Piperazine spray granulation system

The piperazine spray granulation system solves the problems of dust-prone and explosion hazards in the preparation of piperazine powder. The circulating nitrogen cooling and pulse cleaning technology are used to achieve safe and low-cost piperazine production.

CN223127961UActive Publication Date: 2025-07-22TIANHUA INSTITUTE OF CHEMICAL MACHINERY AND AUTOMATION CO LTD +1
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Patent Information

Application Number
CN202422129354.8
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-08-31
Publication Date
2025-07-22
Estimated Expiration
2034-08-31

AI Technical Summary

Technical Problem

The preparation of piperazine powder is prone to dust, high risk of explosion, high sealing requirements for slicer and high failure rate, and it is difficult for the existing technology to achieve safe and low-cost production.

Method used

The piperazine spray granulation system is adopted, including granulation towers, bag dust collectors, product silos, high-efficiency filters, circulating blowers, coolers and related valves and instruments. Through circulating nitrogen cooling and pulse ash cleaning technology, the spray granulation and gas-solid separation of piperazine is achieved.

Benefits of technology

A safe and reliable piperazine spray granulation process is realized, reducing the cost of investment and operation and maintenance of the device, improving the degree of automation and sealing, ensuring production safety and energy-saving effects.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The utility model discloses a piperazine spray granulation system which comprises a granulation tower, a bag-type dust collector and a product bin, an input port of the granulation tower is connected with a piperazine feed pipe, an output port of the granulation tower is connected with the bag-type dust collector, and an output port of the bag-type dust collector is connected with the product bin. The piperazine spray granulation system disclosed by the utility model is short in flow, low in device investment and high in automation and sealing degree, nitrogen can be recycled in the granulation process, and the method is safe, reliable and simple to start, and can ensure safe production; preferably, the circulating air blower in the system method can also be placed on an outlet pipeline of the high-efficiency filter, and waste nitrogen is discharged by gas before cooling, so that energy is saved, and consumption is reduced.
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Description

Technical Field

[0001] The utility model belongs to the technical field of piperazine preparation and production, and particularly relates to a piperazine spray granulation system. Background Technique

[0002] Piperazine is an important pharmaceutical intermediate and fine chemical raw material, and is widely used in the synthesis of drugs such as antibacterial drugs, antihypertensive and hypoglycemic drugs, sedative and analgesic drugs, antihistamines, anthelmintics, etc. and the production of fine chemical products such as surfactants, preservatives, and stabilizers.

[0003] In production, piperazine can be prepared into products in the form of powder or slices. The disadvantage of powder is that it is easy to generate dust, has a very high explosion risk, and is inconvenient for packaging and transportation; in the process route of using a slicing machine to prepare products, the sealing requirement of the slicing machine is relatively high, and the slicing machine has a relatively high failure rate, and the operation and maintenance costs are high. The granulation process uses a circulating nitrogen cooling method to cool and crystallize the molten piperazine material for granulation, with low device investment cost and simple operation. Summary of the Invention

[0004] The utility model provides a piperazine spray granulation system, which includes a granulation tower, a bag filter, a product silo, a high-efficiency filter, a circulating blower, a cooler, and instruments, valves, etc., and can perform piperazine spray granulation operations with a short operation process and low device investment.

[0005] The technical solution adopted by the utility model to solve its technical problems is: a piperazine spray granulation system, which includes a granulation tower, a bag filter, and a product silo. The material inlet of the granulation tower is connected to a piperazine feed pipe, the material outlet of the granulation tower is connected to the bag filter, and the product outlet of the bag filter is connected to the product silo.

[0006] The technical solution adopted by the utility model to solve its technical problems further includes:

[0007] A piperazine feed regulating valve is connected to the piperazine feed pipe, a piperazine feed three-way control valve is also connected to the piperazine feed pipe, and a low-pressure nitrogen input port is connected to the piperazine feed three-way control valve.

[0008] A nitrogen input port is opened on the granulation tower, a nitrogen input pipe is communicated with the nitrogen input port, a solenoid valve is connected to the nitrogen input pipe, an oxygen content analyzer is connected to the nitrogen input pipe, and a waste nitrogen discharge valve is connected to the nitrogen input pipe.

