DL-p-hydroxyphenylglycine recrystallization device
By using a precision microporous membrane filter and a rubber-plastic insulation layer in the swirling p-hydroxyphenylglycine recrystallization device, combined with a rake-shaped agitator and an airflow control valve, the problems of impurity removal and temperature control were solved, improving product purity and production efficiency while reducing operating costs.
Patent Information
- Application Number
- CN202520200367.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-09
- Publication Date
- 2026-02-03
- Estimated Expiration
- 2035-02-09
AI Technical Summary
In the existing technology, impurities such as ammonium sulfate, o-hydroxyphenylglycine and tiny black spots are often encapsulated or trapped in the synthesis and crystallization of racemic p-hydroxyphenylglycine, which affect the purity and conversion rate.
A recrystallization device for p-hydroxyphenylglycine was designed, which uses a precision microporous membrane filter and is equipped with a rubber and plastic insulation layer. Combined with a double-layer rake-shaped stirring paddle and an airflow control valve, the problems of impurity removal and temperature control are solved.
It effectively removes minute impurities, avoids pipe blockage, improves product purity and production efficiency, reduces operating costs, and is easy to operate.
Smart Images
Figure CN223861349U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model belongs to the chemical production device and purification recrystallization technical field, especially relates to a mixed-rotation p-hydroxyphenylglycine recrystallization device. BACKGROUND
[0002] Mixed-rotation p-hydroxyphenylglycine is abbreviated as HPG, and its appearance is white needle-like crystal, and its molecular weight is 167.16, which is an important medicine synthesis and fine organic intermediate. The left-rotation p-hydroxyphenylglycine obtained by the separation of mixed-rotation p-hydroxyphenylglycine is not only an important synthetic medicine chemical product, but also an indispensable side chain acid in the synthesis of broad-spectrum antibiotics such as amoxicillin, cefadroxil, cefoperazone, ceforamide and cefamandole.
[0003] Due to various reasons of the prior art, a certain amount of ammonium sulfate, o-hydroxyphenylglycine, micro black spots and other impurities are often wrapped or entrained in the synthesis and crystallization process of mixed-rotation p-hydroxyphenylglycine. The existence of these impurities directly affects the conversion rate of mixed-rotation p-hydroxyphenylglycine to left-rotation p-hydroxyphenylglycine, and greatly negatively affects the purity of the left-rotation p-hydroxyphenylglycine crystal. Therefore, it is necessary to design a relatively complete mixed-rotation p-hydroxyphenylglycine recrystallization purification device. SUMMARY
[0004] In order to solve the above problems, the utility model technical scheme discloses a mixed-rotation p-hydroxyphenylglycine recrystallization device, and the main innovation points include 3 aspects, 1 is that a relatively precise microporous membrane filter is arranged in the decoloring and impurity removing process of mixed-rotation p-hydroxyphenylglycine, and an oplastic cotton heat preservation layer is additionally arranged on the outer surface of the microporous membrane filter, 2 is that the stirrer of the crystallization kettle is designed as a double-layer structure, and the stirring paddle of the upper layer is designed as a pin rake-shaped stirring paddle, and 3 is that an airflow control valve is additionally arranged between the crystallization kettle and the discharge valve. The mixed-rotation p-hydroxyphenylglycine recrystallization device disclosed by the utility model technical scheme effectively solves the problem that there are still micro impurity points after the mother liquor is filtered, solves the problem that the pipeline is blocked due to the temperature reduction in the middle of the filtration, solves the problem that the discharge valve at the bottom of the crystallization kettle is easily blocked due to the deposition of the crystal, and solves the problem of the purity of the mixed-rotation p-hydroxyphenylglycine crystal. The utility model also has the characteristics of high production efficiency, high product purity, low operation cost and convenient operation.
