Recycling device for catalyst urotropine in production of glycine

By designing a recycling and processing device including pretreatment and separation devices, the problem of difficult recovery of catalyst Ulotropine in the aminoacetic acid production process is solved, and the effective recycling and reuse of catalysts is achieved, reducing production costs and improving production efficiency.

CN222956203UActive Publication Date: 2025-06-10HENAN HDF CHEM CO LTD
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Patent Information

Application Number
CN202422156854.0
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-09-04
Publication Date
2025-06-10
Estimated Expiration
2034-09-04

AI Technical Summary

Technical Problem

During the production process of aminoacetic acid, the catalyst Ulotropine is difficult to recycle, resulting in high cost consumption and affecting the quality of by-products.

Method used

A recycling and processing device including a pretreatment device and a separation device is designed. The aminoacetic acid mother liquor is pretreated through a plate-frame filtration device and an ultrafiltration device, and then the catalyst ulotropine is separated out by three-stage nanofiltration treatment.

Benefits of technology

Effective recycling and reuse of the catalyst Ulotropine reduces production costs, improves the production efficiency of aminoacetic acid, and solves the problem of difficult catalyst recycling.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses a recovery processing device for a catalyst urotropine in glycine production, which comprises a pretreatment device and a separation device, the pretreatment device comprises a plate frame filter device and an ultrafiltration device, the plate frame filter device is connected with the ultrafiltration device, and the ultrafiltration device is connected with the separation device; a feeding pipeline is connected to a feeding hole of the plate-and-frame filtering device, an ultrafiltration standby tank is connected to a discharging hole of the plate-and-frame filtering device, an ultrafiltration device is connected to the ultrafiltration standby tank, and a separating device is connected to the ultrafiltration device; the separation device comprises a first-stage nanofiltration device, a second-stage nanofiltration device and a third-stage nanofiltration device which are the same in structure; in general, the device has the advantages of multi-stage separation, recycling, cost saving and production efficiency improvement.
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Description

Technical Field

[0001] The utility model belongs to the technical field of chemical equipment, and particularly relates to a recovery and treatment device for hexamine, a catalyst in the production of glycine. Background Technique

[0002] Glycine, commonly known as glycine and gum sugar, is mainly used for non-toxic decarbonization of chemical fertilizers, medicine and pesticides. It is one of the raw materials for the synthesis of glyphosate by the alkyl ester method, and can also be used as a raw material and preservative for cosmetics. It has a relatively wide market and application prospects. At present, the domestic synthesis of glycine mainly adopts the chloroacetic acid ammoniation method, using an aqueous solution of hexamine as a catalyst, synthesizing in the aqueous or alcoholic phase at normal temperature and pressure, and then obtaining the product glycine through alcohol precipitation, filtration, refining and drying.

[0003] Among them, hexamine, also known as hexamethylenetetramine, has a structural formula of C6H12N4. It is mainly used as a curing agent for resins and plastics, a catalyst and foaming agent for amino plastics, an accelerator for rubber vulcanization (accelerator H), an anti-shrinking agent for textiles, etc. In the production process of glycine, hexamine participates in the synthesis process of glycine as a catalyst and finally enters the glycine mother liquor, making it difficult to recycle. Most of it enters the by-product ammonium chloride. Due to the increasing domestic demand for glycine, the production of glycine has been promoted, the consumption of the catalyst hexamine has also been increasing, the cost has been increasing day by day, and at the same time, the quality of the by-product has been affected.

[0004] Therefore, to solve the above problems, it is necessary to develop a recovery and treatment device for hexamine, a catalyst in the production of glycine. Content of the Utility Model

[0005] The purpose of the utility model is to overcome the deficiencies of the prior art and provide a recovery and treatment device for hexamine, a catalyst in the production of glycine, so as to solve the problems of difficult recovery of the catalyst hexamine and high cost consumption in the production process of glycine.