[0009] The output port of the granulation tower is arranged at the bottom, and a cleaning liquid control valve is arranged at the top of the granulation tower for controlling the input of the cleaning liquid to clean the inside of the granulation tower through the cleaning liquid.

[0010] An electromagnetic valve is connected to the upper part of the bag filter for pulse backwashing and cleaning of the filter bags; an electromagnetic valve is connected to the lower part of the bag filter for jetting and discharging materials at the bottom of the dust collector; a manual slide valve and a rotary valve are connected to the bottom of the bag filter and are connected to the product silo through the manual slide valve and the rotary valve, and the manual slide valve and the rotary valve are connected in series.

[0011] The purified gas outlet of the bag filter is connected to the inlet pipeline of the high-efficiency filter, connected to the cooler through the high-efficiency filter, the outlet of the cooler is connected to the circulating blower, and the outlet pipeline of the circulating blower is connected to the air inlet on the granulation tower.

[0012] A chilled water supply pipe, a chilled water return pipe, a cooling water inlet pipe and a cooling water return pipe are connected to the cooler.

[0013] A bin dust collector is fixedly installed on the top of the product silo, an electromagnetic valve is installed on the bin dust collector, and the output interface of the bin dust collector is connected to the high-efficiency filter. An electromagnetic valve is provided at the lower part of the product silo, and a manual slide valve and a rotary valve are connected to the bottom of the product silo, and the manual slide valve and the rotary valve are connected in series.

[0014] The beneficial effects of the present utility model are as follows: A piperazine spray granulation system of the present utility model has a short process, low device investment, simple operation and maintenance. Nitrogen in the granulation process can be recycled, with high automation and sealing degree. This method is safe, reliable, and simple to start up, and can ensure safe production; preferably, in the system method of the present invention, the circulating blower can also be placed on the outlet pipeline of the high-efficiency filter, and the waste nitrogen is discharged from the gas before cooling, saving energy and reducing consumption.

[0015] The following will further describe the present utility model in conjunction with the drawings and specific embodiments. Description of the Drawings

[0016] Figure 1 It is a flow chart of the system method for piperazine spray granulation in the present utility model.

[0017] In the figure, 1 - granulation tower, 2 - bag filter, 3 - high-efficiency filter, 4 - cooler, 5 - circulating blower, 6 - product silo, 7 - bin dust collector, 8 - manual slide valve, 9 - rotary valve, 10 - piperazine feed regulating valve, 11 - piperazine feed three-way control valve, 12 - feed nozzle, 13 - oxygen content analyzer, 14 - electromagnetic valve, 15 - waste nitrogen discharge valve, 20 - piperazine liquid, 21 - waste nitrogen, 22 - low-pressure nitrogen, 23 - piperazine powder, 24 - chilled water supply, 25 - chilled water return, 26 - cooling water inlet, 27 - cooling water return, 28 - cleaning liquid. Detailed Embodiments

[0018] This embodiment is the preferred embodiment of the present utility model. Any other embodiments with the same or similar principles and basic structures are within the protection scope of the present utility model.

[0019] Please refer to the attached Figure 1 , the present utility model discloses a piperazine spray granulation system, which mainly includes a granulation tower 1, a bag filter 2 and a product silo 6. The material inlet of the granulation tower 1 is connected to the piperazine feed pipe, the material outlet of the granulation tower 1 is connected to the bag filter 2, and the material outlet of the bag filter 2 is connected to the product silo 6.

[0020] In this embodiment, the piperazine feed pipe is used to input the piperazine liquid 20. A piperazine feed regulating valve 10 is connected to the piperazine feed pipe to regulate the feed rate of the piperazine liquid 20. A piperazine feed three-way control valve 11 is also connected to the piperazine feed pipe. A low-pressure nitrogen input port is connected to the piperazine feed three-way control valve 11 for inputting low-pressure nitrogen 22. It is possible to control the input of the piperazine liquid 20 or the low-pressure nitrogen 22 through the piperazine feed three-way control valve 11, and when needed, the nitrogen purge channel can be opened to purge the pipeline.