[0005] The utility model discloses a kind of mixed-rotation p-hydroxyphenylglycine recrystallization devices, it includes: decoloring and impurity removal kettle, pure water control valve, solid feeding port, acid liquid high tank, acid liquid control valve, mother liquor transfer pump, microporous membrane filter, filter core column, heat preservation layer, crystallization kettle, harrow stirring paddle, lye high tank, lye control valve, airflow control valve, discharge valve, centrifuge, centrifugal feed inlet, elution water control valve, liquid outlet pipe, crystal discharge pipe, characterized in that, the decoloring and impurity removal kettle top is additionally provided with pure water control valve and acid liquid control valve, acid liquid control valve is connected with acid liquid high tank upwards, decoloring and impurity removal kettle bottom is connected with the top of microporous membrane filter by pipeline and mother liquor transfer pump, the microporous membrane filter inside is provided with filter core column, outer wall is wrapped with heat preservation layer, microporous membrane filter bottom is connected with crystallization kettle upper portion by pipeline, the crystallization kettle is provided with lye high tank directly above, is provided with harrow stirring paddle inside, crystallization kettle bottom is equipped with discharge valve, airflow control valve is connected between crystallization kettle bottom and discharge valve, centrifuge is provided with directly below the crystallization kettle, the centrifuge upper portion is provided with centrifugal feed inlet and elution water control valve, centrifugal feed inlet is connected with crystallization kettle bottom by discharge valve, centrifuge is connected with crystal discharge pipe directly below, centrifuge lower portion one side is provided with liquid outlet pipe.
[0006] Preferably, the utility model discloses a kind of mixed-rotation p-hydroxyphenylglycine recrystallization devices, characterized in that, the microporous membrane filter shell is 304 type stainless steel material, is provided with the filter core column of PTFE membrane material inside.This design purpose is to last durable corrosion resistance, can effectively avoid the secondary pollution of mixed-rotation p-hydroxyphenylglycine crystal crystal due to filter.
[0007] Preferably, the utility model discloses a kind of mixed-rotation p-hydroxyphenylglycine recrystallization devices, characterized in that, the filter core column filtering precision is 0.5-10 μm, working pressure 0.1-0.6MPa.This design purpose is to remove maximum mixed-rotation p-hydroxyphenylglycine crude product in various kinds of small impurities, ensure mixed-rotation p-hydroxyphenylglycine crystal purity.
[0008] Preferably, the utility model discloses a kind of mixed-rotation p-hydroxyphenylglycine recrystallization devices, characterized in that, the heat preservation layer wrapped in the outer wall of microporous membrane filter uses the thickness of 60-80mm rubber plastic cotton or glass wool.This design purpose is to effectively avoid the pipe blockage caused by temperature drop in filtration process, it is very favorable to improve production efficiency.
[0009] Preferably, the utility model discloses a kind of mixed rotation p-hydroxyphenyl glycine re-crystallization device, characterized by being provided with 4~8 cylindrical tines of 50mm diameter, 200mm length on the nail rake stirring paddle of the crystallization kettle inside. The purpose of such design is to break the larger crystal lump in re-crystallization process into small, to facilitate discharge from the bottom of crystallization kettle.
[0010] The utility model discloses a kind of mixed rotation p-hydroxyphenyl glycine re-crystallization device, it brings obvious beneficial effect in the following several aspects, 1 using precision microporous membrane filter can effectively remove the possible small black dot, scrap and other mechanical impurities in mixed rotation p-hydroxyphenyl glycine crude product;2 install rubber plastic cotton class heat preservation layer on the outer wall of microporous membrane filter can effectively avoid the problem of pipeline blockage caused by temperature reduction in mother liquor filtration process;3 the nail rake stirring paddle set in crystallization kettle can effectively break the large lump of re-crystallization, and it is beneficial to successful discharge and reduce impurity wrapping entrainment;4 the airflow control valve is set in the bottom of crystallization kettle, which can effectively prevent the deposition of crystals at the discharge valve at the bottom of crystallization kettle, and it is beneficial to safety production and improve production efficiency.5. The utility model also has the characteristics of high production efficiency, high product purity, low operating cost and convenient operation. BRIEF DESCRIPTION OF DRAWINGS
[0011] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the following will briefly introduce the drawings needed to be used in the embodiment or prior art description, and obviously, the drawings in the following description are only some embodiments of the utility model, and those skilled in the art can also obtain other drawings according to these drawings.
[0012] Figure 1 It is the flow and plane structure schematic diagram of the mixed rotation p-hydroxyphenyl glycine re-crystallization device of the utility model technical scheme embodiment.
[0013] Figure 1 In the middle: decolorization and impurity removal kettle 01, pure water control valve 02, solid feeding port 03, acid liquid head tank 04, acid liquid control valve 05, steam inlet 06, drain valve 07, mother liquor transfer pump 08, microporous membrane filter 09, filter core column 91, liquid inlet valve 93, liquid outlet valve 94, heat preservation layer 94, crystallization kettle 10, nail rake stirring paddle 21, alkali head tank 11, alkali control valve 12, airflow control valve 13, discharge valve 22, centrifuge 14, centrifugal feed inlet 15, elution water control valve 16, liquid outlet pipe 17, crystal discharge pipe 18, cooling water inlet 19, cooling water outlet 20. DETAILED DESCRIPTION
[0014] In order to make the purpose, technical scheme and advantage of the utility model more clear, the following will be combined with Figure 1Further description is made to the specific embodiment.
