CN115054983A - A concentrated filtration equipment for preparing intermediate - Google Patents
A concentrated filtration equipment for preparing intermediate Download PDFInfo
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- CN115054983A CN115054983A CN202210871702.1A CN202210871702A CN115054983A CN 115054983 A CN115054983 A CN 115054983A CN 202210871702 A CN202210871702 A CN 202210871702A CN 115054983 A CN115054983 A CN 115054983A
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- 238000001914 filtration Methods 0.000 title claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 101
- 238000010438 heat treatment Methods 0.000 claims abstract description 53
- 239000012528 membrane Substances 0.000 claims abstract description 44
- 238000011084 recovery Methods 0.000 claims abstract description 26
- 238000001704 evaporation Methods 0.000 claims abstract description 25
- 230000008020 evaporation Effects 0.000 claims abstract description 24
- 239000007921 spray Substances 0.000 claims description 28
- 239000011550 stock solution Substances 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 10
- 239000012450 pharmaceutical intermediate Substances 0.000 claims description 9
- 239000000543 intermediate Substances 0.000 claims description 7
- 239000000835 fiber Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 230000008719 thickening Effects 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000005507 spraying Methods 0.000 abstract description 2
- 239000002918 waste heat Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 15
- 230000007246 mechanism Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
- B01D35/18—Heating or cooling the filters
- B01D35/185—Heating or cooling the filters comprising a vaporizing unit
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0064—Feeding of liquid into an evaporator
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0082—Regulation; Control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/26—Multiple-effect evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
- B01D3/065—Multiple-effect flash distillation (more than two traps)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a concentration and filtration device for preparing a medical intermediate. Comprises a control device, a primary filter, a primary concentration device, a secondary concentration device, a multi-stage membrane filter, a liquid collection tank and a plurality of connecting pipelines which are arranged in sequence. The primary filter raw liquid entering the primary concentration device is a high-pressure air pressure mixture through the pressurization device arranged between the primary filter and the primary concentration device, the primary concentration device is internally provided with a concentration tank opposite to a spraying port of the high-pressure air pressure mixture, and the heating blocks on two sides of the concentration tank are preheated, so that the water evaporation speed is increased and the filtering speed is finely controlled; through set up recovery valve subassembly and heat transfer system between primary concentration device and secondary concentration device, carry the waste heat energy that produces in the primary concentration device to the secondary concentration device in through the heat exchanger, realize secondary concentration device's constant temperature and filter.
Description
Technical Field
The invention relates to the technical field of medical processing tools, in particular to a concentrating and filtering device for preparing a medical intermediate.
Background
At present, the existing medicine concentration and filtration equipment generally adopts a concentration reaction tank, and concentration is performed by heating the concentration reaction tank and continuously stirring, for example, the disclosure numbers are: "CN 215781560U" discloses a concentrated filter equipment of medicine intermediate crude, including concentrated mechanism, install at the inside rabbling mechanism of concentrated mechanism and set up at the control panel on concentrated mechanism right side and install the filtering mechanism in concentrated mechanism bottom, the filtering mechanism top and concentrated mechanism bottom turn-on connection, concentrated mechanism includes concentrated room, heater, the heater is through heating with the evaporation of concentrated indoor portion liquid, concentrated room is including concentrated frame, concentrated frame left end top and feeder hopper bottom turn-on connection. The utility model discloses can keep the constant temperature heating with the evaporation of water in the solution, can not cause the energy extravagant like this, can stir when the device heats, the heating is even like this, can increase concentration efficiency. However, the concentration and evaporation efficiency is low.
Disclosure of Invention
The invention provides a concentration and filtration device for preparing a medical intermediate, which is used for solving the problem of low evaporation efficiency of the existing concentration reaction tank. The specific scheme is as follows:
a concentration and filtration device for preparing a medical intermediate comprises a control device, and a primary filter, a primary concentration device, a secondary concentration device, a multi-stage membrane filter, a liquid collection tank and a plurality of connecting pipelines which are arranged in sequence,
the primary filter is used for filtering fibers in the plant stock solution, and a pressurizing device is arranged between the liquid outlet end of the primary filter and the primary concentration device;
the pressurizing device is positioned at the top of the primary concentration device, a pressurizing pump is arranged outside the pressurizing device, a high-pressure air inlet of the pressurizing device is connected with the pressurizing pump, a liquid inlet end of the pressurizing device is connected with a liquid outlet end of the primary filter, and an electric control valve is arranged on the pressurizing device;
the heating part is arranged on the circumferential direction of the inner wall of the primary concentration device, the liquid storage cavity is arranged in the middle of the primary concentration device, and the recovery valve component is arranged outside the primary concentration device;
the output end of the liquid storage bin is arranged corresponding to the heating part, the liquid storage bin is fixedly connected to the primary concentration device, and the input end of the liquid storage bin is connected with the output end of the pressurizing device;
the recovery valve assembly is detachably connected to one side of the top of the primary concentration device, the air inlet end of the recovery valve assembly is connected with the air outlet end of the primary concentration device, and a heat exchange system is arranged between the air outlet end of the recovery valve assembly and the secondary concentration device;
the heat exchange system is respectively connected with the recovery valve assembly and the secondary concentration device;
the liquid inlet end of the secondary concentration device is connected with the liquid outlet end of the primary concentration device, and the liquid outlet end of the secondary concentration device is sequentially connected with a multistage membrane filter and a liquid collection tank.