[0006] The purpose of the utility model is achieved as follows: A recovery and treatment device for hexamine, a catalyst in the production of glycine, includes a pretreatment device and a separation device. Among them, the pretreatment device includes a plate-and-frame filtration device and an ultrafiltration device. The plate-and-frame filtration device is connected to the ultrafiltration device, and the ultrafiltration device is connected to the separation device;

[0007] Among them, a feed pipeline is connected to the feed inlet of the plate-and-frame filtration device. The discharge outlet of the plate-and-frame filtration device is connected to an ultrafiltration standby tank through a discharge pipeline. The ultrafiltration standby tank is connected to the ultrafiltration device through a connecting pipeline. The ultrafiltration device includes a plurality of ultrafiltration components with independent inlet and outlet ports. An ultrafiltration membrane is arranged inside the ultrafiltration components. The discharge outlet of the ultrafiltration device is connected to the separation device through a pipeline;

[0008] The separation device includes a first-stage nanofiltration device, a second-stage nanofiltration device, and a third-stage nanofiltration device. The first-stage nanofiltration device, the second-stage nanofiltration device, and the third-stage nanofiltration device have the same structure and each includes a plurality of nanofiltration components with independent inlet and outlet ports. A nanofiltration membrane is arranged inside the nanofiltration component.

[0009] The inlet of the first-stage nanofiltration device is connected to the ultrafiltration device. The concentrated material generated by the first-stage nanofiltration device enters the second-stage nanofiltration device through a first-stage concentrated material pipeline, and the light material generated by the first-stage nanofiltration device enters the third-stage nanofiltration device through a first-stage light material pipeline.

[0010] The concentrated material generated by the second-stage nanofiltration device enters the storage tank through a second-stage concentrated material pipeline, and the light material generated by the second-stage nanofiltration device enters the third-stage nanofiltration device through a second-stage light material pipeline.

[0011] The concentrated material generated by the third-stage nanofiltration device enters the ultrafiltration spare tank through a third-stage concentrated material pipeline, and the light material generated by the third-stage nanofiltration device enters the finished product spare tank through a third-stage light material pipeline.

[0012] Further, the plate-and-frame filtration device includes a plate-and-frame support. A plurality of filter plates are arranged on the plate-and-frame support. The filter plates are arranged in a cuboid structure with a hollow middle. Filter cloths are installed on the filter plates. Two discharge ports are respectively arranged on both sides of the filter plates. A material converging groove is arranged below the filter plates on the plate-and-frame support. A fixing plate and a pressing plate are respectively arranged on both sides of the filter plates. The pressing plate is slidably arranged on the plate-and-frame support through pulleys. The pressing plate is connected to a hydraulic device through a pressing rod, and the hydraulic device pushes the pressing plate to press the filter plates.

[0013] Further, the filter cloth on the filter plate is made of polytetrafluoroethylene filter cloth, and the pore diameter of the filter cloth is 600 - 800 meshes.

[0014] Further, a pressure gauge is installed on the hydraulic device, and the hydraulic device is connected to an oil tank through an oil pump.

[0015] Further, the ultrafiltration membrane is made of a polytetrafluoroethylene membrane with a pore diameter of 0.01 microns.

[0016] Further, the nanofiltration membrane is made of a polytetrafluoroethylene RO reverse osmosis membrane with a pore diameter of 1 - 2 nanometers.

[0017] Further, a feed pump is arranged on the feed pipeline, a high-pressure pump is arranged on the connection pipeline, and pressure gauges, liquid flow meters, and solenoid valves are arranged on both the feed pipeline and the connection pipeline.

[0018] Further, a first-stage nanofiltration standby tank, a second-stage nanofiltration standby tank, and a third-stage nanofiltration standby tank are respectively connected to the inlets of the first-stage nanofiltration device, the second-stage nanofiltration device, and the third-stage nanofiltration device through connecting pipelines.

