Separation and purification system for kathon production

Abstract

This utility model relates to the field of Kathon production technology, and more particularly to a separation and purification system for Kathon production. The system includes a first adsorption device connected to a feed liquid conveying pipeline; the outlet of the first adsorption device is connected to a filtration device; the outlet of the filtration device is connected to an extraction column; the organic phase outlet of the extraction column is connected to a distillation column; the vent of the distillation column is connected to a condensation device; the condensate outlet of the condensation device is connected to a buffer tank; the outlet of the buffer tank is connected to a second adsorption device; the outlet of the second adsorption device is connected to a first resin column; the outlet of the first resin column is connected to a second resin column; the outlet of the second resin column is connected to a crystallization vessel; and the crystal outlet of the crystallization vessel is connected to a drying device. This separation and purification system is rationally designed, achieving the separation and purification of MIT (methyl methacrylate), improving the purity of MIT, and thus ensuring the purity of the Kathon product.

Description

Technical Field

[0001] This utility model relates to the field of Kathon production technology, and in particular to a separation and purification system for Kathon production. Background Technology

[0002] Kathon is a preservative widely used in the preservation and sterilization processes of cosmetics, detergents, coatings, water-based adhesives, inks, dyes, color pastes, printing pastes, leather, industrial circulating water treatment, textiles, and other industries.

[0003] Kathon, a powerful, broad-spectrum, highly efficient, and non-toxic green adjuvant, is considered one of the most promising preservatives internationally. Its main components are isothiazolinone and its inorganic salt stabilizers, typically in a CMI:MIT ratio of 3:1. Kathon's advantage lies in its broad-spectrum antibacterial properties, effectively inhibiting and killing various bacteria, fungi, and yeasts, remaining effective even at low concentrations. Kathon production involves first synthesizing MIT, then synthesizing CMI from MIT, and finally compounding them to obtain the Kathon product. Therefore, the purity of the MIT directly affects the purity of the Kathon product. Currently, however, after MIT synthesis, it may still contain impurities such as water, solvents, unreacted raw materials, byproducts, added stabilizers (such as magnesium nitrate), and metal ions. If these impurities cannot be effectively removed, the purity of the MIT will decrease, inevitably affecting the purity of the Kathon product. Therefore, to address these issues, it is necessary to develop a separation and purification system for Kathon production. Utility Model Content

[0004] The technical problem to be solved by this utility model is to provide a separation and purification system for Kathon production, which greatly improves the purity of Kathon products by addressing the shortcomings of existing technologies.

[0005] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0006] A separation and purification system for Kathon production includes a first adsorption device connected to a feed liquid conveying pipeline. The outlet of the first adsorption device is connected to a filtration device, the outlet of the filtration device is connected to an extraction column, the organic phase outlet of the extraction column is connected to a distillation column, the vent of the distillation column is connected to a condensation device, the condensate outlet of the condensation device is connected to a buffer tank, the outlet of the buffer tank is connected to a second adsorption device, the outlet of the second adsorption device is connected to a first resin column, the outlet of the first resin column is connected to a second resin column, the outlet of the second resin column is connected to a crystallization vessel, and the crystal outlet of the crystallization vessel is connected to a drying device.

[0007] As an improved technical solution, the first adsorption device includes a body, a feed inlet at the top of the body, a diatomaceous earth adsorption layer and an activated carbon adsorption layer inside the body, and a liquid outlet on one side of the lower part of the body.

[0008] As an improved technical solution, the filtration device is a plate and frame filter.

[0009] As an improved technical solution, the extraction tower includes a tower body, a feed pipe on the upper side of the tower body, an extractant inlet pipe on the lower side of the tower body, a light phase outlet at the top of the tower body, and a heavy phase outlet on the bottom side of the tower body; a distributor connected to the feed pipe is provided at the upper part of the interior of the tower body, and multiple layers of distribution plates are provided below the distributor, with multiple through holes on the distribution plates, and a packing layer between adjacent layers of distribution plates.

[0010] As an improved technical solution, the feeder includes a hollow disc body, the bottom of the disc body is provided with multiple feed holes, the periphery of the disc body is provided with multiple feed tubes communicating with the disc body, and the feed tubes are provided with multiple through holes.