[0015] The re-crystallization device for mixed-rotation p-hydroxyphenylglycine comprises a decoloring and impurity removing kettle 01, a pure water control valve 02, a solid feeding port 03, an acid liquid head tank 04, an acid liquid control valve 05, a steam inlet 06, a drain valve 07, a mother liquor transfer pump 08, a microporous membrane filter 09, a filter core column 91, a liquid inlet valve 93, a liquid outlet valve 94, a heat preservation layer 94, a crystallization kettle 10, a rake stirring paddle 21, an alkali liquid head tank 11, an alkali liquid control valve 12, an airflow control valve 13, a discharge valve 22, a centrifuge 14, a centrifugal feeding port 15, a leaching water control valve 16, a liquid outlet pipe 17, a crystal discharge pipe 18, a cooling water inlet 19, and a cooling water outlet 20.
[0016] The re-crystallization device for mixed-rotation p-hydroxyphenylglycine comprises a decoloring and impurity removing kettle 01, a pure water control valve 02, a solid feeding port 03, an acid liquid head tank 04, an acid liquid control valve 05, a steam inlet 06, a drain valve 07, a mother liquor transfer pump 08, a microporous membrane filter 09, a filter core column 91, a liquid inlet valve 93, a liquid outlet valve 94, a heat preservation layer 94, a crystallization kettle 10, a rake stirring paddle 21, an alkali liquid head tank 11, an alkali liquid control valve 12, an airflow control valve 13, a discharge valve 22, a centrifuge 14, a centrifugal feeding port 15, a leaching water control valve 16, a liquid outlet pipe 17, a crystal discharge pipe 18, a cooling water inlet 19, and a cooling water outlet 20.
[0017] Further, the re-crystallization device for the mixed-rotation p-hydroxyphenylglycine according to the embodiment of the present specific implementation can be described as follows in a simple operation process: first, a certain amount of pure water is added to the decoloring and impurity removing kettle 01, and stirring is started, then the mixed-rotation p-hydroxyphenylglycine crude product and the decoloring and impurity removing auxiliary are put in, then the acid liquid control valve 05 is opened, and the prepared acid liquid is slowly added to the decoloring and impurity removing kettle 01 from the acid liquid high tank 04; next, steam is started to heat and warm up, when the mother liquor is clear and transparent, the mother liquor transfer pump 08 is started, and the hot mixed-rotation p-hydroxyphenylglycine mother liquor is transported to the crystallization kettle 10 through the microporous membrane filter 09, the stirring of the crystallization kettle 01 is started to run at low speed, and the cooling water is slowly cooled; when a large amount of mixed-rotation p-hydroxyphenylglycine crystals are precipitated, the air flow control valve 13 is opened, and the high-speed air pressure flow is bubbled at the bottom of the crystallization kettle 10 to prevent the crystals from depositing; next, the centrifuge 14 is started, the mixed-rotation p-hydroxyphenylglycine crystal mixture is discharged from the bottom of the crystallization kettle 10 through the discharge valve 22 and enters the centrifuge 14 through the centrifugal feed port 15 to separate the solid and liquid, the crystals are washed with pure water through the washing water control valve 16, the centrifugal mother liquor is transferred to the next process through the liquid outlet pipe 17, and the mixed-rotation p-hydroxyphenylglycine crystals are discharged and collected through the crystal discharge pipe 18.
[0018] Further, the re-crystallization device for the mixed-rotation p-hydroxyphenylglycine according to the embodiment of the present specific implementation is characterized in that the microporous membrane filter shell is made of 304 stainless steel, and a filter core column made of PTFE membrane is arranged inside. The purpose of this design is to be durable and corrosion-resistant, and to effectively avoid the secondary pollution of the mixed-rotation p-hydroxyphenylglycine crystals caused by the filter.
[0019] Further, the re-crystallization device for the mixed-rotation p-hydroxyphenylglycine according to the embodiment of the present specific implementation is characterized in that the filter core column has a filtering precision of 0.5-10 μm and a working pressure of 0.1-0.6 MPa. The purpose of this design is to remove various small impurities in the mixed-rotation p-hydroxyphenylglycine crude product to the maximum extent and ensure the purity of the mixed-rotation p-hydroxyphenylglycine crystals.
