CN212269953U - Nylon 6 melt devolatilization reaction kettle and devolatilization device - Google Patents
Nylon 6 melt devolatilization reaction kettle and devolatilization device Download PDFInfo
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- CN212269953U CN212269953U CN202020255003.0U CN202020255003U CN212269953U CN 212269953 U CN212269953 U CN 212269953U CN 202020255003 U CN202020255003 U CN 202020255003U CN 212269953 U CN212269953 U CN 212269953U
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Abstract
The utility model relates to the field of nylon materials, and discloses a devolatilization reaction kettle and a devolatilization device for nylon 6 melt, wherein the devolatilization reaction kettle for nylon 6 melt comprises a shell, a hollow rotating shaft, a motor and at least one devolatilization disc; the bottom of the shell is provided with a melt inlet and a melt outlet, the middle part of the side surface of the shell is provided with a gas inlet, and the top of the shell is provided with a gas outlet; the hollow rotating shaft is horizontally arranged in the shell, one end of the hollow rotating shaft is communicated with the gas inlet, and the motor is used for driving the hollow rotating shaft to rotate; the devolatilization discs are communicated with the hollow rotating shaft, and when the devolatilization discs are multiple, the multiple devolatilization discs are sequentially arranged on the hollow rotating shaft in parallel; the devolatilization disc is distributed with air holes. The utility model discloses can carry out the high efficiency to the nylon 6 fuse-element and take off and wave, and can take off and wave the in-process and make the condensation polymerization of nylon 6 obtain inhibiting, avoid the sudden strain of a muscle of nylon 6 molecular weight under vacuum condition and influence the spinning forming process, also provide the time for nylon 6 amide exchange, make molecular weight distribution narrow down, improved the fuse-element quality.
Description
Technical Field
The utility model relates to a nylon materials field especially relates to a6 fuse-elements of nylon take off and wave reation kettle and take off and wave the device.
Background
The conversion of hydrolytic polymerization of caprolactam is typically around 90%, meaning that around 10% of caprolactam monomer and oligomer (also known as hot water extractables, where monomer is about 75% and oligomer is about 25%) remain in the polymer, and these impurities in the melt have a significant impact on spinning. Therefore, before the spinning of PA6, the chips need to be subjected to extraction treatment, and according to FZ/T51004-2011, the hot water extractables content of the PA6 chips is less than 0.5wt% (superior products). At present, the hot water continuous extraction process is widely adopted in industry to extract monomers and oligomers in PA6 chips, so that the content of extractables in the chips is lower than 0.5wt%, and the requirement of high-speed spinning is met. However, a large amount of water and energy are consumed in the extraction, drying and remelting processes, and according to statistics, in the production process of PA6 slices, the energy consumption in the extraction and drying processes accounts for 15-20% of that in the production process of PA6 slices, so that the production cost of PA6 fibers is greatly increased. In order to avoid the defects, the PA6 spinning technology is pushed to the direction of direct spinning in the future, and compared with the spinning by a slicing method, the melt direct spinning technology can greatly simplify the production flow, has low capital investment per unit yield and is beneficial to further reducing the production cost of fibers.
The main method for reducing the hot water extractable content in the caprolactam hydrolysis polymerization process is to control the polymerization temperature, because the caprolactam polymerization is a balance relation which changes along with the temperature change, and the hot water extractable content is more favorably generated along with the temperature rise, especially cyclic oligomer, so that the hot water extractable content can be effectively controlled by controlling the polymerization temperature, namely low-temperature polymerization. In order to ensure that the polymerization process is carried out in a liquid state, the polymerization temperature is required to be at least 10 ℃ below the melting point of nylon 6, the polymerization temperature can not control the hot water extractables in the range of direct spinning by a fusible body, and the low-temperature polymerization has another defect that the reaction speed is slow, and the molecular weight of the obtained polymer is low; spinning fibres from low temperature polymers requires that the polymer be raised to processing temperature, however, since the reaction is in chemical equilibrium and forms low molecular weight compounds, there is no advantage over normal polymerisation processes and therefore other processes are necessary to reduce the hot water extractables content of the melt.