[0011] As an improved technical solution, the distillation column includes a column body, a feed pipe on one side of the upper part of the column body, a steam inlet on one side of the lower part of the column body, an vent at the top of the column body, a waste liquid outlet on one side of the bottom of the column body, a feed distribution plate at the top inside the column body, a baffle on the periphery of the feed distribution plate, multiple through holes at the bottom of the feed distribution plate and on the baffle, and multiple packing layers inside the column body, with a perforated baffle between adjacent packing layers.

[0012] As an improved technical solution, the condensation device includes a first condenser, the uncondensed gas outlet of the first condenser is connected to a second condenser, and the condensate outlets of the first condenser and the second condenser are connected to a buffer tank.

[0013] As an improved technical solution, the second adsorption device includes a body, with an inlet at the top and an outlet at the bottom, and an ion exchange fiber adsorption layer and a silica gel adsorption layer inside the body.

[0014] As an improved technical solution, the first resin column is provided with a cationic resin layer.

[0015] As an improved technical solution, the second resin column is provided with an anion exchange resin layer.

[0016] After adopting the above technical solution, the beneficial effects of this utility model are:

[0017] The separation and purification system for Kathon production includes a first adsorption unit connected to a feed liquid conveying pipeline. The outlet of the first adsorption unit is connected to a filtration unit, the outlet of the filtration unit is connected to an extraction tower, the organic phase outlet of the extraction tower is connected to a distillation tower, the vent of the distillation tower is connected to a condensation unit, the condensate outlet of the condensation unit is connected to a buffer tank, the outlet of the buffer tank is connected to a second adsorption unit, the outlet of the second adsorption unit is connected to a first resin column, the outlet of the first resin column is connected to a second resin column, the outlet of the second resin column is connected to a crystallizer, and the crystal outlet of the crystallizer is connected to a drying unit. In actual production, the prepared MIT feed solution is pumped into the first adsorption unit. After adsorption and impurity removal, the solution enters a filtration unit to remove solid impurities. The solution then enters an extraction tower for effective extraction with the extractant. The organic phase containing MIT is then pumped to a distillation tower. After distillation, the MIT vapor is condensed and recovered using a condenser and stored in a buffer tank. It is then pumped to the second adsorption unit for further removal of pigments, organic matter, and other impurities. The solution then enters the first resin column for further removal of metal cations, followed by the second resin column for further removal of anions. Finally, it enters a crystallization vessel for cooling and crystallization. The resulting crystals are then dried in a drying unit. The dried MIT is then used to prepare CMI. Finally, the prepared CMI and MIT are mixed in a specific ratio to obtain a high-purity Kathon product. The above separation and purification system is rationally designed, achieving effective separation and purification of MIT, improving its purity, and thus ensuring the purity of the Kathon product.

[0018] The first adsorption device includes a main body with a feed inlet at the top, a diatomaceous earth adsorption layer and an activated carbon adsorption layer inside, and a liquid outlet on one side of the lower part of the main body. The diatomaceous earth adsorption layer and the activated carbon adsorption layer can effectively remove solid particulate impurities, pigments, organic impurities, and other odor-causing substances.

[0019] The filtration device is a plate and frame filter press. Plate and frame filters can effectively remove insoluble particles and other solid impurities from the liquid.

[0020] The extraction tower comprises a tower body with a feed pipe on one side of the upper part and an extractant inlet pipe on one side of the lower part. The top of the tower has a light phase outlet, and the bottom has a heavy phase outlet. Inside the tower, at the top, is a distributor connected to the feed pipe. Below the distributor are multiple distribution plates with various through-holes, and a packing layer exists between adjacent distribution plates. In actual production, the MIT (Methyl Excipient) feed solution, driven by a pump, enters the distributor through the feed pipe. After being evenly dispersed, it flows downwards through the distribution plates and packing layer under gravity. The extractant, driven by a pump, enters the tower through the extractant inlet pipe and then flows upwards through the distribution plates and packing layer. This thorough contact between the extractant and the MIT feed solution significantly improves the extraction efficiency of MIT.

