CN210584856U - Feeding device of polymerization reactor for preparing aramid fibers 1414 - Google Patents
Feeding device of polymerization reactor for preparing aramid fibers 1414 Download PDFInfo
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Abstract
The utility model discloses a feed arrangement for preparing polymerization reactor of aramid fiber 1414 belongs to polymerization equipment technical field. The device comprises a high-temperature fluid channel and a low-temperature fluid channel, wherein one end of the high-temperature fluid channel is provided with a high-temperature material inlet, the other end of the high-temperature fluid channel is provided with a high-temperature material outlet, and a high-temperature heat-insulating jacket is sleeved outside the high-temperature fluid channel; one end of the low-temperature fluid channel is provided with a low-temperature material inlet, the other end of the low-temperature fluid channel is provided with a low-temperature material outlet, and the outer side of the low-temperature fluid channel is sleeved with a low-temperature heat-insulating jacket; the lower part of the high-temperature fluid channel and the lower part of the low-temperature fluid channel are fixed through a fixing piece, an outer jacket is arranged at the lower end of the fixing piece, a heat insulation layer is arranged between the lower part of the high-temperature fluid channel and the lower part of the low-temperature fluid channel, and a reaction cavity is arranged at the lower part of the outer jacket. Two reactants with high temperature difference are contacted and start to react in a tiny cavity before leaving the feeding device to the reactor element, and reaction products can be quickly taken away by a reactor screw without blocking feeding.
Description
Technical Field
The utility model relates to a feed arrangement for polymerization reactor especially relates to a feed arrangement for preparing aramid fiber 1414, polymerization reactor that the difference in temperature is high, belongs to polymerization equipment technical field.
Background
Aramid 1414, namely poly (p-phenylene terephthalamide). In the production process, two reactants of p-phenylenediamine and paraphthaloyl chloride are polymerized to prepare an aramid polymer (namely aramid 1414), and then the aramid polymer is used for preparing a spinning solution for spinning, wherein the quality of the aramid polymer directly influences the spinning process and the quality of a spinning finished product. Because the local reaction is too fast due to large heat release and fast reaction rate in the polymerization reaction process, a large amount of small molecular polymers are formed, and the molecular weight distribution of the polymers is not uniform, the polymerization reaction is generally carried out by adopting a two-step method, which specifically comprises the following steps: in the case of batch polymerization using a polymerization reactor, first, NMP-CaC1 was prepared2Adding TPC (paraphthaloyl chloride TPC) accounting for 20-40% of the total amount of TPC into a PPDA (N-methylpyrrolidone NMP; p-phenylenediamine PPDA) pre-mixed solution for prepolymerization, and continuously removing reaction heat in the prepolymerization process to keep a prepolymer product in a low-temperature state (below 10 ℃); then, the remaining amount of TPC was added to the polymerization reactor, and polymerization was performed to obtain a final polymer.
In the batch polymerization process, as TPC is in a solid state at normal temperature, the polymerization efficiency is low, the effective polymerization quality is poor, and the industrial production usually needs a continuous production process to obtain sufficient productivity and production efficiency. TPC can be molten into liquid at more than 85 ℃, is convenient to adopt a pump and a metering device to carry out continuous conveying and metering, and the molten state of TPC is easier to disperse than the solid state, so that the reaction is more sufficient and rapid in the polymerization reaction process, but the TPC has the following problems: on one hand, the respective feeding temperatures of the pre-mixture and the pre-polymer need to be controlled, and the reaction progress can be controlled in a low-temperature state; on the other hand, it is necessary to keep the temperature of TPC above the melting point before the polymerization reaction is carried out.
At present, an existing polymerization reactor is adopted, in the first-step prepolymerization reaction process, TPC and a premix carry out prepolymerization reaction, although the process is a rapid exothermic reaction, in the process, equivalent TPC does not react with PPDA in the premix, so that a polymer formed at the end point of the reaction is a small molecular weight polymer, is an oily liquid in a solvent system, has good fluidity, does not block a mixture channel, and thus the materials in the channel of the polymerization reactor start to react by self-contact; in the second polymerization step, the residual equivalent of TPC reacts with the prepolymer, the reactive monomers TPC and PPDA are completely equivalent, the reaction end point is the high-molecular aramid polymer, and the high-molecular aramid polymer and the solvent form a powdery solid material in the solvent, so that blockage is easy to occur. In addition, the remaining equivalent amount of TPC (high temperature) and the prepolymer (low temperature) need to enter the polymerization reactor at the same time, and the TPC needs to contact the prepolymer and start to react before contacting the components in the polymerization reactor, because the TPC once contacts the components in the polymerization reactor first, the TPC will decrease to below the melting point and become solid, and the TPC will attach to the components (such as screw, cylinder, etc.), and the TPC cannot be dispersed and polymerized in a liquid form, thereby causing the problem of uneven molecular weight distribution.