[0019] Further, the inlet of the first-stage nanofiltration standby tank is connected to the outlet of the ultrafiltration device, and the outlet of the first-stage nanofiltration standby tank is connected to the inlet of the first-stage nanofiltration device; the inlet of the second-stage nanofiltration standby tank is connected to the concentrated material outlet of the first-stage nanofiltration device through a first-stage concentrated material pipeline, and the outlet of the second-stage nanofiltration standby tank is connected to the inlet of the second-stage nanofiltration device; the inlet of the third-stage nanofiltration standby tank is connected to the light material outlet of the first-stage nanofiltration device and the light material outlet of the second-stage nanofiltration device through a first-stage light material pipeline and a second-stage light material pipeline respectively, and the outlet of the third-stage nanofiltration standby tank is connected to the inlet of the third-stage nanofiltration device.

[0020] The beneficial effects of the present utility model are as follows: In the present utility model, the aminoacetic acid mother liquor is pretreated by a plate and frame filtration device and an ultrafiltration device, and then subjected to three-stage nanofiltration treatment, so that the catalyst hexamethylenetetramine can be effectively separated out and continue to be used in the production of aminoacetic acid, saving costs and having high utilization rate, effectively solving the problems of difficult recovery of the catalyst hexamethylenetetramine and large cost consumption during the production of aminoacetic acid; generally, the present utility model has the advantages of multi-stage separation, recycling, cost saving, and production efficiency improvement. Description of the Drawings

[0021] Figure 1 is a structural schematic diagram of the present utility model.

[0022] Figure 2 is a structural schematic diagram of the plate and frame filtration device in the present utility model.

[0023] In the figure: 1. Pretreatment device 2. Separation device;

[0024] 11. Plate and frame filtration device 12. Ultrafiltration device 13. Ultrafiltration standby tank;

[0025] 11a. Plate and frame support 11b. Filter plate 11c. Material converging groove 11d. Fixed plate 11e. Extrusion plate 11f. Extrusion rod 11g. Hydraulic device 11h. Oil tank;

[0026] 21. First-stage nanofiltration device 22. Second-stage nanofiltration device 23. Third-stage nanofiltration device 24. Storage tank 25. Finished product standby tank 26. First-stage nanofiltration standby tank 27. Second-stage nanofiltration standby tank 28. Third-stage nanofiltration standby tank;

[0027] 01. Feed pipeline 02. Discharge pipeline 03. Connecting pipeline 04. Primary concentrated material pipeline 05. Primary dilute material pipeline 06. Secondary concentrated material pipeline 07. Secondary dilute material pipeline 08. Tertiary concentrated material pipeline 09. Tertiary dilute material pipeline;

[0028] a. Feed pump b. High-pressure pump c. Pressure gauge d. Liquid flowmeter e. Solenoid valve. Specific implementation mode

[0029] The technical solution of the present utility model will be further specifically described below with reference to the accompanying drawings.

[0030] As Figure 1 、 Figure 2 shown, a recovery and treatment device for the catalyst hexamine when producing glycine includes a pretreatment device 1 and a separation device 2; wherein, the pretreatment device 1 includes a plate-frame filtration device 11 and an ultrafiltration device 12, the plate-frame filtration device 11 is connected to the ultrafiltration device 12, and the ultrafiltration device 12 is connected to the separation device 2.

[0031] Among them, the plate-frame filtration device 11 is used to remove crystals and a small amount of granular impurities in the glycine mother liquor. Specifically, a feed pipeline 01 is connected to the feed port of the plate-frame filtration device 11, and an ultrafiltration standby tank 13 is connected to the discharge port of the plate-frame filtration device 11 through a discharge pipeline 02. The discharge port of the ultrafiltration standby tank 13 is connected to the ultrafiltration device 12 through a connecting pipeline 03; a feed pump a, a pressure gauge c, a liquid flowmeter d, and a solenoid valve e are provided on the feed pipeline 01.