[0021] The feeder includes a disc body with multiple feed holes at the bottom and multiple feed tubes connected to the disc body on its periphery, each with multiple through holes. Under the action of the delivery pump, the feed liquid enters the disc body through the feed tubes and is evenly dispersed through the feed holes at the bottom of the disc body and on the feed tubes, facilitating full contact with the extractant and promoting complete extraction of MIT.

[0022] The distillation column comprises a column body with a feed pipe on one side of the upper part, a steam inlet on one side of the lower part, an vent at the top, and a waste liquid outlet on one side of the bottom. Inside the column, at the top, is a feed distribution plate surrounded by baffles. Multiple through-holes are present on the bottom of the distribution plate and on the baffles. The column contains multiple layers of packing, with perforated baffles between adjacent packing layers. The extracted MIT feed liquid, driven by a pump, enters the feed distribution plate through the feed pipe, dispersing evenly through the through-holes at the bottom and on the baffles. Hot steam enters the column through the steam inlet. Under gravity, the feed liquid flows downwards through the baffles and packing, while the hot steam flows upwards, exchanging heat with the MIT feed liquid. The MIT vapor exits through the vent and enters a condenser for condensation. This distillation column design is efficient and effectively separates MIT from impurities.

[0023] The condensation unit includes a first condenser, whose uncondensed gas outlet is connected to a second condenser, and whose condensate outlets are connected to a buffer tank. The purified MIT vapor from distillation is condensed in the first and second condensers, collected in the buffer tank, and then proceeds to subsequent processing.

[0024] The second adsorption device includes a main body with an inlet at the top and an outlet at the bottom. The interior of the main body contains an ion exchange fiber adsorption layer and a silica gel adsorption layer. These layers further remove pigments and organic impurities.

[0025] The first resin column contains a cationic resin layer. This cationic resin layer can adsorb metal cations, thereby improving the purity of Kathon products.

[0026] The second resin column contains an anion exchange resin layer. This anion exchange resin layer can adsorb anions, thereby improving the purity of Kathon products. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the separation and purification system for Kathon production according to this utility model;

[0028] Among them, 1-liquid conveying pipeline, 2-first adsorption device, 20-diatomaceous earth adsorption layer, 21-activated carbon adsorption layer, 3-filtration device, 4-extraction tower, 40-distributor, 41-distributor plate, 42-packing layer, 5-distillation tower, 50-plate, 51-baffle, 52-packing layer, 53-baffle plate, 6-condensation device, 60-first cooler, 61-second condenser, 7-buffer tank, 8-second adsorption device, 80-ion exchange fiber adsorption layer, 81-silica gel adsorption layer, 9-first resin column, 10-second resin column, 11-crystallization kettle, 12-drying device. Detailed Implementation

[0029] To make the objectives, technical solutions, and advantages of this utility model clearer, the present utility model will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present utility model and are not intended to limit the present utility model.

[0030] A separation and purification system for Kathon production, such as Figure 1As shown, the device includes a first adsorption unit 2 (comprising a main body with a feed inlet at the top, a diatomaceous earth adsorption layer 20 and an activated carbon adsorption layer 21 inside, and a liquid outlet on one side of the lower part) connected to a feed liquid conveying pipeline 1. The liquid outlet of the first adsorption unit 2 is connected to a filtration unit 3 (plate and frame filter). The liquid outlet of the filtration unit 3 is connected to an extraction tower 4. The organic phase outlet of the extraction tower 4 is connected to a distillation tower 5. The vent of the distillation tower 5 is connected to a condensation unit 6. The condensate outlet of the condensation unit 6 is connected to a buffer tank 7. The liquid outlet of the buffer tank 7 is connected to a second adsorption unit 8 (comprising a main body with a feed inlet at the top and a discharge outlet at the bottom, and an ion exchange layer inside). The ion exchange fiber 80 and silica gel adsorption layer 81 are used, wherein the ion exchange fiber is a strong acid ion exchange fiber that can remove alkaline impurities in MIT. The outlet of the second adsorption device 8 is connected to the first resin column 9. The outlet of the first resin column 9 is connected to the second resin column 10. The outlet of the second resin column 10 is connected to the crystallization vessel (including the vessel body, the outer side of the vessel body is provided with a jacket, the top of the vessel body is provided with a feed port and a crystal inlet, the bottom of the vessel body is provided with a discharge port, the lower side of the vessel body is provided with a mother liquor outlet, the inner wall of the vessel body corresponding to the mother liquor outlet is provided with a filter screen, the inside of the vessel body is provided with a stirrer, one end of the stirrer is connected to a motor) 11. The crystal outlet of the crystallization vessel 11 is connected to the drying device 12 (oven).