The applicant found that in the previous studies, under certain devolatilization conditions, the monomer in the nylon 6 melt can be effectively removed, and in the process, the removal of the monomer can also drive other oligomers, especially cyclic dimer, to sublimate and be removed from the melt, thereby providing a way for reducing the content of hot water extractables in the nylon 6 melt. However, to achieve a large amount of hot water extractables removal requires a high devolatilization area and vacuum in the apparatus, and at this high devolatilization efficiency, the molecular weight of nylon 6 rapidly increases and the melt viscosity increases greatly, resulting in molding difficulties. In addition, how to collect the volatile, avoid the pipeline to block up to effective retrieval and utilization volatile also influences PA6 production efficiency. Therefore, the development of a special devolatilization device for nylon 6 is a trend of development of the nylon 6 industry, so that the content of hot water extractables in a nylon 6 melt is reduced, and the high-efficiency recycling of the hot water extractables is realized.
SUMMERY OF THE UTILITY MODEL
In order to solve the technical problem, the utility model provides a nylon 6 fuse-element takes off and waves reation kettle and takes off and wave the device, the utility model discloses a take off and wave reation kettle not only can improve and take off and wave efficiency, can avoid the sudden rise of nylon 6 molecular weight and influence spinning forming process under vacuum condition simultaneously, also provide the time for nylon 6 amide exchange, make molecular weight distribution narrow down, improved the fuse-element quality.
The utility model discloses a concrete technical scheme does:
in a first aspect, the utility model provides a nylon 6 melt devolatilization reaction kettle, which comprises a shell, a hollow rotating shaft, a motor and at least one devolatilization disc; the bottom of the shell is provided with a melt inlet and a melt outlet, the middle part of the side surface of the shell is provided with a gas inlet, and the top of the shell is provided with a gas outlet; the hollow rotating shaft is horizontally arranged in the shell, one end of the hollow rotating shaft is communicated with the gas inlet, and the motor is used for driving the hollow rotating shaft to rotate; the devolatilization discs are communicated with the hollow rotating shaft, and when the devolatilization discs are multiple, the multiple devolatilization discs are sequentially arranged on the hollow rotating shaft in parallel; the devolatilization disc is distributed with air holes.
The utility model discloses devolatilizing reation kettle's theory of operation does: the nylon 6 melt enters the devolatilization reaction kettle through a melt inlet, wet nitrogen is introduced from a gas inlet, a hollow rotating shaft drives a devolatilization disc to rotate (the rotating devolatilization disc can take up the nylon 6 melt at the bottom of the devolatilization disc (the melt is attached to the surface of the devolatilization disc to form a layer of film), an external heating device heats the devolatilization reaction kettle, the external vacuum device vacuumizes the devolatilization reaction kettle, under the conditions, the nylon 6 melt is adhered to the surface of the devolatilization disc, and the flow path of the wet nitrogen is from the hollow rotating shaft → a hollow branch pipe → the devolatilization disc, in the process, the hot nitrogen containing trace moisture is blown out of the devolatilization disc through air holes, so that the nylon 6 melt attached to the devolatilization disc is bubbled to form a thinner melt film, the devolatilization area can be further increased, the devolatilization efficiency is improved, and the melt bubbles can be broken when being increased to a certain degree, the gas is carried away from the system under vacuum. In addition, as the cyclic dimer and other nonvolatile components have better solubility in hot water, the moisture in the hot nitrogen gas flow can interact with the cyclic dimer and other nonvolatile components, the cyclic dimer and other nonvolatile components can be driven to volatilize, the content of the nonvolatile components in the melt is reduced, the content of oligomers in the melt is further reduced, and the quality of the melt is improved. Finally, gas containing the devolatilized components is discharged from a gas outlet, and the devolatilized nylon 6 melt flows out from a melt outlet, the hot water extractables content of the obtained nylon 6 melt is less than or equal to 1.5wt%, wherein the cyclic dimer content is less than or equal to 0.3 wt%, and the nylon 6 melt can be directly spun or directly made into plastic products.
