimentation tanks. Furthermore, this invention features low investment, convenient operation, and high efficiency.

[0006] This utility model discloses an apparatus for recovering p-hydroxyphenylglycine from centrifugal mother liquor. It comprises: a mother liquor sedimentation tank, a mud pump, a centrifugal control valve, an upward swirl control valve, an upward swirl pipe, jet nozzle A, jet nozzle B, a downward swirl control valve, a downward swirl pipe, a baffle plate, jet nozzle C, jet nozzle D, a centrifuge, a centrifugal feed pipe, a rinsing control valve, a liquid outlet pipe, a discharge pipe, a receiving hopper, a waste liquid tank, and a waste liquid transfer pump. The mother liquor sedimentation tank has two openings at its top; one opening houses the upward swirl pipe, and the other opening houses the downward swirl pipe. A mud pump is located in the middle of the outer side of the mother liquor sedimentation tank. The slurry pump is connected to the centrifuge via a pipeline and a centrifugal control valve. The mud pump is connected to the upper swirl pipe via a pipeline and an upper swirl control valve. The mud pump is connected to the lower swirl pipe via a pipeline and a lower swirl control valve. The upper swirl pipe has an upper swirl control valve. The lower swirl pipe has a lower swirl control valve. The lower swirl pipe has a baffle plate in the middle. The lower swirl pipe has a lower swirl nozzle C and a lower swirl nozzle D. The centrifuge has a receiving hopper at the bottom. The centrifuge is connected to a waste liquid tank at the bottom via a liquid outlet pipe. A waste liquid transfer pump is installed on the outer side of the lower part of the waste liquid tank.

[0007] Preferably, the apparatus for recovering p-hydroxyphenylglycine from centrifugal mother liquor according to the present invention is characterized in that the mother liquor sedimentation tank has a depth of 450-500 cm and a diameter of 350-400 cm, and the mud pump is installed in the middle of the outer side of the mother liquor sedimentation tank, 200-250 cm above the bottom of the mother liquor sedimentation tank. The purpose of installing the mud pump in the middle of the outer side of the mother liquor sedimentation tank is to prevent inorganic impurities such as ammonium sulfate deposited at the bottom from being pumped up during operation, which is beneficial for the purity recovery and cost control of p-hydroxyphenylglycine.

[0008] Preferably, the apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor according to the present invention is characterized in that the mud pump is an acid-resistant pump made of plastic-lined or stainless steel, and the flow rate of the mud pump is 8-10 m³ / s. 3 The head of the mud pump is 20-32m. The purpose of designing a larger flow rate mud pump is to generate a larger impact force and drive the mixture to rotate when jet nozzles A, B, C and D are running simultaneously.

[0009] Preferably, the apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor according to the present invention is characterized in that the upper spiral tube is inserted into the mother liquor sedimentation tank to a depth of 150 cm, and the lower spiral tube is inserted into the mother liquor sedimentation tank to a depth of 250 cm. This design aims to ensure that the mixed liquid at a depth of 250 cm or more is rotated under the drive of the mud pump.

[0010] Preferably, the apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor according to the present invention is characterized in that the jet nozzle A is disposed along the inner wall of the mother liquor sedimentation tank at a depth of 100cm in the upper swirl tube, and the jet nozzle B is disposed along the inner wall of the mother liquor sedimentation tank at a depth of 150cm in the upper swirl tube. The diameter of the jet nozzle A is 0.5-1.0cm, and the diameter of the jet nozzle B is 0.5-1.0cm.

[0011] Preferably, the apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor according to the present invention is characterized in that the jet nozzle C is disposed along the inner wall of the mother liquor sedimentation tank at a depth of 200 cm in the lower swirling tube, and the jet nozzle D is disposed along the inner wall of the mother liquor sedimentation tank at a depth of 250 cm in the lower swirling tube. The diameter of the jet nozzle C is 0.5-1.0 cm, and the diameter of the jet nozzle D is 0.5-1.0 cm.

[0012] Preferably, the apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor according to the present invention is characterized in that the baffle plate is disposed at a depth of 60-160 cm in the lower swirling tube, and the wide surface of the baffle plate is perpendicular to the inner wall of the mother liquor sedimentation tank. The purpose of setting the baffle plate is to avoid unidirectional swirling flow when the mixed liquid rotates. The function of the baffle plate is to generate a certain resistance when the mixed liquid rotates, thereby promoting the mixing of materials.