[0031] In actual production, the prepared MIT solution is pumped into the first adsorption unit. The diatomaceous earth and activated carbon adsorption layers effectively remove solid particulate impurities, pigments, organic impurities, and other odor-causing substances. After adsorption and impurity removal, the solution enters a filtration unit (plate and frame filter) to remove solid particulate impurities. The solution then enters an extraction tower for effective extraction with an extractant. The organic phase containing MIT is pumped to a distillation tower. After distillation, the MIT vapor is condensed and recovered using a condenser and stored in a buffer tank. It is then pumped to the second adsorption unit, where ion exchange fiber and silica gel adsorption layers further remove pigments and organic impurities. The purified solution then enters the first resin column for further removal of metal cations, followed by the second resin column for further removal of anions. Finally, it enters a crystallization vessel for cooling and crystallization, followed by drying. The dried MIT is then used to prepare CMI. The prepared CMI and MIT are then mixed in a specific ratio to obtain a high-purity Kathon product. The separation and purification system described above is reasonably designed, which enables the separation and purification of MIT, improves the purity of MIT, and thus ensures the purity of Kathon products.

[0032] The extraction tower 4 includes a tower body with a feed pipe on one side of the upper part and an extractant inlet pipe on one side of the lower part. The tower body has a light phase outlet at the top and a heavy phase outlet on one side of the bottom. Inside the tower body, at the top, is a distributor 40 connected to the feed pipe. Below the distributor 40 are multiple distribution plates 41 with multiple through holes. Between adjacent distribution plates 41 are packing layers 42 (Pall ring packing layers). In actual production, the MIT (Methyl Excipient) liquid enters the distributor through the feed pipe under the action of a delivery pump. After being evenly dispersed, it flows downwards through the multiple distribution plates and packing layers under gravity. The extractant enters the tower body through the extractant inlet pipe under the action of a delivery pump, and then flows upwards through the multiple distribution plates and packing layers. The extractant and MIT liquid come into full contact, greatly improving the extraction efficiency of MIT.

[0033] The feeder 40 includes a hollow disc 400 (welded to the inner wall of the tower via a connecting plate). The bottom of the disc has multiple feed holes, and the periphery of the disc has multiple feed pipes 401 connected to the disc 400, each with multiple through holes. Under the action of the delivery pump, the liquid feeds into the disc along the feed pipe, passing through the feed holes at the bottom of the disc and the feed holes on the feed pipes, dispersing evenly to facilitate sufficient contact with the extractant and promote complete extraction of MIT.

[0034] The distillation column 5 includes a column body with a feed pipe on one side of the upper part and a steam inlet pipe on one side of the lower part. The top of the column body has an vent, and the bottom has a waste liquid outlet. Inside the column body, a feed distribution plate 50 (welded to the inner wall of the column body via a connecting plate) is located at the top. A baffle 51 surrounds the feed distribution plate 50. Multiple through holes are located on the bottom of the feed distribution plate 50 and on the baffle 51. The column body contains multiple layers of packing 52 (Pall ring packing layers), with perforated baffles 53 between adjacent packing layers 52. The extracted MIT feed liquid, driven by a pump, enters the feed distribution plate through the feed pipe, dispersing evenly through the through holes at the bottom of the distribution plate and on the baffles. Hot steam enters the column body through the steam inlet pipe. Under gravity, the feed liquid flows downwards through the baffles and packing layers, while the hot steam flows upwards through the baffles and packing layers, achieving heat exchange with the MIT feed liquid. The MIT steam exits through the vent and enters a condenser for condensation. The distillation column with the above structure is reasonably designed and can distill out MIT, achieving effective separation of MIT from impurities.