Preferably, the primary concentrating device is of a hollow structure, a primary liquid collecting area is arranged at the bottom of the inner side of the primary concentrating device, an airflow outlet is arranged at one side of the primary concentrating device close to the recovery valve component,
a primary liquid outlet is formed in the primary liquid collecting area;
the heating part comprises a plurality of heating blocks which are arranged on the inner wall of the primary concentration device at intervals;
the heating block is detachably connected to the primary concentration device, the heating block is electrically connected with the control device respectively, and a concentration tank is formed between the heating blocks.
Preferably, the liquid storage bin comprises a gas-liquid mixing cavity and a spray pipe which are arranged up and down,
the gas-liquid mixing cavity is fixedly connected with the top of the primary concentration device,
the input end of the gas-liquid mixing cavity is connected with the output end of the pressurizing device, and the output end of the gas-liquid mixing cavity is connected with the input end of the spray pipe;
a plurality of spray heads are arranged on the spray pipe at intervals;
the spouts of the spray heads are arranged in one-to-one correspondence with the concentration tanks, the spout orientations of the spray heads face the concentration tanks, and the spray heads are fixedly connected to the spray pipes.
Preferably, the recovery valve assembly includes a valve body,
the valve body is positioned at the air outlet end of the primary concentration device, the valve body is detachably connected with the outer side of a primary filtrate output port of the primary concentration device, the valve body is of a hollow structure and comprises a pressure cavity and an operation cabin which are horizontally arranged,
the operation bin is positioned on one side of the pressure cavity, which is far away from the primary concentration device, and an air cylinder is arranged in the operation bin;
the cylinder barrel of the cylinder is fixedly connected in the operation cabin, the piston end of the cylinder faces the pressure cavity, the piston end of the cylinder is provided with a shaft rod, and the cylinder is electrically connected with the control device;
one end of the shaft lever is detachably connected with the piston end of the cylinder, and the other end of the shaft lever penetrates through the operation cabin and is positioned in the pressure cavity;
a film pressure plate is arranged in the pressure cavity, an air inlet of the pressure cavity is connected with an air outlet end of the primary concentration device, an air outlet is arranged at the top of the pressure cavity, and the air outlet is connected with an input end of a heat exchange system;
the film pressure plate is correspondingly arranged at an air inlet of the pressure cavity, the film pressure plate is vertically connected to one end, located at the pressure cavity, of the shaft rod, and a pressure film is arranged in the film pressure plate;
the pressure membrane is embedded in the middle of the membrane pressure plate and extends out of the membrane pressure plate, and the part of the pressure membrane extending out of the membrane pressure plate is fixedly connected to the inner wall of the pressure cavity and divides the pressure cavity into a first area and a second area which are independent;
the first area is close to one side of the gas outlet end of the primary concentration device, and the second area is positioned close to one side of the valve body;
the air inlet and the air outlet of the pressure cavity are both positioned in the first area.
Preferably, at least two secondary concentration devices are arranged, each secondary concentration device comprises a concentration tank,
the concentration tank is of a cavity structure, a secondary liquid inlet is formed in the top of the concentration tank, a secondary liquid collecting area is formed in the bottom of the inner side of the concentration tank, an evaporation outlet is formed in one side of the top of the concentration tank, and a section of sealed hollow heating groove is formed in the side wall of the concentration tank;
the heating tank is fixedly connected with one side of the concentration tank close to the bottom, a conduction sheet is arranged in the heating tank, a heat medium inlet and a heat medium outlet are respectively arranged on the heating tank,
the evaporation outlet, the heat medium inlet and the heat medium outlet are respectively connected with the heat exchange system;
the secondary liquid collecting area is provided with a secondary liquid outlet which is connected with a liquid inlet of the multistage film filter;
the secondary liquid inlet is connected with the primary liquid outlet.