Disclosure of Invention
The utility model aims to solve the problems in the prior art and provides a feeding device of a polymerization reactor for preparing aramid fibers 1414. In the technical scheme, the device effectively solves the problems that two substances participating in the reaction in the prior art cannot continuously and stably enter a polymerization reactor, so that aramid polymers with uniform molecular weight distribution cannot be continuously and stably produced, and the like; by adopting the device, two reactants with high temperature difference are contacted and start to react from leaving the feeding device to entering the reaction cavity before entering the polymerization reactor element, and the reaction product can be quickly taken away by the reactor screw without blocking the feeding; the formed reactants continue to react in the polymerization reactor to the end of the reaction to form the final desired high molecular weight polymer, which exits from the polymerization reactor outlet and enters a downstream production process.
In order to achieve the technical purpose, the following technical scheme is proposed:
the feeding device of the polymerization reactor for preparing the aramid fibers 1414 comprises a high-temperature fluid channel and a low-temperature fluid channel which are connected with the polymerization reactor, wherein one end of the high-temperature fluid channel is provided with a high-temperature material inlet, the other end of the high-temperature fluid channel is provided with a high-temperature material outlet, and the outer side of the high-temperature fluid channel is sleeved with a high-temperature heat-insulation jacket;
one end of the low-temperature fluid channel is provided with a low-temperature material inlet, the other end of the low-temperature fluid channel is provided with a low-temperature material outlet, and a low-temperature heat-insulating jacket is sleeved outside the low-temperature fluid channel;
the lower part of the high-temperature fluid channel and the lower part of the low-temperature fluid channel are fixed through a fixing piece, an outer jacket is arranged at the lower end of the fixing piece, the upper part of the outer jacket is sleeved outside the lower part of the high-temperature fluid channel and the lower part of the low-temperature fluid channel, and a heat insulation layer is arranged between the lower part of the high-temperature fluid channel and the lower part of;
the lower part of the outer jacket is provided with a reaction cavity, and the high-temperature fluid channel and the low-temperature fluid channel are both communicated with the reaction cavity.
Furthermore, the lower end of the outer jacket is provided with an end face matched with the polymerization reactor, and the matching comprises matching of shape, size, connection mode and the like.
Furthermore, a high-temperature medium inlet and a high-temperature medium outlet are arranged on the high-temperature heat-preservation jacket.
Furthermore, the high-temperature medium inlet is arranged on the jacket at the high-temperature material inlet, and the high-temperature medium outlet is arranged on the jacket at the high-temperature material outlet.
Furthermore, a low-temperature medium inlet and a low-temperature medium outlet are formed in the low-temperature heat-preservation jacket.
Furthermore, the low-temperature medium inlet is arranged on the jacket at the low-temperature material outlet, and the low-temperature medium outlet is arranged on the jacket at the low-temperature material inlet.
Furthermore, the fixing piece is a flange and is connected and fixed through a nut.
Furthermore, the heat insulation layer is a heat insulation sleeve filled with silicate heat insulation materials, so that heat transfer is effectively prevented.
Furthermore, the distance between the end face and a screw in the polymerization reactor is 5-10 mm.
By adopting the technical scheme, the related working principle is as follows:
the technical scheme is that the feeding device is specially used for continuously feeding reaction components with high temperature difference in front of a polymerization reactor, and in the device, a high-temperature material and a low-temperature material are isolated from each other through arrangement of a high-temperature fluid channel, a low-temperature fluid channel and a heat insulation layer from a material inlet to a material outlet, so that the materials with high temperature difference are prevented from influencing each other; on the other hand, the arrangement of the heat-insulating jacket ensures that the materials of all components can still keep the required temperature after entering the polymerization reactor.
After the reaction component with high temperature difference enters a polymerization reactor, the high-temperature material and the low-temperature material firstly contact and start to react, and a polymer is formed in a micro cavity before the high-temperature material and the low-temperature material contact elements such as a screw rod, so that the polymer cannot be completely solidified to block the end face, and the temperature is not required to be strictly controlled (when monomer materials are fed, the temperature is required to be strictly controlled); can be rapidly fed into a polymerization reactor when contacting elements such as a screw and the like, and continuously react until the reaction end point, thereby realizing continuous and stable feeding and polymerization reaction.