To the best of the applicant's knowledge, the existing techniques for nylon 6 melt are all hot water extraction devolatilization, and there is no nylon 6 devolatilization system similar to the above working principle of the present invention. As described in the background of the present application, in the conventional devolatilization process, a device with a high devolatilization area and a high vacuum degree are required, and under the high devolatilization, the molecular weight of nylon 6 can be rapidly increased, and the melt viscosity is greatly increased, so that the molding is difficult. And the utility model discloses take off and wave the advantage of system and lie in: because the system contains a certain amount of water, the polycondensation reaction of the nylon 6 is inhibited, the phenomenon that the molecular weight of the nylon 6 swells under the vacuum condition to influence the spinning forming process is avoided, time is provided for the amide exchange of the nylon 6, the molecular weight distribution is narrowed, and the melt quality is improved. In addition, as the cyclic dimer and other nonvolatile components have better solubility in hot water, the moisture in the hot nitrogen gas flow can interact with the cyclic dimer and other nonvolatile components, the cyclic dimer and other nonvolatile components can be driven to volatilize, the content of the nonvolatile components in the melt is reduced, the content of oligomers in the melt is further reduced, and the quality of the melt is improved.
Preferably, the devolatilization disc is fixed on the hollow rotating shaft through a hollow branch pipe communicated with the hollow rotating shaft and is communicated with the hollow rotating shaft.
Preferably, the diameter of the air hole of the devolatilization reaction kettle is 0.1-10 mm.
The diameter of the air hole is limited within the range of 0.1-10mm, the air hole can be adjusted according to the viscosity of the melt in actual production, attention needs to be paid to avoid the melt from flowing into the air hole when the diameter is designed, and meanwhile, the resistance of the melt flowing on the devolatilization disc is reduced.
In a second aspect, the utility model provides a devolatilization device, which comprises a devolatilization system and a component collection system which are connected in sequence.
The devolatilization system comprises a plurality of devolatilization reaction kettles which are connected in series and/or in parallel; the gas outlet of the devolatilization reaction kettle is connected with a component collecting system; the component collection system includes a low boiling point component removal unit.
It should be noted that, for a plurality of devolatilization reaction kettles connected in series, only the devolatilization reaction kettle positioned at the foremost end is introduced with a nitrogen gas flow containing moisture, and for the devolatilization reaction kettle at the rear end, no gas is introduced, only vacuum pumping is performed, and the action is relatively short, so as to further remove the volatiles, and simultaneously remove the moisture in the system, so as to meet the spinning requirement.
Component collection system: hot water extractables removed from the melt are mixed with gas, then are introduced into a component collecting system in a gaseous state, are treated by a low boiling point component removing unit, are condensed and collected in the system, and finally are conveyed to a polymerization system again to participate in polymerization reaction.
Preferably, the devolatilization reaction kettles connected in series and/or in parallel are connected through a melt inlet and a melt outlet, and the gas outlets are converged through a pipeline.
Preferably, the low boiling point component removal unit comprises one or more of a low boiling point component removal column, a recovery tank, a spray column, a fractionation column, a condensation column and a vacuum device connected in parallel; a rotatable scraper attached to the inner wall of the low-boiling-point component removing tower is arranged in each low-boiling-point component removing tower, and a gas outlet of the devolatilization reaction kettle is communicated with the low-boiling-point component removing tower; the recovery tank is connected with the bottom of the low-boiling-point component removal tower; the spray tower is arranged at the top of the low-boiling-point component removing tower, and a fractionating tower, a condensing tower and a vacuum device are sequentially connected behind the spray tower.
The utility model discloses a low boiling point component desorption tower is horizontal structure, and its theory of operation is: the scraper is arranged in the low boiling point component removing tower and can periodically rotate along the inner wall, so that the low boiling point component (the main component is caprolactam) is prevented from being accumulated on the inner wall and being accumulated into hard substances after a long time, and the heat transfer and the working efficiency of the system are influenced. The gas moves upwards after entering the low boiling point component removing tower and needs to pass through a spray tower, the spray medium of the spray tower can be water or caprolactam, and the spray temperature is 60-80 ℃; the low boiling point component in the gas is separated from the gas after being cooled, and the liquid obtained by spraying and cooling is collected in a recovery tank and can be conveyed to a polymerization system under the action of a conveying pump for direct recycling. While the gas fraction continues to be processed through a fractionation column and a condensation column in that order. Wherein the fractionating tower is condensed with hot water at a temperature of 70-80 deg.C in order to condense caprolactam remaining in the gas stream, the gas is then passed through a condensing tower at a temperature of 0-30 deg.C in order to condense water from the gas stream, and finally passed through a vacuum device.