[0021] In this embodiment, a nitrogen input port is also provided on the granulation tower 1. The nitrogen input pipe is communicated with the nitrogen input port. A solenoid valve 14 is connected to the nitrogen input pipe. The low-pressure nitrogen 22 is input into the granulation tower 1 through the nitrogen input pipe to supplement the nitrogen in the system. In this embodiment, an oxygen content analyzer 13 is connected to the nitrogen input pipe for analyzing the oxygen content in the circulating nitrogen. A waste nitrogen discharge valve 15 is connected to the nitrogen input pipe. When the oxygen content analyzer 13 detects that the oxygen content in the nitrogen exceeds the preset value, the solenoid valve 14 of the low-pressure nitrogen 22 can be opened to supplement the low-pressure nitrogen 22.

[0022] In this embodiment, the material outlet of the granulation tower 1 is arranged at the bottom, and a cleaning liquid control valve is provided at the top of the granulation tower 1 for controlling the input of the cleaning liquid 28 to clean the inside of the granulation tower 1 through the cleaning liquid 28.

[0023] In this embodiment, a solenoid valve 14 is connected to the upper part of the bag filter 2, and the input of the low-pressure nitrogen 22 to the upper part of the bag filter 2 is controlled through the solenoid valve 14, and pulse cleaning is carried out with the low-pressure nitrogen 22. A solenoid valve 14 is connected to the lower part of the bag filter 2, and the input of the low-pressure nitrogen 22 to the lower part of the bag filter 2 is controlled through the solenoid valve 14, and the bottom of the bag filter 2 is cleared of materials through the low-pressure nitrogen 22.

[0024] In this embodiment, a manual slide valve 8 and a rotary valve 9 are connected to the bottom of the bag filter 2. The material is discharged through the rotary valve 9, and the manual slide valve 8 is used to control the opening and closing of the material output. The bag filter 2 is connected to the product bin 6 through the manual slide valve 8 and the rotary valve 9. The piperazine particles after dust removal by the bag filter 2 can be discharged into the product bin 6 through the manual slide valve 8 and the rotary valve 9. Among them, the discharge speed can be automatically controlled through the rotary valve 9, and the discharge can be manually controlled for opening and closing through the manual slide valve 8. The manual slide valve 8 and the rotary valve 9 are connected in series. In specific implementation, only one of them can also be set.

[0025] In this embodiment, the top of the bag filter 2 is connected to the high-efficiency filter 3, and is connected to the cooler 4 through the high-efficiency filter 3. The nitrogen discharged from the bag filter 2 is filtered through the high-efficiency filter 3, and then enters the next cycle after being cooled by the cooler 4. The outlet of the cooler 4 is connected to the circulation blower 5, and the circulation blower 5 is connected to the nitrogen inlet on the granulation tower 1. The nitrogen cooled by the cooler 4 is blown into the granulation tower 1 through the circulation blower 5 to enter the next cycle. In this embodiment, a chilled water supply pipe, a chilled water return pipe, a cooling water inlet pipe, and a cooling water return pipe are connected to the cooler 4, and the filtered nitrogen is cooled by a water-cooling method.

[0026] In this embodiment, a bin dust collector 7 is fixedly installed on the top of the product bin 6, which can further remove the dust in the product bin 6. An electromagnetic valve 14 is installed on the bin dust collector 7, and low-pressure nitrogen 22 can be input into the bin dust collector 7 through the electromagnetic valve 14. The bin dust collector 7 is pulse-cleaned with the low-pressure nitrogen 22. The output interface of the bin dust collector 7 is connected to the high-efficiency filter 3. The nitrogen discharged from the bin dust collector 7 is filtered through the high-efficiency filter 3, and then enters the next cycle after being cooled by the cooler 4.