[0013] Preferably, the device for recovering p-hydroxyphenylglycine from centrifuged mother liquor according to the present invention is characterized in that the baffle plate is made of rigid PP or stainless steel, with a width of 10-15cm and a height of 80-100cm.

[0014] The device for recovering p-hydroxyphenylglycine from centrifuged mother liquor, as described in this utility model, has the following significant advantages: 1. Using a mud pump to drive the rotation of the mixture in the mother liquor sedimentation tank is safer and more efficient than mechanical stirring; 2. The introduction of baffles effectively promotes the formation of baffles in the rotating mixture in the mother liquor sedimentation tank, which is beneficial to improving the mixing effect; 3. The staggered nozzle design effectively promotes the rotation of the entire mixture in the upper part of the mother liquor sedimentation tank, which is beneficial to achieving uniform mixing; 4. This utility model also features low investment, convenient operation, and simple and efficient operation. Attached Figure Description

[0015] 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.

[0016] Figure 1 This is a schematic diagram of the planar structure and process flow of an apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor, as described in an embodiment of the present invention.

[0017] Figure 1 In the middle: Mother liquor sedimentation tank 01, mud pump 02, centrifugal control valve 03, upward swirl control valve 04, upward swirl pipe 05, jet nozzle A51, jet nozzle B52, downward swirl control valve 06, downward swirl pipe 07, baffle plate 08, jet nozzle C09, jet nozzle D10, centrifuge 11, centrifugal feed pipe 12, rinsing control valve 13, liquid outlet pipe 14, discharge pipe 15, receiving hopper 16, waste liquid tank 17, waste liquid transfer pump 18. Detailed Implementation

[0018] 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.

[0019] The apparatus for recovering p-hydroxyphenylglycine from centrifugal mother liquor as described in this specific embodiment includes: a mother liquor sedimentation tank 01, a mud pump 02, a centrifugal control valve 03, an upward swirl control valve 04, an upward swirl pipe 05, a jet nozzle A51, a jet nozzle B52, a downward swirl control valve 06, a downward swirl pipe 07, a baffle plate 08, a jet nozzle C09, a jet nozzle D10, a centrifuge 11, a centrifugal feed pipe 12, a rinsing control valve 13, a liquid outlet pipe 14, a discharge pipe 15, a receiving hopper 16, a waste liquid tank 17, and a waste liquid transfer pump 18.

[0020] The apparatus for recovering p-hydroxyphenylglycine from centrifugal mother liquor as described in this specific embodiment is characterized in that the top of the mother liquor sedimentation tank 01 is provided with two openings, one opening is provided with an upper vortex tube 05, and the other opening is provided with a lower vortex tube 07. A mud pump 02 is provided in the middle of the outer side of the mother liquor sedimentation tank 01. The mud pump 02 is connected to the centrifuge 11 through a pipe and a centrifugal control valve 03. The mud pump 02 is connected to the upper vortex tube 05 through a pipe and an upper vortex control valve 04, and the mud pump 02 is connected to the lower vortex tube 07 through a pipe and a lower vortex control valve 06. 7. An upper swirl control valve 04 is installed at the upper position of the upper swirl tube 05. A jet nozzle A51 and a jet nozzle B52 are installed at the lower position of the upper swirl tube 05. A lower swirl control valve 06 is installed at the upper position of the lower swirl tube 07. A baffle plate 08 is installed in the middle of the lower swirl tube 07. A jet nozzle C09 and a jet nozzle D10 are installed at the lower position of the lower swirl tube 07. A receiving hopper 16 is installed at the lower part of the centrifuge 11. The lower part of the centrifuge 11 is connected to a waste liquid tank 17 through a liquid outlet pipe 14. A waste liquid transfer pump 18 is installed on the outer side of the lower part of the waste liquid tank 17.

[0021] Furthermore, the apparatus for recovering p-hydroxyphenylglycine from centrifugal mother liquor described in this specific embodiment is characterized in that the mother liquor sedimentation tank has a depth of 450-500 cm and a diameter of 350-400 cm, and the mud pump is installed in the middle of the outer side of the mother liquor sedimentation tank, 200-250 cm above the bottom of the mother liquor sedimentation tank. The purpose of installing the mud pump in the middle of the outer side of the mother liquor sedimentation tank is to avoid pumping up inorganic impurities such as ammonium sulfate deposited at the bottom when the mud pump is running, which is more beneficial for the purity recovery of p-hydroxyphenylglycine and the control of recovery costs.