Preferably, the vacuum device comprises one or a combination of multiple stages of a rotary vane vacuum pump, a molecular vacuum pump, a jet vacuum pump, a diffusion pump and a diffusion jet pump.
Preferably, both the inner wall of the low boiling point component removal column and the scraper are subjected to a non-stick treatment.
The parts can avoid the adhesion and accumulation of sticky materials on the surfaces of the parts after non-stick treatment.
Compared with the prior art, the beneficial effects of the utility model are that:
(1) the utility model provides a can be with taking off reation kettle of hot water extractables desorption in the nylon 6 fuse-element, compare in conventional hot water extraction technology, have that the flow is short, fast, energy consumption low grade advantage to through this device, can realize nylon 6's fuse-element direct spinning, greatly reduced nylon 6 manufacturing cost, the single line productivity is greatly improved, and the flow is short, the capital construction investment greatly reduced of unit productivity.
(2) In each devolatilization reaction kettle, introduced gas can make the melt attached to the devolatilization disc bubble to form a thinner melt film, thereby further increasing the devolatilization area, improving the devolatilization efficiency, breaking when the melt bubbles are increased to a certain degree, leading the gas to be taken out of the system under the vacuum action, further improving the diffusion area and greatly improving the devolatilization effect. Meanwhile, because the system contains a certain amount of water, the polycondensation reaction of the nylon 6 is inhibited, the phenomenon that the molecular weight of the nylon 6 swells under the vacuum condition to influence the spinning forming process is avoided, time is provided for nylon 6 amide exchange, the molecular weight distribution is narrowed, and the melt quality is improved. In addition, as the cyclic dimer and other nonvolatile components have better solubility in hot water, the moisture in the hot nitrogen gas flow can interact with the cyclic dimer and other nonvolatile components, the cyclic dimer and other nonvolatile components can be driven to volatilize, the content of the nonvolatile components in the melt is reduced, the content of oligomers in the melt is further reduced, and the quality of the melt is improved.
(3) The mixed gas generated by the devolatilization system is separated to collect hot water extractables in the gas, low-boiling components are collected in a spray condensing mode, a scraper plate is arranged to avoid the components from being accumulated in the equipment, and a fractionating tower and a condensing tower are arranged to further purify the gas flow so as to avoid the influence of the volatile components entering a vacuum pump on the working efficiency and the service life of the vacuum pump; these designs greatly increase the life cycle of the condensing system and increase the stability of the system.
Drawings
Fig. 1 is a schematic structural diagram of embodiment 1 of the present invention;
fig. 2 is a schematic structural diagram of embodiment 2 of the present invention;
fig. 3 is a schematic structural diagram of embodiment 2 of the present invention;
fig. 4 is a schematic structural view of the devolatilization plate in embodiments 1 to 3 of the present invention.
The reference signs are: a devolatilization reaction kettle 1, a low boiling point component removing tower 4, a spray tower 5, a fractionating tower 6, a condensing tower 7, a vacuum device 8, a recovery tank 9, a shell 101, a hollow rotating shaft 102, a motor 103, a devolatilization disc 104, a melt inlet 105, a melt outlet 106, a gas inlet 107, a gas outlet 108, a hollow branch pipe 109, an air hole 110 and a scraper 401.
Detailed Description
The present invention will be further described with reference to the following examples.
General examples
A nylon 6 melt devolatilization device comprises a devolatilization system and a component collection system which are sequentially connected.