Preferably, the heat exchange system comprises a heat exchanger, a cooling tank and a standby tank,
the input end of the heat exchanger is connected with the air outlet end of the valve body, and the output end of the heat exchanger is connected with the heat medium inlet;
the standby tank is connected with the heat medium outlet;
the cooling tank is connected with the evaporation port.
Preferably, the primary filter is a multi-stage membrane filter with a large aperture, and the liquid inlet end of the primary filter is connected with the stock solution tank through a filtering pipeline;
and the filtering pipeline is provided with an electromagnetic valve.
Preferably, each air flow pipeline of the equipment is provided with an electromagnetic valve.
Compared with the prior art, the beneficial effect of this application lies in:
the method comprises the following steps of realizing fine filtration of plant stock solution by a primary filter, a primary concentration device, a secondary concentration device and a multi-stage membrane filter which are sequentially arranged, wherein a pressurizing device is arranged between the primary filter and the primary concentration device, the primary filtration stock solution entering the primary concentration device is a high-pressure air-pressure mixture by the pressurizing device, a concentration groove opposite to a spraying port of the high-pressure air-pressure mixture is arranged in the primary concentration device, and the evaporation speed of water is improved by preheating heating blocks on two sides of the concentration groove;
meanwhile, when the plant stock solution is sprayed to the surface of the concentration tank, part of the plant primary filtering stock solution is subjected to flash evaporation on the surface of the concentration tank to form an isolated steam film, and the isolated steam film enables the rest plant stock solution not to be directly contacted with the surface of the concentration tank and only can be used for carrying out partial evaporation in heat convection formed between the heating block and the heating block, so that the water evaporation capacity of the plant stock solution entering the interior of the primary concentration device in each period can be controlled, and the fine control of the evaporation speed is realized;
this application is through setting up recovery valve subassembly and heat transfer system between primary enrichment facility and secondary enrichment facility, and the multi-waste heat that produces in the primary enrichment facility can be carried to the secondary enrichment facility in through the heat exchanger, realizes secondary enrichment facility's constant temperature and filters, has realized providing the constant temperature effect of longer time under the same energy consumption to the energy consumption has been reduced.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic structural diagram of a concentration and filtration apparatus for preparing pharmaceutical intermediates according to an embodiment of the present invention;
FIG. 2 is a schematic view showing the connection between a primary concentrating device and a recovery valve assembly in a concentrating and filtering apparatus for preparing pharmaceutical intermediates according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a secondary concentration device in a concentration and filtration apparatus for preparing pharmaceutical intermediates according to an embodiment of the present invention;
wherein, 1-a first electromagnetic valve, 2-a primary filter, 3-a second electromagnetic valve, 4-a third electromagnetic valve, 5-a pressure pump, 6-a first concentration device, 7-a liquid storage bin 7, 8-a high-pressure air inlet, 9-a pressure device, 10-an electric control valve, 11-a fourth electromagnetic valve, 12-a recovery valve component, 13-a fifth electromagnetic valve, 14-a sixth electromagnetic valve, 15-a seventh electromagnetic valve, 16-a heat exchanger, 17-an eighth electromagnetic valve, 18-a cooling tank, 19-a ninth electromagnetic valve, 20-a second concentration device, 21-a tenth electromagnetic valve, 22-an eleventh electromagnetic valve, 23-a twelfth electromagnetic valve, 24-a multistage membrane filter, 25-a thirteenth electromagnetic valve, 26-a liquid collection tank, 100-control device, 120-valve body, 121-pressure chamber, 122-operation chamber, 123-shaft lever, 124-spring, 125-pressure plate, 600-mixing chamber, 601-primary liquid collecting area, 602-primary liquid outlet, 603-spray pipe, 604-spray head, 605-heating block, 606-concentration tank, 607-air flow outlet, 20-secondary concentration device, 200-primary liquid inlet, 201-concentration tank, 202-evaporation outlet, 203-conducting sheet, 204-heating tank, 205-secondary liquid collecting area, 206-secondary liquid outlet, 207-heat medium inlet, and 208-heat medium outlet.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
The concentration and filtration equipment for preparing the medical intermediate shown in the attached figures 1-3 comprises a control device 100, and a primary filter 2, a primary concentration device 6, a secondary concentration device 2, a multi-stage membrane filter 24, a liquid collection tank 26 and a plurality of connecting pipelines which are arranged in sequence,
the primary filter 2 is used for filtering fibers in the plant stock solution, and a pressurizing device 9 is arranged between the liquid outlet end of the primary filter 2 and the primary concentration device 6;