[0027] In this embodiment, an electromagnetic valve 14 is provided at the lower part of the product bin 6. Low-pressure nitrogen 22 can be input into the product bin 6 through the electromagnetic valve 14, and the bottom of the product bin 6 is cleared of materials by the low-pressure nitrogen 22. A manual slide valve 8 and a rotary valve 9 are connected to the bottom of the product bin 6, and the material can be discharged by its own gravity. The piperazine powder 23 is discharged from the product bin 6 through the manual slide valve 8 and the rotary valve 9. Among them, the discharge speed can be automatically controlled through the rotary valve 9, and the discharge can be manually controlled for opening and closing through the manual slide valve 8. The manual slide valve 8 and the rotary valve 9 are connected in series. In specific implementation, the manual slide valve 8 can also be changed to a ball valve or only the rotary valve 9 can be set.

[0028] A method for spray granulation of piperazine in the present utility model. Among them, the piperazine liquid 20 material from the feed pump adjusts the flow rate through the piperazine feed regulating valve 10 and then enters the feed nozzle 12 in the granulation tower 1 through the piperazine feed three-way control valve 11. The piperazine liquid 20 is atomized by the feed nozzle 12 and sprayed into the interior of the granulation tower 1 equipment. The circulating cooling nitrogen inlet is arranged at the top of the granulation tower 1. The cooling nitrogen comes from the circulating blower 5 and contacts the atomized piperazine liquid 1 in a co-current manner for cooling granulation.

[0029] The granulated piperazine powder 23 enters the bag filter 2 of the granulation tower under the action of air flow for gas-solid separation. The separated piperazine powder 23 enters the product silo 6 from the bottom of the bag filter through the manual slide valve 8 and the rotary valve 9. The top of the product silo 6 is equipped with a silo dust collector 7. The gas purified by the silo dust collector 7 and the gas purified by the bag filter 2 of the granulation tower enter the downstream high-efficiency filter 3 for further purification and filtration together.

[0030] The filtered circulating nitrogen enters the cooler 4 and is cooled to the required temperature, and then enters the granulation tower 1 again through the circulating blower 5 for circulation.

[0031] In this embodiment, a manual slide valve 8 and a rotary valve 9 are installed at the bottom of the product silo 6, and it can enter the downstream packaging machine subsequently.

[0032] In this embodiment, the piperazine feed pipeline and feed valves of the granulation tower all adopt jacketed pipes and jacketed valves. The feed nozzle 12 adopts steam tracing to prevent the material from solidifying and blocking the pipeline and nozzle; the piperazine feed three-way control valve 11 contains a feed channel and a nitrogen purging channel. The feed channel is opened during normal operation, and the feed channel is closed during abnormal operation (such as when the downstream pipeline is blocked or after shutdown), and the nitrogen purging channel is opened to purge the pipeline; a cleaning port is arranged at the top of the granulation tower 1; a blockage clearing port is arranged at the bottom of the granulation tower 1 and an air hammer is installed for clearing the material at the bottom during abnormal shutdown.

[0033] Nitrogen jet cleaning devices are arranged at the bottom of the bag filter 2 and the bottom of the product silo 6, and the solenoid valve 14 is used to control the jet switch.

[0034] Preferably, the cooler 4 adopts a finned tube heat exchanger, and the cooling medium adopts circulating cooling water and chilled water for two-stage series cooling. The chilled water supply 24 enters the last group of fins of the last few groups of fins (in a series counter-current manner) of the finned tube heat exchanger, and the chilled water return 25 is discharged from the water outlet of the first group of fins of the last few groups of fins. The chilled water exchanges heat with the circulating nitrogen in a counter-current manner; the cooling water inlet 26 enters from the last group of fins of the first few groups of fins, and the cooling water return 27 is discharged from the water outlet of the first group of fins of the first few groups of fins. The cooling water exchanges heat with the circulating nitrogen in a counter-current manner.

[0035] An oxygen content analyzer 13 is installed on the circulating nitrogen pipeline to prevent the oxygen content in the system from exceeding the standard, and at the same time adjust the flow rate of the fresh nitrogen replenished according to the oxygen content.

[0036] A waste nitrogen 21 discharge pipeline is installed on the circulating nitrogen pipeline, and the waste nitrogen discharge flow rate is controlled by the outlet pressure of the circulating blower 5 to prevent overpressure in the system.