Wherein, the devolatilization system comprises a plurality of devolatilization reaction kettles 1 which are connected in series and/or in parallel; the devolatilization reaction kettle comprises a shell 101, a hollow rotating shaft 102, a motor 103 and at least one devolatilization disk 104; the bottom of the shell is provided with a melt inlet 105 and a melt outlet 106, the middle of the side surface of the shell is provided with a gas inlet 107, and the top of the shell is provided with a gas outlet 108 (the melt inlet and the melt outlet, the gas inlet and the gas outlet are positioned on opposite sides); the hollow rotating shaft is horizontally arranged in the shell, one end of the hollow rotating shaft is communicated with the gas inlet, and the motor is used for driving the hollow rotating shaft to rotate; the devolatilization discs are fixed on the hollow rotating shaft through hollow branch pipes 109 communicated with the hollow rotating shaft, and when the number of the devolatilization discs is multiple, a plurality of the devolatilization discs are sequentially arranged in parallel on the hollow rotating shaft; the devolatilization disc is distributed with air holes 110; the gas outlet of the devolatilization reaction kettle is connected with a component collecting system.
The component collection system includes a low boiling point component removal unit.
Preferably, the diameter of the air hole of the devolatilization reaction kettle is 0.1-10 mm.
Preferably, the devolatilization reaction kettles connected in series and/or in parallel are connected through a melt inlet and a melt outlet, and the gas outlets are converged through a pipeline.
Preferably, the low boiling point component removal unit includes one or more of a low boiling point component removal column 4, a recovery tank 9, a spray column 5, a fractionation column 6, a condensation column 7 and a vacuum apparatus 8 connected in parallel. A rotatable scraper 401 attached to the inner wall of the low-boiling-point component removal tower is arranged in each low-boiling-point component removal tower, and the recovery tank is connected with the bottom of the low-boiling-point component removal tower; the spray tower is arranged at the top of the low-boiling-point component removing tower, and a fractionating tower, a condensing tower and a vacuum device are sequentially connected behind the spray tower.
Preferably, the vacuum device comprises one or a combination of multiple stages of a rotary vane vacuum pump, a molecular vacuum pump, a jet vacuum pump, a diffusion pump and a diffusion jet pump.
Preferably, both the inner wall of the low boiling point component removal column and the scraper are subjected to a non-stick treatment.
Example 1
A nylon 6 melt devolatilization device comprises a devolatilization system and a component collection system which are sequentially connected.
Wherein, as shown in figure 1, the devolatilization system is a devolatilization reaction kettle 1; the devolatilization reaction kettle comprises a shell 101, a hollow rotating shaft 102, a motor 103 and eleven devolatilization discs 104; the bottom of the shell is provided with a melt inlet 105 and a melt outlet 106, the middle of the side surface of the shell is provided with a gas inlet 107, and the top of the shell is provided with a gas outlet 108 (the melt inlet and the melt outlet, the gas inlet and the gas outlet are positioned on opposite sides); the hollow rotating shaft is horizontally arranged in the shell, one end of the hollow rotating shaft is communicated with the gas inlet, and the motor is used for driving the hollow rotating shaft to rotate; as shown in fig. 4, the devolatilization discs are fixed on the hollow rotating shaft through hollow branch pipes 109 communicated with the hollow rotating shaft, eleven devolatilization discs are sequentially connected in series and arranged in parallel on the hollow rotating shaft; the devolatilization disc is distributed with air holes 110 (the diameter is 10 mm); the gas outlet of the devolatilization reaction kettle is connected with a component collecting system.
The component collection system includes a low boiling point component removal unit. The low boiling point component removing unit comprises a low boiling point component removing tower 4, a recovery tank 9, a spray tower 5, a fractionating tower 6, a condensing tower 7 and a vacuum device 8. A rotatable scraper 401 (driven by a rotating motor) attached to the inner wall of the low-boiling-point component removal tower is arranged in the low-boiling-point component removal tower, and the recovery tank is connected with the bottom of the low-boiling-point component removal tower; the spray tower is arranged at the top of the low boiling point component removing tower, and a fractionating tower, a condensing tower and a vacuum device (a rotary vane vacuum pump) are sequentially connected behind the spray tower. Wherein the inner wall of the low boiling point component removal tower, the scraper and the inner wall of the connected pipeline are subjected to non-stick treatment.