[0032] Preferably, the plate-frame filtration device 11 includes a plate-frame support 11a, a plurality of filter plates 11b are provided on the plate-frame support 11a, the filter plates 11b are arranged in a cuboid structure with a hollow middle, filter cloth is installed on the filter plates 11b, the filter cloth can adopt polytetrafluoroethylene filter cloth, the pore size of the filter cloth is 600-800 meshes, two discharge ports are provided on each of the filter plates 11b and are located on both sides of the filter plates 11b respectively, a material converging groove 11c is provided on the plate-frame support 11a below the filter plates 11b, a fixing plate 11d and a pressing plate 11e are respectively provided on both sides of the filter plates 11b, the pressing plate 11e is slidably arranged on the plate-frame support 11a through a pulley, the pressing plate 11e is connected to a hydraulic device 11g through a pressing rod 11f, the hydraulic device 11g pushes the pressing plate 11e to press the filter plates 11b, a pressure gauge c is installed on the hydraulic device 11g, the hydraulic device 11g is connected to an oil tank 11h through an oil pump, the oil tank 11h is arranged in a cuboid structure, and a solenoid valve is also provided on the oil tank 11h.

[0033] Among them, the ultrafiltration device 12 is used to further process the material after plate-and-frame filtration, remove small particle impurities in the material, and then separate hexamine; specifically, the ultrafiltration device 12 includes a plurality of ultrafiltration components with independent inlet and outlet ports, and an ultrafiltration membrane is arranged inside the ultrafiltration components. Preferably, the ultrafiltration membrane is a polytetrafluoroethylene membrane with a pore size of 0.01 micrometers. The outlet of the ultrafiltration device 12 is connected to a separation device 2 through a connecting pipe 03, and the inlet and outlet ports of the plurality of ultrafiltration components are respectively connected to the connecting pipe 03 and the pipe at the outlet of the ultrafiltration device 12.

[0034] Among them, the main equipment of the separation device 2 is a nanofiltration device, which separates hexamine by the difference in the molecular weights of the components in the material. Specifically, a multi-stage nanofiltration device is used for separation to recycle most of the hexamine; specifically, the separation device 2 includes a first-stage nanofiltration device 21, a second-stage nanofiltration device 22, and a third-stage nanofiltration device 23. The first-stage nanofiltration device 21, the second-stage nanofiltration device 22, and the third-stage nanofiltration device 23 have the same structure and each includes a plurality of nanofiltration components with independent inlet and outlet ports. A nanofiltration membrane is arranged inside the nanofiltration components. Preferably, the nanofiltration membrane is a polytetrafluoroethylene RO reverse osmosis membrane with a pore size of 1-2 nanometers.

[0035] Among them, the inlet of the first-stage nanofiltration device 21 is connected to the outlet of the ultrafiltration device 12. The concentrated material generated by the first-stage nanofiltration device 21 enters the second-stage nanofiltration device 22 through a first-stage concentrated material pipe 04, and the light material generated by the first-stage nanofiltration device 21 enters the third-stage nanofiltration device 23 through a first-stage light material pipe 05.

[0036] The concentrated material generated by the second-stage nanofiltration device 22 enters a storage tank 24 through a second-stage concentrated material pipe 06. Here, the concentrated material generated by the second-stage nanofiltration device 22 is a concentrated glycine mother liquor, which enters the storage tank for further processing. The light material generated by the second-stage nanofiltration device 22 enters the third-stage nanofiltration device 23 through a second-stage light material pipe 07.

[0037] The concentrated material generated by the third-stage nanofiltration device 23 enters an ultrafiltration spare tank 13 through a third-stage concentrated material pipe 08 for continuous separation; the light material generated by the third-stage nanofiltration device 23 enters a finished product spare tank 25 through a third-stage light material pipe 09. The light material generated by the third-stage nanofiltration device 23 is the separated hexamine solution, which enters the spare tank 25 and can be reused as a catalyst for glycine production to achieve recycling.