By adopting the technical scheme, the beneficial technical effects brought are as follows:
1) the utility model effectively solves the problems that two substances participating in the reaction in the prior art can not continuously and stably enter a polymerization reactor, so that aramid polymers with uniform molecular weight distribution can not be continuously and stably produced, and the like; by adopting the device, two reactants with high temperature difference are contacted and start to react in a micro cavity before entering a polymerization reactor element from a feeding device, and a reaction product can be quickly taken away by a reactor screw without blocking feeding; the formed reactant continues to react in the polymerization reactor to the reaction end point, and the finally needed high molecular polymer is formed and leaves from the outlet of the polymerization reactor and enters a downstream production process;
2) the polymerization reaction of the aramid fiber 1414 is an exothermic reaction, and a large amount of low molecular polymers are generated due to too high temperature, so that the molecular weight distribution range is widened, and the generation of high molecular polymers with concentrated molecular weight is not facilitated.
In the feeding device, the low-temperature fluid channel is arranged, so that the prepolymer can enter a polymerization reactor in a low-temperature state (the prepolymer contains a large amount of solvent and has a large mass ratio, and therefore the initial temperature of the part of materials has great influence on the temperature of the whole polymerization reaction;
the high-temperature fluid channel is arranged to enable the TPC to enter a polymerization reactor in a molten state and to contact and react with a low-temperature prepolymer in the molten state. The molten state TPC has a much higher dispersibility than the solid state TPC, and therefore, the molten state TPC (high temperature TPC) is very advantageous for the sufficiency of polymerization and the uniformity of the final molecular weight distribution.
The setting of reaction cavity guarantees that high low temperature material contacts and preliminary reaction in the cavity, because the low temperature material can effectively restrain reaction temperature, the polymer that forms has certain mobility, is easily taken away by components such as rotation screw rod. Meanwhile, the two materials are in a liquid state before contacting, are uniformly dispersed, and the polymer has good viscosity stability, uniform molecular weight distribution and good product quality after continuous reaction.
Drawings
Fig. 1 is a schematic structural view of the present invention;
FIG. 2 is a sectional view of the structure of the present invention;
FIG. 3 is a schematic view of the installation structure of the present invention on a polymerization reactor;
the polymerization reactor comprises a polymerization reactor 1, a high-temperature fluid channel 2, a low-temperature fluid channel 3, a low-temperature fluid channel 4, a high-temperature material inlet 5, a high-temperature material outlet 6, a high-temperature heat-preservation jacket 7, a low-temperature material inlet 8, a low-temperature material outlet 9, a low-temperature heat-preservation jacket 10, a fixing piece 11, an outer jacket 12, a heat-insulation layer 13, an end face 14, a high-temperature medium inlet 15, a high-temperature medium outlet 16, a low-temperature medium inlet 17, a low-temperature medium outlet 18 and a reaction cavity.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Example 1
The feeding device for the polymerization reactor for preparing the aramid fibers 1414 comprises a high-temperature fluid channel 2 and a low-temperature fluid channel 3 which are connected with the polymerization reactor 1, wherein one end of the high-temperature fluid channel 2 is provided with a high-temperature material inlet 4, the other end of the high-temperature fluid channel is provided with a high-temperature material outlet 5, and the outer side of the high-temperature fluid channel 2 is sleeved with a high-temperature heat-insulating jacket 6; one end of the low-temperature fluid channel 3 is provided with a low-temperature material inlet 7, the other end of the low-temperature fluid channel is provided with a low-temperature material outlet 8, and a low-temperature heat-insulating jacket 9 is sleeved outside the low-temperature fluid channel 3;
the lower part of the high-temperature fluid channel 2 and the lower part of the low-temperature fluid channel 3 are fixed through a fixing piece 10, an outer jacket 11 is arranged at the lower end of the fixing piece 10, the upper part of the outer jacket 11 is sleeved on the outer sides of the lower parts of the high-temperature fluid channel 2 and the low-temperature fluid channel 3, and a heat insulation layer 12 is arranged between the lower part of the high-temperature fluid channel 2 and the lower part of the; the lower part of the outer jacket 11 is provided with a reaction cavity 18, the high-temperature fluid channel 2 and the low-temperature fluid channel 3 are both communicated with the reaction cavity 18, and the high-temperature material and the low-temperature material are contacted in the reaction cavity 18 and start polymerization reaction.