The devolatilization method of the apparatus of this example was as follows:
1) respectively introducing the nylon 6 melt and hot nitrogen with the water content of 0.1wt% into a devolatilization reaction kettle through respective channels for devolatilization, removing most of hot water extractables in the nylon 6 melt, mixing the hot water extractables with the hot nitrogen to form a gaseous mixture, discharging the gaseous mixture from the devolatilization reaction kettle, and discharging the devolatilized nylon 6 melt from a melt outlet.
2) The gaseous mixture enters a low boiling point component removing tower after confluence, and the low boiling point component in the gaseous mixture falls into the tower bottom to be discharged and collected after the gaseous mixture is sprayed, fractionated and condensed in the rising process; and residual gas is discharged after vacuum treatment. The operating temperature of the low boiling point component removal column was 80 ℃. The spraying medium is water, and the spraying temperature is 80 ℃; the fractionation is a hot water fractionation at 70 ℃; the temperature of the condensation was 30 ℃.
Example 2
A nylon 6 melt devolatilization device comprises a devolatilization system and a component collection system which are sequentially connected.
As shown in fig. 2, the devolatilization system comprises a front devolatilization reaction kettle 1 and a rear devolatilization reaction kettle 1 which are connected in series; the devolatilization reaction kettle comprises a shell 101, a hollow rotating shaft 102, a motor 103 and eleven devolatilization discs 104; the bottom of the shell is provided with a melt inlet 105 and a melt outlet 106, the middle of the side surface of the shell is provided with a gas inlet 107, and the top of the shell is provided with a gas outlet 108 (the melt inlet and the melt outlet, the gas inlet and the gas outlet are positioned on opposite sides); the hollow rotating shaft is horizontally arranged in the shell, one end of the hollow rotating shaft is communicated with the gas inlet, and the motor is used for driving the hollow rotating shaft to rotate; as shown in fig. 4, the devolatilization discs are fixed on the hollow rotating shaft through hollow branch pipes 109 communicated with the hollow rotating shaft, eleven devolatilization discs are sequentially connected in series and arranged in parallel on the hollow rotating shaft; the devolatilization disc is distributed with air holes 110 (the diameter is 10 mm); the gas outlet of the devolatilization reaction kettle is connected with a component collecting system. The devolatilization reaction kettles connected in series are connected through a melt inlet and a melt outlet, and all gas outlets converge through a pipeline.
The component collection system includes a low boiling point component removal unit. The low boiling point component removing unit comprises a low boiling point component removing tower 4, a recovery tank 9, a spray tower 5, a fractionating tower 6, a condensing tower 7 and a vacuum device 8. A rotatable scraper 401 (driven by a rotating motor) attached to the inner wall of the low-boiling-point component removal tower is arranged in the low-boiling-point component removal tower, and the recovery tank is connected with the bottom of the low-boiling-point component removal tower; the spray tower is arranged at the top of the low boiling point component removing tower, and a fractionating tower, a condensing tower and a vacuum device (a rotary vane vacuum pump) are sequentially connected behind the spray tower. Wherein, the inner wall of the low boiling point component removing tower, the scraper and the inner wall of the connected pipeline are subjected to non-stick treatment.
The devolatilization method of the apparatus of this example was as follows:
1) respectively introducing a nylon 6 melt and hot nitrogen with the water content of 0.1wt% into a devolatilization reaction kettle at the front end through respective channels for devolatilization, removing most of hot water extractables in the nylon 6 melt, mixing the hot water extractables with the hot nitrogen to form a gaseous mixture, discharging the gaseous mixture from the devolatilization reaction kettle, conveying the devolatilized nylon 6 melt to a devolatilization reaction kettle at the rear end for secondary devolatilization without introducing nitrogen, and discharging the nylon 6 melt and the gaseous mixture generated after the secondary devolatilization from the devolatilization reaction kettle respectively. Wherein the absolute pressure in the devolatilization reaction kettle positioned at the front end is 500Pa, the temperature is 240 ℃, and the residence time of the nylon 6 melt in the devolatilization reaction kettle is 0.5 h; the absolute pressure in the devolatilization reaction kettle positioned at the rear end is below 500Pa, the temperature is 270 ℃, and the residence time of the nylon 6 melt in the devolatilization reaction kettle is 10 min.