[0038] Among them, the feed inlets of the first-stage nanofiltration device 21, the second-stage nanofiltration device 22, and the third-stage nanofiltration device 23 are respectively connected with a first-stage nanofiltration standby tank 26, a second-stage nanofiltration standby tank 27, and a third-stage nanofiltration standby tank 28 through connecting pipelines 03; preferably, a high-pressure pump b, a pressure gauge c, a liquid flowmeter d, and a solenoid valve e are arranged on the connecting pipeline 03.

[0039] Specifically, the feed inlet of the first-stage nanofiltration standby tank 26 is connected to the discharge outlet of the ultrafiltration device 12, and the discharge outlet of the first-stage nanofiltration standby tank 26 is connected to the feed inlet of the first-stage nanofiltration device 21 through the connecting pipeline 03; the feed inlet of the second-stage nanofiltration standby tank 27 is connected to the concentrated material outlet of the first-stage nanofiltration device 21 through a first-stage concentrated material pipeline 04, and the discharge outlet of the second-stage nanofiltration standby tank 27 is connected to the feed inlet of the second-stage nanofiltration device 22 through the connecting pipeline 03; the feed inlet of the third-stage nanofiltration standby tank 28 is connected to the light material outlet of the first-stage nanofiltration device 21 and the light material outlet of the second-stage nanofiltration device 22 respectively through a first-stage light material pipeline 05 and a second-stage light material pipeline 07, and the discharge outlet of the third-stage nanofiltration standby tank 28 is connected to the feed inlet of the third-stage nanofiltration device 23.

[0040] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A recovery and treatment device for the catalyst urotropine when producing glycine, characterized in that: Comprising a pretreatment device (1) and a separation device (2), wherein the pretreatment device (1) comprises a plate-and-frame filter device (11) and an ultrafiltration device (12), the plate-and-frame filter device (11) is connected to the ultrafiltration device (12), and the ultrafiltration device (12) is connected to the separation device (2); The feed port of the plate-and-frame filter device (11) is connected to a feed pipe (01), the discharge port of the plate-and-frame filter device (11) is connected to an ultrafiltration standby tank (13) via a discharge pipe (02), the ultrafiltration standby tank (13) is connected to an ultrafiltration device (12) via a connecting pipe (03), the ultrafiltration device (12) comprises a plurality of ultrafiltration components with independent feed ports, ultrafiltration membranes are arranged inside the ultrafiltration components, and the discharge port of the ultrafiltration device (12) is connected to a separation device (2) via a pipe; The separation device (2) comprises a primary nanofiltration device (21), a secondary nanofiltration device (22) and a tertiary nanofiltration device (23); the primary nanofiltration device (21), the secondary nanofiltration device (22) and the tertiary nanofiltration device (23) have the same structure and each comprises a plurality of nanofiltration components with independent inlet and outlet ports; a nanofiltration membrane is disposed inside the nanofiltration component; The feed port of the first-stage nanofiltration device (21) is connected to the ultrafiltration device (12); the concentrated material produced by the first-stage nanofiltration device (21) enters the second-stage nanofiltration device (22) through the first-stage concentrated material pipeline (04); the dilute material produced by the first-stage nanofiltration device (21) enters the third-stage nanofiltration device (23) through the first-stage dilute material pipeline (05); The concentrated material produced by the secondary nanofiltration device (22) enters the storage tank (24) through the secondary concentrated material pipeline (06), and the dilute material produced by the secondary nanofiltration device (22) enters the tertiary nanofiltration device (23) through the secondary dilute material pipeline (07). The concentrated material produced by the three-stage nanofiltration device (23) enters the ultrafiltration standby tank (13) through the three-stage concentrated material pipeline (08), and the dilute material produced by the three-stage nanofiltration device (23) enters the finished product standby tank (25) through the three-stage dilute material pipeline (09).