[0022] Furthermore, the device for recovering p-hydroxyphenylglycine from centrifugal mother liquor described in this specific embodiment can be simply described as follows: First, close the centrifugal control valve 03, open the upper swirl control valve 04 and the lower swirl control valve 06, start the mud pump 02, and then adjust the opening of the upper swirl control valve 04 and the lower swirl control valve 06 to achieve equilibrium. At this time, the mixture in the mother liquor sedimentation tank 01 will start to rotate. Due to the resistance force generated by the baffle plate 08 on the rotating mixture, the rotating mixture will form a baffle, so that the mixture can achieve uniform mixing within 1 hour. After 1 hour, close the upper swirl control valve 04 and the lower swirl control valve 06, open the centrifugal control valve 03, and transfer the p-hydroxyphenylglycine mixture in the mother liquor sedimentation tank 01 to the centrifuge 11 for solid-liquid separation. The crude p-hydroxyphenylglycine is obtained from the receiving hopper 16, and the centrifugal mother liquor flows into the waste liquid tank 17 through the outlet pipe 14, and is then transported to the next process for harmless treatment by the waste liquid transfer pump 18.

[0023] Furthermore, the apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor described in this specific embodiment is characterized in that the mud pump is an acid-resistant pump made of plastic-lined or stainless steel, and the flow rate of the mud pump is 8-10 m³ / h. 3 The head of the mud pump is 20-32m. The purpose of designing a larger flow rate mud pump is to generate a larger impact force and drive the mixture to rotate when jet nozzles A, B, C and D are running simultaneously.

[0024] Furthermore, in this specific embodiment, the apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor is characterized in that the upper spiral tube is inserted into the mother liquor sedimentation tank to a depth of 150 cm, and the lower spiral tube is inserted into the mother liquor sedimentation tank to a depth of 250 cm. This design aims to ensure that the mixed liquid at a depth of 250 cm or more is rotated under the impingement of the mud pump.

[0025] Furthermore, in the specific embodiment of the apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor, the jet nozzle A is positioned along the inner wall of the mother liquor sedimentation tank at a depth of 100 cm in the upper swirl tube, and the jet nozzle B is positioned along the inner wall of the mother liquor sedimentation tank at a depth of 150 cm in the upper swirl tube. The diameter of the jet nozzle A is 0.5–1.0 cm, and the diameter of the jet nozzle B is 0.5–1.0 cm.

[0026] Furthermore, in the specific embodiment of the apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor, the jet nozzle C is positioned along the inner wall of the mother liquor sedimentation tank at a depth of 200 cm in the lower swirling tube, and the jet nozzle D is positioned along the inner wall of the mother liquor sedimentation tank at a depth of 250 cm in the lower swirling tube. The diameter of the jet nozzle C is 0.5–1.0 cm, and the diameter of the jet nozzle D is 0.5–1.0 cm.

[0027] Furthermore, in the specific embodiment of this apparatus for recovering p-hydroxyphenylglycine from centrifuged mother liquor, the baffle plate is characterized in that it is positioned at a depth of 60-160 cm in the lower swirling tube, and the wide surface of the baffle plate is perpendicular to the inner wall of the mother liquor sedimentation tank. The purpose of setting the baffle plate is to avoid unidirectional swirling flow when the mixture rotates. The function of the baffle plate is to generate a certain resistance when the mixture rotates, thereby promoting the mixing of materials.

[0028] Furthermore, the device for recovering p-hydroxyphenylglycine from centrifuged mother liquor as described in this specific embodiment is characterized in that the baffle plate is made of rigid PP or stainless steel, with a width of 10-15cm and a height of 80-100cm.

[0029] The device for recovering p-hydroxyphenylglycine from centrifuged mother liquor, as described in this utility model, has the following significant advantages: 1. Using a mud pump to drive the rotation of the mixture in the mother liquor sedimentation tank is safer and more efficient than mechanical stirring; 2. The introduction of baffles effectively promotes the formation of baffles in the rotating mixture in the mother liquor sedimentation tank, which is beneficial to improving the mixing effect; 3. The staggered nozzle design effectively promotes the rotation of the entire mixture in the upper part of the mother liquor sedimentation tank, which is beneficial to achieving uniform mixing; 4. This utility model also features low investment, convenient operation, and simple and efficient operation.