2) The gaseous mixture enters a low boiling point component removing tower, and the low boiling point component in the gaseous mixture falls into the tower bottom to be discharged and collected after the gaseous mixture is sprayed, fractionated and condensed in the rising process; and residual gas is discharged after vacuum treatment. The operating temperature of the low boiling point component removal column was 80 ℃. The spraying medium is water, and the spraying temperature is 80 ℃; the fractionation is a hot water fractionation at 70 ℃; the temperature of the condensation was 30 ℃.
Example 3
A nylon 6 melt devolatilization device comprises a devolatilization system and a component collection system which are sequentially connected.
As shown in fig. 3, the devolatilization system comprises a front devolatilization reaction kettle 1 and a back devolatilization reaction kettle 1 which are connected in parallel, and a devolatilization reaction kettle which is connected in series with the two devolatilization reaction kettles which are connected in parallel; each devolatilization reaction kettle comprises a shell 101, a hollow rotating shaft 102, a motor 103 and eleven devolatilization discs 104; the bottom of the shell is provided with a melt inlet 105 and a melt outlet 106, the middle of the side surface of the shell is provided with a gas inlet 107, and the top of the shell is provided with a gas outlet 108 (the melt inlet and the melt outlet, the gas inlet and the gas outlet are positioned on opposite sides); the hollow rotating shaft is horizontally arranged in the shell, one end of the hollow rotating shaft is communicated with the gas inlet, and the motor is used for driving the hollow rotating shaft to rotate; as shown in fig. 4, the devolatilization discs are fixed on the hollow rotating shaft through hollow branch pipes 109 communicated with the hollow rotating shaft, eleven devolatilization discs are sequentially connected in series and arranged in parallel on the hollow rotating shaft; the devolatilization disc is distributed with air holes 110 (the diameter is 0.1 mm); a clapboard 111 fixed at the bottom of the shell is arranged between the adjacent devolatilization discs and is connected with a component collection system. The devolatilization reaction kettles connected in series are connected through a melt inlet and a melt outlet, and all gas outlets converge through a pipeline.
The component collection system includes a low boiling point component removal unit. The low boiling point component removing unit comprises a low boiling point component removing tower 4, a recovery tank 9, a spray tower 5, a fractionating tower 6, a condensing tower 7 and a vacuum device 8. A rotatable scraper 401 (driven by a rotating motor) attached to the inner wall of the low-boiling-point component removal tower is arranged in the low-boiling-point component removal tower, and the recovery tank is connected with the bottom of the low-boiling-point component removal tower; the spray tower is arranged at the top of the low boiling point component removal tower, and a fractionating tower, a condensing tower and a vacuum device (a molecular vacuum pump) are sequentially connected behind the spray tower. Wherein the inner wall of the low boiling point component removal tower, the scraper and the inner wall of the connected pipeline are subjected to non-stick treatment.
The devolatilization method of the apparatus of this example was as follows:
1) respectively introducing a nylon 6 melt and hot nitrogen with the water content of 10wt% into devolatilization reaction kettles (two parallel) at the front end through respective channels for devolatilization, removing most of hot water extractables in the nylon 6 melt, mixing the hot water extractables with the hot nitrogen to form a gaseous mixture and discharging the gaseous mixture from the devolatilization reaction kettles, conveying the devolatilized nylon 6 melt to the devolatilization reaction kettle at the rear end (positioned at the rear end in series) for secondary devolatilization without nitrogen, and discharging the nylon 6 melt and the gaseous mixture generated after the secondary devolatilization from the devolatilization reaction kettles respectively. Wherein the absolute pressure in the devolatilization reaction kettle positioned at the front end is 1000Pa, the temperature is 250 ℃, and the residence time of the nylon 6 melt in the devolatilization reaction kettle is 2 hours; the absolute pressure in the devolatilization reaction kettle positioned at the rear end is below 500Pa, the temperature is 255 ℃, and the residence time of the nylon 6 melt in the devolatilization reaction kettle is 10 min.