2. The device for recovering and treating the catalyst urotropine when producing glycine according to claim 1, characterized in that: The plate-and-frame filter device (11) comprises a plate-and-frame support (11a), a plurality of filter plates (11b) being arranged on the plate-and-frame support (11a), the filter plates (11b) being arranged in a rectangular parallelepiped structure with a hollow center, filter cloth being mounted on the filter plates (11b), two discharge ports being arranged on the filter plates (11b) and being respectively located on both sides of the filter plates (11b), a material convergence trough (11c) being arranged on the plate-and-frame support (11a) below the filter plates (11b), a fixing plate (11d) and an extrusion plate (11e) being respectively arranged on both sides of the filter plates (11b), the extrusion plates (11e) being slidably arranged on the plate-and-frame support (11a) via pulleys, the extrusion plates (11e) being connected to a hydraulic device (11g) via an extrusion rod (11f), the hydraulic device (11g) pushing the extrusion plates (11e) to press the filter plates (11b).

3. The recovery and processing device for the catalyst urotropine when producing glycine according to claim 2, characterized in that: The filter cloth on the filter plate (11b) is made of polytetrafluoroethylene filter cloth, and the pore size of the filter cloth is 600-800 meshes.

4. The recovery and processing device for the catalyst urotropine when producing glycine according to claim 2, characterized in that: A pressure gauge (c) is installed on the hydraulic device (11g), and the hydraulic device (11g) is connected to an oil tank (11h) via an oil pump.

5. The recovery and processing device for the catalyst urotropine used in the production of glycine according to claim 1, characterized in that: The ultrafiltration membrane adopts a polytetrafluoroethylene membrane with a pore size of 0.01 micron.

6. The recovery and processing device for the catalyst urotropine used in the production of glycine according to claim 1, characterized in that: The nanofiltration membrane adopts a polytetrafluoroethylene RO reverse osmosis membrane with a pore size of 1-2 nanometers.

7. The recovery and processing device for the catalyst urotropine used in the production of glycine according to claim 1, characterized in that: The feed pipeline (01) is provided with a feed pump (a), the connecting pipeline (03) is provided with a high-pressure pump (b), and the feed pipeline (01) and the connecting pipeline (03) are both provided with a pressure gauge (c), a liquid flow meter (d) and a solenoid valve (e).

8. The device for recovering and treating the catalyst urotropine when producing glycine according to claim 1, characterized in that: The feed inlets of the first-stage nanofiltration device (21), the second-stage nanofiltration device (22) and the third-stage nanofiltration device (23) are respectively connected to a first-stage nanofiltration standby tank (26), a second-stage nanofiltration standby tank (27) and a third-stage nanofiltration standby tank (28) via connecting pipes (03).

9. The device for recovering and treating the catalyst urotropine when producing glycine according to claim 8, characterized in that: The feed port of the first-stage nanofiltration standby tank (26) is connected to the discharge port of the ultrafiltration device (12), and the discharge port of the first-stage nanofiltration standby tank (26) is connected to the feed port of the first-stage nanofiltration device (21); the feed port of the second-stage nanofiltration standby tank (27) is connected to the concentrated material outlet of the first-stage nanofiltration device (21) via the first-stage concentrated material pipeline (04), and the discharge port of the second-stage nanofiltration standby tank (27) is connected to the feed port of the second-stage nanofiltration device (22); the feed port of the third-stage nanofiltration standby tank (28) is connected to the dilute material outlet of the first-stage nanofiltration device (21) and the dilute material outlet of the second-stage nanofiltration device (22) via the first-stage dilute material pipeline (05) and the second-stage dilute material pipeline (07), respectively, and the discharge port of the third-stage nanofiltration standby tank (28) is connected to the feed port of the third-stage nanofiltration device (23).