[0037] The piperazine liquid 20 and the circulating cooling nitrogen are in countercurrent contact granulation.

[0038] The bag filter 2 and the bin dust collector 7 both use low-pressure nitrogen 22 for pulse dust cleaning.

[0039] A cleaning port is provided at the top of the granulation tower 1, and the cleaning liquid 28 can be introduced from the cleaning port to clean the equipment.

[0040] The circulating blower 5 can be installed behind the cooler 4, and the corresponding waste nitrogen 21 discharge pipeline is also installed on the pipeline behind the circulating blower 5, which can reduce the load of the cooler and save energy and reduce consumption.

[0041] A piperazine spray granulation system of the present utility model has a short process, low device investment, the nitrogen in the granulation process can be recycled, high automation and sealing degree, this method is safe, reliable, simple to start up, and can ensure safe production. Preferably, in the system method of the present invention, the circulating blower can also be placed on the outlet pipeline of the high-efficiency filter, and the discharged waste nitrogen is the gas before cooling, which can save energy and reduce consumption.

Claims

1. A piperazine spray granulation system, characterized in that: The described system includes a granulation tower (1), a bag filter (2), and a product silo (6). The material inlet of the granulation tower (1) is connected to a piperazine feed pipe. The material outlet of the granulation tower (1) is connected to the bag filter (2). The product outlet of the bag filter (2) is connected to the product silo (6).

2. The piperazine spray granulation system according to claim 1, characterized in that: A piperazine feed regulating valve (10) is connected to the piperazine feed pipe. A piperazine feed three-way control valve (11) is also connected to the piperazine feed pipe. A low-pressure nitrogen input port is connected to the piperazine feed three-way control valve (11).

3. The piperazine spray granulation system according to claim 1, characterized in that: A nitrogen input port is provided on the granulation tower (1). A nitrogen input pipe is in communication with the nitrogen input port. An electromagnetic valve (14) is connected to the nitrogen input pipe. An oxygen content analyzer (13) is connected to the nitrogen input pipe. A waste nitrogen discharge valve (15) is connected to the nitrogen input pipe.

4. The piperazine spray granulation system according to claim 1, characterized in that: The output port of the granulation tower (1) is provided at the bottom. A cleaning liquid control valve is provided at the top of the granulation tower (1) for controlling the input of the cleaning liquid (28) to clean the interior of the granulation tower (1) through the cleaning liquid (28).

5. The piperazine spray granulation system according to claim 1, characterized in that: An electromagnetic valve (14) is connected to the upper part of the bag filter (2). An electromagnetic valve (14) is connected to the lower part of the bag filter (2). A manual slide valve (8) and a rotary valve (9) are connected to the bottom of the bag filter (2) and are in communication with the product silo (6) through the manual slide valve (8) and the rotary valve (9). The manual slide valve (8) and the rotary valve (9) are connected in series.

6. The piperazine spray granulation system according to claim 1, wherein: The purified gas outlet of the bag filter (2) is connected to the inlet pipe of a high-efficiency filter (3). It is connected to a cooler (4) through the high-efficiency filter (3). The outlet of the cooler (4) is connected to a circulating blower (5). The outlet pipe of the circulating blower (5) is connected to the air inlet on the granulation tower (1).

7. The piperazine spray granulation system according to claim 6, characterized in that: A chilled water supply pipe, a chilled water return pipe, a cooling water inlet pipe, and a cooling water return pipe are connected to the cooler (4).

8. The piperazine spray granulation system according to claim 6, characterized in that: A bin dust collector (7) is fixedly installed at the top of the product silo (6). An electromagnetic valve (14) is installed on the bin dust collector (7). The output interface of the bin dust collector (7) is connected to the high-efficiency filter (3).

9. The piperazine spray granulation system according to claim 1, characterized in that: An electromagnetic valve (14) is provided at the lower part of the product silo (6). A manual slide valve (8) and a rotary valve (9) are connected to the bottom of the product silo (6). The manual slide valve (8) and the rotary valve (9) are connected in series.