2) The gaseous mixture enters a low boiling point component removing tower, and the low boiling point component in the gaseous mixture falls into the tower bottom to be discharged and collected after the gaseous mixture is sprayed, fractionated and condensed in the rising process; and residual gas is discharged after vacuum treatment. The operating temperature of the low boiling point component removal column was 60 ℃. The spraying medium is caprolactam, and the spraying temperature is 60 ℃; the fractionation is hot water fractionation at 80 ℃; the temperature of the condensation was 0 ℃.
The raw materials and the equipment used in the utility model are common raw materials and equipment in the field if no special description is provided; the methods used in the present invention are conventional methods in the art unless otherwise specified.
The above, only be the utility model discloses a preferred embodiment, it is not right the utility model discloses do any restriction, all according to the utility model discloses the technical entity all still belongs to any simple modification, change and equivalent transformation of doing above embodiment the utility model discloses technical scheme's protection scope.
Claims (8)
1. The utility model provides a nylon 6 fuse-element devolatilization reation kettle which characterized in that: comprises a shell, a hollow rotating shaft, a motor and at least one devolatilization disk; the bottom of the shell is provided with a melt inlet and a melt outlet, the middle part of the side surface of the shell is provided with a gas inlet, and the top of the shell is provided with a gas outlet; the hollow rotating shaft is horizontally arranged in the shell, one end of the hollow rotating shaft is communicated with the gas inlet, and the motor is used for driving the hollow rotating shaft to rotate; the devolatilization discs are communicated with the hollow rotating shaft, and when the devolatilization discs are multiple, the multiple devolatilization discs are sequentially arranged on the hollow rotating shaft in parallel; the devolatilization disc is distributed with air holes.
2. The nylon 6 melt devolatilization reactor as claimed in claim 1 wherein said devolatilization plates are secured to and in communication with the hollow shaft by means of hollow legs in communication with the hollow shaft.
3. The nylon 6 melt devolatilization reactor as claimed in claim 1 wherein said devolatilization reactor has a pore diameter of from 0.1mm to 10 mm.
4. A devolatilization apparatus comprising the nylon 6 melt devolatilization reactor of claim 1, 2 or 3 wherein: comprises a devolatilization system and a component collection system which are connected in sequence;
the devolatilization system comprises a plurality of devolatilization reaction kettles which are connected in series and/or in parallel; the gas outlet of the devolatilization reaction kettle is connected with a component collecting system; the component collection system includes a low boiling point component removal unit.
5. The devolatilizer as claimed in claim 4 wherein the devolatilizer reactors in series and/or parallel are connected by a melt inlet and a melt outlet and the gas outlets are confluent by a conduit.
6. The devolatilizer as claimed in claim 4 wherein said low boiling component removal unit comprises one or more of a low boiling component removal column, a recovery tank, a spray column, a fractionation column, a condensing column and a vacuum apparatus connected in parallel; a rotatable scraper attached to the inner wall of the low-boiling-point component removing tower is arranged in each low-boiling-point component removing tower, and a gas outlet of the devolatilization reaction kettle is communicated with the low-boiling-point component removing tower; the recovery tank is connected with the bottom of the low-boiling-point component removal tower; the spray tower is arranged at the top of the low-boiling-point component removing tower, and a fractionating tower, a condensing tower and a vacuum device are sequentially connected behind the spray tower.
7. The devolatilizer as claimed in claim 6 wherein said vacuum means comprises one or more of a rotary-vane vacuum pump, a molecular vacuum pump, a jet vacuum pump, a diffusion pump and a diffusion jet pump in series.
8. The devolatilizer of claim 6 wherein both the internal walls of said low boiling point component removal column and the wipers are treated to be non-stick.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113461937A (en) * | 2021-06-29 | 2021-10-01 | 浙江恒澜科技有限公司 | Fine devolatilization device for nylon 6 melt |
| CN114712997A (en) * | 2022-05-11 | 2022-07-08 | 广东寰球广业工程有限公司 | Process for removing heavy components and system and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113461937A (en) * | 2021-06-29 | 2021-10-01 | 浙江恒澜科技有限公司 | Fine devolatilization device for nylon 6 melt |
| CN114712997A (en) * | 2022-05-11 | 2022-07-08 | 广东寰球广业工程有限公司 | Process for removing heavy components and system and application thereof |
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