the pressurizing device 9 is positioned at the top of the primary concentrating device 6, a pressurizing pump 5 is further arranged outside the pressurizing device 9, a high-pressure air inlet 8 of the pressurizing device 9 is connected with the pressurizing pump 5, the liquid inlet end of the pressurizing device 9 is connected with the liquid outlet end of the primary filter 2, and an electric control valve 10 is arranged on the pressurizing device 9;
a heating part is arranged on the circumferential direction of the inner wall of the primary concentration device 6, a liquid storage cavity is arranged in the middle of the primary concentration device 6, and a recovery valve component 12 is arranged outside the primary concentration device 6;
the output end of the liquid storage bin 7 is arranged corresponding to the heating part, the liquid storage bin 7 is fixedly connected to the primary concentration device 6, and the input end of the liquid storage bin 7 is connected with the output end of the pressurizing device 9;
the recovery valve assembly 12 is detachably connected to one side of the top of the primary concentration device 6, the air inlet end of the recovery valve assembly 12 is connected with the air outlet end of the primary concentration device 6, and a heat exchange system is arranged between the air outlet end of the recovery valve assembly 12 and the secondary concentration device 20;
the heat exchange system is respectively connected with the recovery valve assembly 12 and the secondary concentration device 20;
the liquid inlet end of the secondary concentration device 20 is connected with the liquid outlet end of the primary concentration device 6, and the liquid outlet end of the secondary concentration device 20 is sequentially connected with a multistage membrane filter 24 and a liquid collection tank 26.
Further, the primary concentrating device 6 is a hollow structure, a primary liquid collecting area 601 is arranged at the bottom of the inner side of the primary concentrating device 6, an airflow outlet 607 is arranged at one side of the primary concentrating device 6 close to the recovery valve component 12,
a primary liquid outlet 602 is arranged at the primary liquid collecting area 601;
the heating part comprises a plurality of heating blocks 605 which are arranged on the inner wall of the primary concentration device 6 at intervals;
the heating blocks 605 are detachably connected to the primary concentration device 6, the heating blocks 605 are electrically connected to the control device 100, and a concentration tank 606 is formed between adjacent heating blocks 605.
Further, the liquid storage bin 7 comprises a gas-liquid mixing cavity 600 and a spray pipe 603 which are arranged up and down,
the gas-liquid mixing cavity 600 is fixedly connected to the top of the primary concentration device 6, the input end of the gas-liquid mixing cavity 600 is connected with the output end of the pressurizing device 9, and the output end of the gas-liquid mixing cavity 600 is connected with the input end of the spray pipe 603;
a plurality of spray heads 604 are arranged on the spray pipe 603 at intervals;
the nozzles of the spray heads 604 correspond to the thickening tanks 606 one by one, the nozzle directions of the spray heads 604 face the thickening tanks 606, and the spray heads 604 are fixedly connected to the spray pipes 603.
Further, the recovery valve assembly 12 includes a valve body 120,
the valve body 120 is located at the air outlet end of the primary concentration device 6, the valve body 120 is detachably connected to the outer side of the primary filtrate outlet of the primary concentration device 6, the valve body 120 is of a hollow structure, the valve body 120 comprises a pressure chamber 121 and an operation chamber 122 which are horizontally arranged,
the operation cabin 122 is positioned on one side of the pressure chamber 121 far away from the primary concentration device 6, and an air cylinder 126 is arranged in the operation cabin 122;
the cylinder barrel of the air cylinder 126 is fixedly connected in the operation cabin 122, the piston end of the air cylinder 126 faces the pressure chamber 121, the piston end of the air cylinder 126 is provided with a shaft rod 123, and the air cylinder 126 is electrically connected with the control device 100;
one end of the shaft rod 123 is detachably connected with the piston end of the cylinder 126, and the other end of the shaft rod 123 passes through the operation cabin 122 and is positioned in the pressure cavity 121;
a film pressure plate 125 is arranged in the pressure chamber 121, an air inlet of the pressure chamber 121 is connected with an air outlet end of the primary concentration device 6, an air outlet is arranged at the top of the pressure chamber 121, and the air outlet is connected with an input end of a heat exchange system;
the film pressure plate 125 is correspondingly arranged at the air inlet of the pressure chamber 121, the film pressure plate 125 is vertically connected to one end of the shaft 123 at the pressure chamber 121, and a pressure film is arranged in the film pressure plate 125;
the pressure membrane is embedded in the middle of the membrane pressure plate 125 and extends out of the membrane pressure plate 125, the part of the pressure membrane extending out of the membrane pressure plate 125 is fixedly connected to the inner wall of the pressure chamber 121, and the pressure chamber 121 is divided into a first area and a second area which are independent;
the first area is close to one side of the gas outlet end 607 of the primary concentration device 6, and the second area is close to one side of the valve body 120;
the inlet and outlet of the pressure chamber 121 are located in the first region.