Example 2
On the basis of example 1, further,
the lower end of the outer jacket 11 is provided with an end face 13 which is matched with the polymerization reactor 1, and the matching comprises matching of shape, size, connection mode and the like. The polymerization reactant is a screw reactor and comprises a cylindrical shell, wherein a screw is arranged in the shell, and the screw conveys the reactant.
Example 3
On the basis of example 2, further,
the high-temperature heat-preservation jacket 6 is provided with a high-temperature medium inlet 14 and a high-temperature medium outlet 15, the high-temperature medium inlet is arranged on the jacket at the high-temperature material inlet 4, and the high-temperature medium outlet 15 is arranged on the jacket at the high-temperature material outlet 5. High-temperature media are arranged in the high-temperature heat-preservation jacket 6, such as: steam, hot water, etc. And (3) introducing a high-temperature medium into the high-temperature heat-insulation jacket 6 from the high-temperature medium inlet, then discharging the high-temperature medium from the high-temperature medium outlet 15, and enabling the heat tracing medium of the jacket to be smooth, so that the temperature of the high-temperature material in the high-temperature fluid channel 2 in the jacket is ensured, and continuous heat tracing and heat insulation are carried out.
The low-temperature heat-preservation jacket 9 is provided with a low-temperature medium inlet 16 and a low-temperature medium outlet 17, the low-temperature medium inlet 16 is arranged on the jacket at the low-temperature material outlet 8, and the low-temperature medium outlet 17 is arranged on the jacket at the low-temperature material inlet 7. The low-temperature insulating jacket 9 is internally provided with low-temperature media, such as: cold water, etc. And a low-temperature medium is introduced into the low-temperature heat-insulation jacket 9 from the low-temperature medium inlet 16, then the low-temperature medium is discharged from the low-temperature medium outlet 17, the heat tracing medium of the jacket is enabled to be smooth, and the temperature of the low-temperature material in the low-temperature fluid channel 3 in the jacket is further ensured to be continuously constant.
Example 4
On the basis of example 3, further,
the distance between the end face 13 and the screw in the polymerization reactor 1 was 5 mm. The polymer is kept for a long time due to the overlarge distance, so that the polymer reacts until no solid in a flowing state exists, is not easy to be taken away by a screw element and is easy to block a channel; too small a distance causes molten TPC to easily contact elements such as threads and cylinders, become solid when cooled, cannot rapidly participate in the reaction, and accumulate between the polymerization reactor and the feeding device to block the end face 13.
Example 5
On the basis of example 4, this example differs in that the end face 13 is at a distance of 10mm from the screw in the polymerization reactor 1.
Example 6
On the basis of examples 4 to 5, this example differs in that the end face 13 is at a distance of 8mm from the screw in the polymerization reactor 1.
Example 7
The present feed apparatus was implemented and used based on example 6. Firstly, preparing a prepolymer solution by adopting a PPDA solution (the solute is PPDA, and the solvent is NMP-CaCl 2) with the mass fraction of 4.5% and molten TPC with the total amount of 30% of TPC, and then cooling the prepolymer solution to 10 ℃; then the TPC is conveyed to a polymerization reactor through a low-temperature fluid channel 3, and simultaneously, the remaining 70 percent of the TPC in a molten state (82-120 ℃) is conveyed to the polymerization reactor through a high-temperature fluid channel 2. The two materials with high temperature difference start to contact and react in a micro cavity between the feeding device and the polymerization reactor, reactants are taken away by elements such as a rotating screw rod and the like, continue to react in the polymerization reactor until the reaction end point, and finally leave the polymerization reactor to enter a downstream process.
In the polymerization reactor, samples were taken at random and the viscosity of the polymerization product was measured to obtain the following results in Table 1:
example 8
Adopting three consistent double-screw polymerization reactors, namely a double-screw polymerization reactor I, a double-screw polymerization reactor II and a double-screw polymerization reactor III; next, the feeding apparatus will be described by taking as an example the production of a polyterephthalic acid terephthalate resin by polymerization between a prepolymer of NMP-CaC12-PPDA and molten TPC.
Feeding a high-temperature material (molten TPC) and a low-temperature material (prepolymer) into a double-screw polymerization reactor I by using the feeding device in the embodiment 4; and the double-screw polymerization reactor II and the double-screw polymerization reactor III do not adopt any feeding device, and directly add high-temperature materials (molten TPC) and low-temperature materials (prepolymer).