[0020] Further, the re-crystallization device for the mixed-rotation p-hydroxyphenylglycine according to the embodiment of the present specific implementation is characterized in that the heat preservation layer wrapped around the outer wall of the microporous membrane filter is made of rubber-plastic cotton or glass wool with a thickness of 60-80 mm. The purpose of this design is to effectively avoid the pipeline blockage caused by temperature drop in the filtering process, which is very beneficial to improving the production efficiency.
[0021] Further, the embodiment of the present specific implementation is a mixed-rotation p-hydroxyphenylglycine recrystallization device, characterized in that 4-8 cylindrical tines with a diameter of 50 mm and a length of 200 mm are installed on the harrow stirring paddle in the crystallization kettle. The purpose of this design is to break up large crystal lumps that appear during the recrystallization process into smaller ones, thereby facilitating discharge from the bottom of the crystallization kettle.
[0022] The technical scheme of the mixed-rotation p-hydroxyphenylglycine recrystallization device has the following obvious beneficial effects: 1. The use of a precision microporous membrane filter can effectively remove small black spots, debris and other mechanical impurities that may be present in the mixed-rotation p-hydroxyphenylglycine crude product; 2. The addition of an rubber-plastic cotton insulation layer to the outer wall of the microporous membrane filter can effectively prevent pipeline blockage caused by temperature reduction during mother liquor filtration; 3. The harrow stirring paddle installed in the crystallization kettle can effectively break up large lumps formed during recrystallization, which is beneficial for smooth discharge and reduction of impurity wrapping and entrainment; 4. The airflow control valve installed at the bottom of the crystallization kettle can effectively prevent crystals from depositing at the discharge valve at the bottom of the crystallization kettle, which is beneficial for safe production and improved production efficiency. 5. The present utility model also has the characteristics of high production efficiency, high product purity, low operating cost and convenient operation.
[0023] Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present utility model should be included in the protection scope of the present utility model. The protection scope of the present utility model is the widest scope consistent with the principles and novel features described in the present text.
Claims
1. A recrystallization apparatus for racemic p-hydroxyphenylglycine, comprising: The system comprises a decolorizing and impurity removal kettle, a pure water control valve, a solid feed inlet, an acid high-level tank, an acid control valve, a mother liquor transfer pump, a microporous membrane filter, a filter element column, an insulation layer, a crystallization kettle, a rake stirring paddle, an alkali high-level tank, an alkali control valve, an airflow control valve, a discharge valve, a centrifuge, a centrifuge feed inlet, a rinsing water control valve, a liquid outlet pipe, and a crystal discharge pipe. The decolorizing and impurity removal kettle is characterized by having a pure water control valve and an acid control valve installed above it. The acid control valve is connected upwards to the acid high-level tank. The bottom of the decolorizing and impurity removal kettle is connected to the top of the microporous membrane filter via a pipe and a mother liquor transfer pump. The microporous membrane filter contains a filter element column, and its outer wall is wrapped with an insulation layer. The bottom of the microporous membrane filter is connected to the upper part of the crystallization vessel through a pipe. An alkaline solution high-level tank is set directly above the crystallization vessel, and a rake stirring paddle is installed inside. A discharge valve is installed at the bottom of the crystallization vessel, and an airflow control valve is connected between the bottom of the crystallization vessel and the discharge valve. A centrifuge is set directly below the crystallization vessel. A centrifuge inlet and a rinsing water control valve are set on the upper part of the centrifuge. The centrifuge inlet is connected to the bottom of the crystallization vessel through the discharge valve. A crystal discharge pipe is connected directly below the centrifuge, and a liquid outlet pipe is set on one side of the lower part of the centrifuge.
2. The apparatus for recrystallizing racemic p-hydroxyphenylglycine according to claim 1, characterized in that, The outer shell of the microporous membrane filter is made of 304 stainless steel, and the filter element column is made of PTFE membrane material inside.
3. The apparatus for recrystallizing racemic p-hydroxyphenylglycine according to claim 1, characterized in that, The filter element column has a filtration accuracy of 0.5–10 μm and a working pressure of 0.1–0.6 MPa.
4. The apparatus for recrystallizing racemic p-hydroxyphenylglycine according to claim 1, characterized in that, The insulation layer wrapped around the outer wall of the microporous membrane filter is made of 60-80mm thick rubber-plastic cotton or glass wool.
5. The apparatus for recrystallizing racemic p-hydroxyphenylglycine according to claim 1, characterized in that, The rake-shaped stirring paddle located inside the crystallizer is equipped with 4 to 8 cylindrical rake teeth with a diameter of 50 mm and a length of 200 mm.