In this application, the valve body 120 is hollow, the push rod of the cylinder 126 fixed inside the valve body 120 is connected with the shaft 123, the end of the shaft 123 far away from the cylinder 126 is connected with the membrane pressure plate 125, and the pressure membrane is arranged inside the membrane pressure plate 125, when the membrane pressure plate 125 is pulled by the shaft 123 towards the primary concentration device 6 under the action of the cylinder 126, the airflow outlet 607 is opened, and the high-pressure airflow and the high-pressure steam are input into the heat exchanger 16 through the airflow outlet 607 and through the fifth solenoid valve 14 and the sixth solenoid valve 15.
Further, at least two secondary concentration devices 20 are provided, the secondary concentration device 20 comprises a concentration tank 201,
the concentration tank 201 is of a cavity structure, a secondary liquid inlet 200 is formed in the top of the concentration tank 201, a secondary liquid collecting area 205 is formed in the bottom of the inner side of the concentration tank 201, an evaporation outlet 202 is formed in one side of the top of the concentration tank 201, and a section of sealed hollow heating groove 204 is formed in the side wall of the concentration tank 201;
the heating tank 204 is fixedly connected to one side of the concentration tank 201 close to the bottom, a conduction sheet 203 is arranged in the heating tank 204, a heat medium inlet 207 and a heat medium outlet 208 are respectively arranged on the heating tank 204,
the evaporation outlet 202, the heat medium inlet 207 and the heat medium outlet 208 are respectively connected with the heat exchange system;
the secondary liquid collecting area 205 is provided with a secondary liquid outlet 206, and the secondary liquid outlet 206 is connected with a liquid inlet of the multistage membrane filter 24;
the secondary inlet port 200 is connected to the primary outlet port 602.
In the application, the heat medium may be steam or oil, the heat medium outlet may be connected to the spare tank, the 208 heat medium outlet is connected to the spare tank, and the spare tank is connected to the heat exchanger 16 and circulates into the heat exchanger 16 again, so that the heat medium inside the heating tank 204 can form a circulation, and the temperature of the secondary concentration tank is ensured to be constant;
the cooling tank 18 is used for cooling and collecting the water vapor generated in the secondary concentration process.
Further, the heat exchange system comprises a heat exchanger 16, a cooling tank 18 and a spare tank,
the input end of the heat exchanger 16 is connected with the gas outlet end of the valve body 120, and the output end of the heat exchanger 16 is connected with the heat medium inlet 207;
the spare tank is connected to the heat medium outlet 208;
the cooling tank 18 is connected to the evaporation port 202.
Further, the primary filter 2 is a multi-stage membrane filter with a large aperture, and the liquid inlet end of the primary filter 2 is connected with the stock solution tank through a filtering pipeline;
and the filtering pipeline is provided with an electromagnetic valve 1.
In the present application, in the process of delivering the plant raw liquid to the multistage membrane filter by the primary filter 2, i.e., the raw liquid tank, it is necessary to pressurize the plant raw liquid by a pressurizing pump according to actual needs.
Furthermore, each air flow pipeline of the equipment is provided with an electromagnetic valve.
It should be noted that the detachable connection in the present application is realized by, but not limited to, a screw/bolt connection;
the joints in the application are sealed in a conventional sealing mode;
the shaft 123 in the present application is further sleeved with a spring 124, the spring 124 is located in the pressure strong chamber 121, one end of the spring 124 abuts against the membrane pressure plate 125, and the other end of the spring 124 is clamped at the connection between the pressure chamber 121 and the valve body 120;
in the application, a first electromagnetic valve 1 is arranged on a liquid inlet pipeline of a primary filter 2; a second electromagnetic valve 3 is arranged on an output pipeline of the primary filter 2; a third electromagnetic valve 4 is arranged on an output pipeline of the pressure pump 5; a fourth electromagnetic valve 11 is arranged on an output pipeline of the primary concentration device 6, and a sixth electromagnetic valve 14 and a seventh electromagnetic valve 15 are respectively arranged between the heat exchanger 16 and the recovery valve component 12; a fifth electromagnetic valve 13 and a twelfth electromagnetic valve 23 are respectively arranged on a connecting pipeline of the heat exchanger 16 and the secondary concentration device 20; a ninth electromagnetic valve 19 and a tenth electromagnetic valve 21 are respectively arranged on pipelines between the two secondary concentration devices 20 and the cooling tank 18; an eleventh electromagnetic valve 22 is arranged on a pipeline between the two secondary concentration devices 20 and the standby tank; an eighth electromagnetic valve 17 is arranged on a connecting pipeline between the secondary concentration device 20 and the multistage membrane filter 24; a thirteenth electromagnetic valve 25 is arranged between the multistage membrane filter 24 and the liquid storage tank 26, all the electromagnetic valves, the air cylinder 126 and the heat exchanger 16 in the application are electrically connected with the control device 100, and the automatic control of the device is realized through the control device 100.