The polymerization reaction involves specific processes including:
dissolving p-phenylenediamine in NMP-CaCl2 to form a solution with the mass fraction of the p-phenylenediamine being 6%, cooling to 5 ℃, adding molten p-phthaloyl chloride accounting for 40% of the total amount of the p-phthaloyl chloride into the solution, and reacting to generate a prepolymer; cooling the prepolymer to 8 ℃, simultaneously heating the molten terephthaloyl chloride to 90 ℃, and then adding the cooled prepolymer and the molten terephthaloyl chloride into a polymerization reactor according to a stoichiometric coefficient; the polymerization reaction is carried out in a polymerization reactor with the temperature controlled within 60 ℃.
In the polymerization reactor, samples were taken at random and the viscosity of the polymerization product was measured to obtain the following results in Table 2:
Claims (9)
1. a feed arrangement for preparing polymerization reactor of aramid fiber 1414 characterized in that: the device comprises a high-temperature fluid channel (2) and a low-temperature fluid channel (3) which are connected with a polymerization reactor (1), wherein one end of the high-temperature fluid channel (2) is provided with a high-temperature material inlet (4), the other end of the high-temperature fluid channel is provided with a high-temperature material outlet (5), and the outer side of the high-temperature fluid channel (2) is sleeved with a high-temperature heat-insulating jacket (6); one end of the low-temperature fluid channel (3) is provided with a low-temperature material inlet (7), the other end of the low-temperature fluid channel is provided with a low-temperature material outlet (8), and a low-temperature heat-insulating jacket (9) is sleeved on the outer side of the low-temperature fluid channel (3);
the lower part of the high-temperature fluid channel (2) and the lower part of the low-temperature fluid channel (3) are fixed through a fixing piece (10), an outer jacket (11) is arranged at the lower end of the fixing piece (10), the upper part of the outer jacket (11) is sleeved on the outer sides of the lower part of the high-temperature fluid channel (2) and the lower part of the low-temperature fluid channel (3), and a heat insulation layer (12) is arranged between the lower part of the high-temperature fluid channel (2) and the lower part of; the lower part of the outer jacket (11) is provided with a reaction cavity (18), and the high-temperature fluid channel (2) and the low-temperature fluid channel (3) are both communicated with the reaction cavity (18).
2. The feeding device of the polymerization reactor for preparing the aramid fiber 1414 as claimed in claim 1, wherein: the lower end of the outer jacket (11) is provided with an end face (13) matched with the polymerization reactor (1).
3. The feeding device of the polymerization reactor for preparing the aramid fiber 1414 as claimed in claim 1, wherein: the high-temperature heat-preservation jacket (6) is provided with a high-temperature medium inlet (14) and a high-temperature medium outlet (15).
4. The feeding device of the polymerization reactor for preparing the aramid fiber 1414 according to claim 3, characterized in that: the high-temperature medium inlet (14) is arranged on the jacket at the high-temperature material inlet (4), and the high-temperature medium outlet (15) is arranged on the jacket at the high-temperature material outlet (5).
5. The feeding device of the polymerization reactor for preparing the aramid fiber 1414 as claimed in claim 1, wherein: and a low-temperature medium inlet (16) and a low-temperature medium outlet (17) are formed in the low-temperature heat-insulating jacket (9).
6. The feeding device of the polymerization reactor for preparing the aramid fiber 1414 according to claim 5, characterized in that: the low-temperature medium inlet (16) is arranged on the jacket at the low-temperature material outlet (8), and the low-temperature medium outlet (17) is arranged on the jacket at the low-temperature material inlet (7).
7. The feeding device of the polymerization reactor for preparing the aramid fiber 1414 as claimed in claim 1, wherein: the fixing member (10) includes a flange.
8. The feeding device of the polymerization reactor for preparing the aramid fiber 1414 as claimed in claim 1, wherein: the heat insulation layer (12) is a heat insulation sleeve filled with silicate heat insulation materials.
9. The feeding device of the polymerization reactor for preparing the aramid fiber 1414 as claimed in claim 2, wherein: the distance between the end face (13) and a screw in the polymerization reactor (1) is 5-10 mm.
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| CN201921344340.0U CN210584856U (en) | 2019-08-19 | 2019-08-19 | Feeding device of polymerization reactor for preparing aramid fibers 1414 |
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| CN201921344340.0U CN210584856U (en) | 2019-08-19 | 2019-08-19 | Feeding device of polymerization reactor for preparing aramid fibers 1414 |
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