[0030] Any modifications, equivalent substitutions, or improvements made within the spirit and principles of this utility model shall be included within the protection scope of this utility model. The protection scope of this utility model shall conform to the widest range consistent with the principles and novel features described herein.

Claims

1. An apparatus for recovering p-hydroxyphenylglycine from a centrifuged mother liquor, comprising: The mother liquor deposition tank, slurry pump, centrifugal control valve, up-spin control valve, up-spin pipe, jet nozzle A, jet nozzle B, down-spin control valve, down-spin pipe, baffle, jet nozzle C, jet nozzle D, centrifuge, centrifuge feed pipe, elution control valve, liquid outlet pipe, discharge pipe, receiving hopper, waste liquid tank, waste liquid transfer pump are characterized in that the top of the mother liquor deposition tank is provided with two openings, one side opening is provided with an up-spin pipe, and the other side opening is provided with a down-spin pipe, a slurry pump is arranged on the middle part of the outer side of the mother liquor deposition tank, the slurry pump is connected with the centrifuge through a pipeline and a centrifugal control valve, the slurry pump is connected with the up-spin pipe through a pipeline and an up-spin control valve, the slurry pump is connected with the down-spin pipe through a pipeline and a down-spin control valve, the up-spin control valve is arranged at the upper position of the up-spin pipe, the jet nozzle A and the jet nozzle B are respectively arranged at the lower position of the up-spin pipe, the down-spin control valve is arranged at the upper position of the down-spin pipe, the baffle is arranged in the middle part of the down-spin pipe, the jet nozzle C and the jet nozzle D are respectively arranged at the lower position of the down-spin pipe, the receiving hopper is arranged at the lower part of the centrifuge, the centrifuge is connected with the waste liquid tank through a liquid outlet pipe, and the waste liquid transfer pump is arranged at the lower part of the outer side of the waste liquid tank.

2. An apparatus for recovering p-hydroxyphenylglycine from a centrifuged mother liquor according to claim 1, characterized in that The depth of the mother liquor deposition tank is 450-500 cm, the diameter is 350-400 cm, and the slurry pump is arranged at the middle part of the outer side of the mother liquor deposition tank and is higher than the bottom of the mother liquor deposition tank by 200-250 cm.

3. An apparatus for recovering p-hydroxyphenylglycine from a centrifuged mother liquor according to claim 1, characterized in that, The mud pump is acid-proof pump made of plastic or stainless steel, and the flow of the mud pump is 8-10 m 3 / h, and the head of the mud pump is 20-32 m.

4. An apparatus for recovering p-hydroxyphenylglycine from a centrifuged mother liquor according to claim 1, characterized in that, The up-spin pipe is inserted into the mother liquor deposition tank by a depth of 150 cm, and the down-spin pipe is inserted into the mother liquor deposition tank by a depth of 250 cm.

5. An apparatus for recovering p-hydroxyphenylglycine from a centrifuged mother liquor according to claim 1, characterized in that, The jet nozzle A is arranged at a position with a depth of 100 cm of the up-spin pipe along the inner wall of the mother liquor deposition tank, the jet nozzle B is arranged at a position with a depth of 150 cm of the up-spin pipe along the inner wall of the mother liquor deposition tank, the diameter of the jet nozzle A is 0.5-1.0 cm, and the diameter of the jet nozzle B is 0.5-1.0 cm.

6. An apparatus for recovering p-hydroxyphenylglycine from a centrifuged mother liquor according to claim 1, characterized in that, The jet nozzle C is arranged at a position with a depth of 200 cm of the down-spin pipe along the inner wall of the mother liquor deposition tank, the jet nozzle D is arranged at a position with a depth of 250 cm of the down-spin pipe along the inner wall of the mother liquor deposition tank, the diameter of the jet nozzle C is 0.5-1.0 cm, and the diameter of the jet nozzle D is 0.5-1.0 cm.

7. An apparatus for recovering p-hydroxyphenylglycine from a centrifuged mother liquor according to claim 1, characterized in that, The baffle is arranged at a position with a depth of 60-160 cm of the down-spin pipe, and the wide surface of the baffle is perpendicular to the inner wall of the mother liquor deposition tank.

8. An apparatus for recovering p-hydroxyphenylglycine from a centrifuged mother liquor according to claim 1, characterized in that, The baffle is made of hard PP or stainless steel, has a width of 10-15 cm, and has a height of 80-100 cm.