The working process of the equipment is as follows:
first, the primary filtration of the plant stock solution
The plant stock solution is conveyed into a primary filter 2, the primary filter 2 filters fibers in the plant stock solution, and then the primary filtered stock solution is conveyed into a primary concentration device 6 through a pressurizing device 9, and the primary concentration device 6 carries out primary filtration on the plant stock solution; in the process that the primary filter 2 conveys the primary filtering stock solution to the primary concentration device 6, the control device 100 controls the flow rate of the plant stock solution entering the pressurization device 9 in each period by controlling the periodic opening and closing of the electric control valve 10 on the pressurization device 9; the primary concentration device 6 comprises a control device 100 for controlling a pressure pump 5 to pressurize a pressure device 9, so that the primary plant filtered stock solution and the high-pressure air flow entering the pressure device 9 are mixed in a mixing cavity 600, the mixed stock solution is sprayed into a concentration tank 606 between a heating block and the heating block through a plurality of spray heads arranged on a spray pipe 603 by a spray pipe 603 arranged on the lower part of the mixing cavity 600, the preheating temperature of the heating block is controlled by the control device 100, so that when the primary plant stock solution is sprayed onto the surface of the concentration tank 606, part of the primary plant stock solution is flashed on the surface of the concentration tank 606 to form an isolation steam film, the isolation steam film prevents the rest of the primary plant stock solution from directly contacting the surface of the concentration tank 606 and only partially evaporates in the heat convection formed between the heating block and the heating block, and therefore, the evaporation capacity of moisture of the primary plant stock solution entering the primary concentration device in each period can be controlled, thereby controlling the concentration to obtain a primary concentrated solution, and improving the concentration efficiency of the primary concentration device 6;
secondly, the primary filtrate filtered by the primary concentration device 6 is conveyed to a secondary concentration device 20,
during the process of jet evaporation, the pressure inside the primary concentration device 6 rises sharply due to the high-pressure airflow and the high-pressure steam formed due to evaporation inside the primary concentration device 6, the initial threshold value of the membrane pressure plate 125 is exceeded, the membrane pressure plate 125 is forced to open the airflow outlet between the primary concentration device and the primary concentration device, and the high-pressure airflow and the high-pressure steam are conveyed into the heat exchanger 16 through the airflow outlet;
at least one set of secondary concentration devices 20; each secondary concentration device 20 comprises a shell 201, a section of sealed hollow heating groove 204 is arranged at the lower part of the shell 201 and positioned inside, a conducting sheet 203 is arranged inside the heating groove, the heating groove 204 is connected with a heat exchanger 16 through a first pipeline, and heat is transferred to the inside of the heating groove 204 through the first pipeline after heat exchange of high-pressure air flow and high-pressure steam is carried out through the heat exchanger 16, so that the primary concentrated solution entering the inside of the secondary concentration device 20 is subjected to constant-temperature evaporation concentration;
and (5) obtaining a secondary concentrated solution after constant-temperature evaporation and concentration.