[0035] The condensation unit 6 includes a first condenser 60 (a shell-and-tube condenser), the uncondensed gas outlet of the first condenser 60 is connected to a second condenser 61 (a shell-and-tube condenser), and the condensate outlets of the first condenser 60 and the second condenser 61 are connected to a buffer tank 7. The MIT vapor obtained from distillation is condensed by the first and second condensers, collected in the buffer tank, and then sent to subsequent processing.

[0036] The first resin column 9 contains a cation exchange resin layer (specifically, a 001×7 type strong acid styrene-based cation exchange resin). This cation exchange resin layer adsorbs metal cations, thereby improving the purity of the Kathon product.

[0037] The second resin column 10 contains an anion exchange resin layer (specifically, a 201×7 type strong base styrene-based anion exchange resin). This anion exchange resin layer adsorbs anions, thereby improving the purity of the Kathon product.

[0038] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. A separation and purification system for kava production, characterized by, The system includes a first adsorption device connected to a feed liquid conveying pipeline; the outlet of the first adsorption device is connected to a filtration device; the outlet of the filtration device is connected to an extraction tower; the organic phase outlet of the extraction tower is connected to a distillation tower; the vent of the distillation tower is connected to a condensation device; the condensate outlet of the condensation device is connected to a buffer tank; the outlet of the buffer tank is connected to a second adsorption device; the outlet of the second adsorption device is connected to a first resin column; the outlet of the first resin column is connected to a second resin column; the outlet of the second resin column is connected to a crystallization vessel; and the crystal outlet of the crystallization vessel is connected to a drying device.

2. The separation and purification system for producing a casone according to claim 1, wherein, The first adsorption device includes a body, with a feed inlet at the top of the body, a diatomaceous earth adsorption layer and an activated carbon adsorption layer inside the body, and a liquid outlet on one side of the lower part of the body.

3. The separation and purification system for producing a casone according to claim 1, characterized by, The filtration device is a plate and frame filter.

4. The separation and purification system for producing a cardanol according to claim 1, characterized by, The extraction tower includes a tower body, with a feed pipe on one side of the upper part of the tower body and an extractant inlet pipe on one side of the lower part of the tower body. The top of the tower body has a light phase outlet, and the bottom of the tower body has a heavy phase outlet. Inside the tower body, at the top, there is a distributor connected to the feed pipe. Below the distributor, there are multiple layers of distribution plates with multiple through holes. Between two adjacent layers of distribution plates, there is a packing layer.

5. The separation and purification system for producing a casone according to claim 4, wherein The fabric feeder includes a hollow disc body with multiple fabric feeding holes at the bottom and multiple fabric feeding tubes connected to the disc body on the periphery, with multiple through holes on the fabric feeding tubes.

6. The separation and purification system for producing a casone according to claim 1, wherein, The distillation column includes a column body, a feed pipe on one side of the upper part of the column body, a steam inlet on one side of the lower part of the column body, an vent at the top of the column body, a waste liquid outlet on one side of the bottom of the column body, a feed distribution plate at the top inside the column body, a baffle on the periphery of the feed distribution plate, multiple through holes at the bottom of the feed distribution plate and on the baffle, and multiple packing layers inside the column body, with a perforated baffle between adjacent packing layers.

7. The separation and purification system for Kathon production according to claim 1, characterized in that, The condensation device includes a first condenser, the uncondensed gas outlet of the first condenser is connected to a second condenser, and the condensate outlets of the first condenser and the second condenser are connected to a buffer tank.

8. The separation and purification system for producing a casone according to claim 1, wherein, The second adsorption device includes a body, with an inlet at the top and an outlet at the bottom. The interior of the body contains an ion exchange fiber adsorption layer and a silica gel adsorption layer.

9. The separation and purification system for producing a casone according to claim 1, characterized by, The first resin column contains a cationic resin layer.

10. The separation and purification system for producing a casone according to claim 1, wherein, The second resin column contains an anion exchange resin layer.

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