Wherein the control apparatus 100 sets the initial threshold value of the thin film pressure plate 125 by the following method;
the control device 100 controls the air cylinder 126 to push the shaft 123 to drive the membrane pressure plate 125 on the shaft to move towards the side of the air outlet 607 until the air outlet is sealed, and an initial threshold value of the membrane pressure plate 125 is obtained through conversion according to the advancing stroke of the air cylinder 126; and acquires a corresponding pressure range value through the advancing stroke of one unit amount of cylinder, stores the pressure range values corresponding to the advancing strokes of different cylinders in the memory of the control device 100, meanwhile, the control device 100 may also control the retraction process of the air cylinder 126 according to the pressure range value corresponding to the propulsion stroke of different air cylinders, specifically, by arranging a pressure sensor at the air flow outlet, the pressure sensor being connected to the control device 100, the control device 100 loading the data in the memory and comparing the real-time pressure collected by the pressure sensor with the set initial threshold value, when the real-time pressure inside the primary concentrating device 6 is compared with the set initial threshold, the control device 100 controls the cylinder to drive the membrane pressure plate 125 to retreat by a set stroke position every time the real-time pressure exceeds the initial threshold and increases by a unit amount; when the real-time pressure is less than the set initial threshold, the control means controls the cylinder to advance to seal the gas flow outlet, that is, the membrane pressure plate 125 opens the gas flow outlet 607 with the cylinder returning only when the real-time pressure is greater than the initial threshold.
Thirdly, the secondary concentrated solution is filtered for the second time by a multistage membrane filter 24 and is conveyed to a liquid collecting tank 26 to finish the final filtration,
it will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (8)
1. A concentration and filtration device for preparing a medical intermediate is characterized by comprising a control device (100), and a primary filter (2), a primary concentration device (6), a secondary concentration device (2), a multi-stage membrane filter (24), a liquid collection tank (26) and a plurality of connecting pipelines which are arranged in sequence,
the primary filter (2) is used for filtering fibers in the plant stock solution, and a pressurizing device (9) is arranged between the liquid outlet end of the primary filter (2) and the primary concentration device (6);
the pressurizing device (9) is positioned at the top of the primary concentrating device (6), a pressurizing pump (5) is further arranged outside the pressurizing device (9), a high-pressure air inlet (8) of the pressurizing device (9) is connected with the pressurizing pump (5), the liquid inlet end of the pressurizing device (9) is connected with the liquid outlet end of the primary filter (2), and an electric control valve (10) is arranged on the pressurizing device (9);
a heating part is arranged on the circumferential direction of the inner wall of the primary concentration device (6), a liquid storage cavity is arranged in the middle of the primary concentration device (6), and a recovery valve component (12) is arranged outside the primary concentration device (6);
the output end of the liquid storage bin (7) is arranged corresponding to the heating part, the liquid storage bin (7) is fixedly connected to the primary concentration device (6), and the input end of the liquid storage bin (7) is connected with the output end of the pressurizing device (9);
the recovery valve assembly (12) is detachably connected to one side of the top of the primary concentration device (6), the air inlet end of the recovery valve assembly (12) is connected with the air outlet end of the primary concentration device (6), and a heat exchange system is arranged between the air outlet end of the recovery valve assembly (12) and the secondary concentration device (20);
the heat exchange system is respectively connected with the recovery valve assembly (12) and the secondary concentration device (20);
the liquid inlet end of the secondary concentration device (20) is connected with the liquid outlet end of the primary concentration device (6), and the liquid outlet end of the secondary concentration device (20) is sequentially connected with a multistage membrane filter (24) and a liquid collection tank (26).
2. A concentration and filtration apparatus for the preparation of pharmaceutical intermediate according to claim 1, wherein the primary concentration device (6) is a hollow structure, a primary liquid collecting area (601) is provided at the bottom of the inner side of the primary concentration device (6), an air flow outlet (607) is provided at the side of the primary concentration device (6) close to the recovery valve assembly (12),
a primary liquid outlet (602) is arranged at the primary liquid collecting area (601);
the heating part comprises a plurality of heating blocks (605) which are arranged on the inner wall of the primary concentration device (6) at intervals;
the heating blocks (605) are detachably connected to the primary concentration device (6), the heating blocks (605) are respectively and electrically connected with the control device (100), and a concentration groove (606) is formed between every two adjacent heating blocks (605).
3. The apparatus for the preparation of pharmaceutical intermediates according to claim 2, wherein the liquid storage tank (7) comprises a gas-liquid mixing chamber (600) and a nozzle (603) arranged above each other,
the gas-liquid mixing cavity (600) is fixedly connected to the top of the primary concentration device (6), the input end of the gas-liquid mixing cavity (600) is connected with the output end of the pressurizing device (9), and the output end of the gas-liquid mixing cavity (600) is connected with the input end of the spray pipe (603);
a plurality of spray heads (604) are arranged on the spray pipe (603) at intervals;
the spouts of the spray head (604) are arranged in one-to-one correspondence with the thickening tank (606), the spout orientations of the spray head (604) face the thickening tank (606), and the spray head (604) is fixedly connected to the spray pipe (603).
4. A concentration and filtration apparatus for the preparation of pharmaceutical intermediate according to claim 1, wherein the recovery valve assembly (12) comprises a valve body (120),
the valve body (120) is positioned at the air outlet end of the primary concentration device (6), the valve body (120) is detachably connected to the outer side of a primary filtrate output port outside the primary concentration device (6), the valve body (120) is of a hollow structure, the valve body (120) comprises a pressure cavity (121) and an operation cabin (122) which are horizontally arranged,
the operation cabin (122) is positioned on one side of the pressure cavity (121) far away from the primary concentration device (6), and an air cylinder (126) is arranged in the operation cabin (122);
the cylinder barrel of the air cylinder (126) is fixedly connected in the operation cabin (122), the piston end of the air cylinder (126) faces to the pressure cavity (121), the piston end of the air cylinder (126) is provided with a shaft rod (123), and the air cylinder (126) is electrically connected with the control device (100);
one end of the shaft rod (123) is detachably connected with the piston end of the air cylinder (126), and the other end of the shaft rod (123) penetrates through the operation cabin (122) and is positioned in the pressure cavity (121);
a film pressure plate (125) is arranged in the pressure cavity (121), an air inlet of the pressure cavity (121) is connected with an air outlet end of the primary concentration device (6), an air outlet is arranged at the top of the pressure cavity (121), and the air outlet is connected with an input end of a heat exchange system;
the film pressure plate (125) is correspondingly arranged at an air inlet of the pressure cavity (121), the film pressure plate (125) is vertically connected to one end, located at the pressure cavity (121), of the shaft rod (123), and a pressure film is arranged in the film pressure plate (125);
the pressure membrane is embedded in the middle of the membrane pressure plate (125) and extends out of the membrane pressure plate (125), the part of the pressure membrane extending out of the membrane pressure plate (125) is fixedly connected with the inner wall of the pressure cavity (121) and divides the pressure cavity (121) into a first area and a second area which are independent;
the first area is close to one side of the air outlet end (607) of the primary concentration device (6), and the second area is positioned close to one side of the valve body (120);
the air inlet and the air outlet of the pressure cavity (121) are both positioned in the first area.
5. The concentration and filtration apparatus for the preparation of pharmaceutical intermediate according to claim 4, wherein the secondary concentration device (20) is provided with at least two, the secondary concentration device (20) comprises a concentration tank (201),
the concentration tank (201) is of a cavity structure, a secondary liquid inlet (200) is formed in the top of the concentration tank (201), a secondary liquid collecting area (205) is formed in the bottom of the inner side of the concentration tank (201), an evaporation outlet (202) is formed in one side of the top of the concentration tank (201), and a section of sealed hollow heating groove (204) is formed in the side wall of the concentration tank (201);
the heating tank (204) is fixedly connected with one side of the concentration tank (201) close to the bottom, a conduction sheet (203) is arranged in the heating tank (204), a heat medium inlet (207) and a heat medium outlet (208) are respectively arranged on the heating tank (204),
the evaporation outlet (202), the heat medium inlet (207) and the heat medium outlet (208) are respectively connected with the heat exchange system;
the secondary liquid collecting area (205) is provided with a secondary liquid outlet (206), and the secondary liquid outlet (206) is connected with a liquid inlet of the multi-stage membrane filter (24);
the secondary liquid inlet (200) is connected with the primary liquid outlet (602).
6. A concentration and filtration apparatus for the preparation of pharmaceutical intermediates according to claim 5, wherein the heat exchange system comprises a heat exchanger (16), a cooling tank (18) and a backup tank,
the input end of the heat exchanger (16) is connected with the air outlet end of the valve body (120), and the output end of the heat exchanger (16) is connected with the heat medium inlet (207);
the spare tank is connected with the heat medium outlet (208);
the cooling tank (18) is connected to the evaporation port (202).
7. The concentration and filtration equipment for preparing the pharmaceutical intermediate according to claim 1, wherein the primary filter (2) is a multi-stage membrane filter with large aperture, and the liquid inlet end of the primary filter (2) is connected with a raw liquid tank through a filtration pipeline;
and the filtering pipeline is provided with an electromagnetic valve (1).
8. The apparatus as claimed in claim 1, wherein each of the gas flow lines of the apparatus is provided with a solenoid valve.
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| CN202210871702.1A CN115054983B (en) | 2022-07-23 | 2022-07-23 | A concentrated filtration equipment for preparing medical intermediate |
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| CN202210871702.1A CN115054983B (en) | 2022-07-23 | 2022-07-23 | A concentrated filtration equipment for preparing medical intermediate |
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