CN115646395B - System and method for producing aramid fiber slurry by multi-device combined continuous polymerization - Google Patents
System and method for producing aramid fiber slurry by multi-device combined continuous polymerization Download PDFInfo
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Abstract
The invention provides a system and a method for producing aramid fiber slurry by multi-device combination continuous polymerization, which belong to the technical field of aramid fiber production and comprise a feed inlet of a first screw reactor communicated with a mixed raw material feed pipeline, a discharge outlet of the first screw reactor communicated with a first feed inlet of a micro-channel reactor, a second feed inlet of the micro-channel reactor communicated with a neutralizer feed pipeline, a discharge outlet of the micro-channel reactor communicated with a feed inlet of a filter, a first feed inlet and a second feed inlet arranged at the feed end of the second screw reactor, a discharge outlet of the filter communicated with the first feed inlet of the second screw reactor, a second feed inlet of the second screw reactor communicated with an aromatic acyl chloride feed pipeline, a third feed inlet arranged at the discharge end of the second screw reactor communicated with an organic base feed pipeline, and the problems of low production efficiency of batch polymerization, high heat exchange load of a reaction system and the like are solved.
Description
Technical Field
The invention belongs to the technical field of aramid fiber production, and particularly relates to a system and a method for producing aramid fiber slurry by continuous polymerization with multiple devices.
Background
The meta-aramid fiber is flame-retardant fiber with excellent performance, and has excellent performances of high temperature resistance, flame retardance, insulation, radiation resistance, chemical corrosion resistance and the like due to the stable chemical structure, so that the fabric of the fiber is flame-retardant, does not melt or drip, has quite wide application range, and is generally manufactured into equipment in the fields of industry, military, fire protection, automobile racing and the like, such as protective clothing of firefighters, filler of high-temperature filter equipment and indoor articles in public buildings.
Along with the rapid development of economy, the demand of meta-aramid fiber is continuously increased, and the production efficiency and the quality of the meta-aramid fiber are more and more required. At present, the polymerization production of meta-aramid fiber slurry mainly comprises gas phase polymerization, emulsion polymerization, interfacial polymerization and solution polymerization, the former two methods are limited to research, and the latter two methods have been used for industrial production.
Interfacial polymerization is carried out in aqueous solution and organic solution by stirring, and the reaction is intense, and has the defect that the molecular weight is difficult to control, and the polymerization degree is easily influenced by a plurality of factors such as the molecular proportion of a monomer, the stirring rotating speed, the feeding speed and the like. The monomer can not be added to adjust the molecular weight once the material is fed, and the main chain structure is not easy to control when the copolymer is prepared;
The solution polymerization is easy to generate side reaction, but the reaction system is stable, and the product can be directly used for spinning, so that the intermittent solution polymerization with more mature process technology is adopted in the production.
Batch polymerization is suitable for small-scale, multi-variety and multi-batch production, and is convenient for adjusting the yield and variety, but with the development of large-scale production, the annual output of an aramid fiber slurry polymerization device exceeds 6 ten thousand tons, and the defects of batch polymerization production technology are increasingly prominent:
(1) The utilization efficiency of production equipment is low: the number of the reaction kettle devices is multiplied, the investment is high, and the occupied area is large;
(2) Unavoidable differences in the quality of the polymeric slurries from batch to batch, leading to fluctuations in the quality of the product;
(3) In the polymerization process, acyl chloride needs to be added into the reaction system for many times until indexes reach the requirements, and the operation is complex;
(4) The temperature and pressure of the device are greatly changed, and the requirement on equipment is high;
(5) Not sensitive to product quality adjustment;
(6) The production efficiency of preparing the polymerization slurry is low.
In order to stabilize production quality and improve productivity efficiency, the invention patent with publication number of CN104072757A discloses a preparation method of poly-p-phenylene terephthalamide resin by adopting multi-device combination continuous polymerization, which adopts a mixer, a pre-reaction and a double-screw reactor to distribute heat energy generated by the whole reaction system to each device, thereby solving the problem of heat dissipation of a heat release system and effectively controlling the polymerization process; the invention patent with publication number of CN1546552A discloses a method for preparing poly-paraphenylene terephthalamide resin in a semi-continuous way, which comprises the steps of pre-polycondensing p-phenylene diamine and part of paraphthaloyl chloride, reacting the pre-polycondensate with the rest of paraphthaloyl chloride in a double-screw extruder, simultaneously introducing dry liquid ammonia for neutralization, and adding polyvinylpyrrolidone in the double-screw extruder to obtain polymer resin; the invention patent with publication number of CN112961342A discloses a continuous polymerization method of heterocyclic aramid fiber, which uses a double-screw extruder as a continuous polymerization reactor to carry out continuous polymerization reaction of the heterocyclic aramid fiber.
The above patents all carry out continuous polymerization through a double-screw reactor, but the addition of liquid acyl chloride into the double-screw reactor in a molten state has adverse effect on the control of polymerization reaction, aggravates the heat exchange load of a system, and meanwhile, the excessive and too fast addition of the acyl chloride is unfavorable for controlling the molecular weight of the polymer, so that the control difficulty is large for production.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a system and a method for producing aramid fiber slurry by multi-device combined continuous polymerization, which are based on a mode of using a screw reactor and a micro-channel reactor in series, replace a single kettle type reaction and a single double screw reactor, realize continuous polymerization automatic control of the aramid fiber slurry, avoid the amplification effect of the kettle type reactor, solve the problems of low production efficiency of intermittent polymerization, high heat exchange load of a reaction system and the like, and have high equipment utilization rate, constant product quality and high-efficiency continuous and stable preparation of the finished aramid fiber slurry.
In order to achieve the above purpose, the present invention provides the following technical solutions: the utility model provides a system for continuous polymerization production aramid fiber thick liquids of multi-device combination, includes first screw rod reactor, microchannel reactor, filter and second screw rod reactor, the feed inlet and the mixed raw materials feed line intercommunication of first screw rod reactor are used for letting in the mixed liquor of aromatic diamine solution and aromatic acyl chloride, the discharge gate of first screw rod reactor with the first feed inlet intercommunication of microchannel reactor, the second feed inlet and the neutralizer feed line intercommunication of microchannel reactor, the discharge gate of microchannel reactor with the feed inlet intercommunication of filter, the second screw rod reactor feed end is provided with first feed inlet and second feed inlet, the discharge gate of filter with the first feed inlet intercommunication of second screw rod reactor, the second feed inlet and the aromatic acyl chloride feed line intercommunication of second screw rod reactor, the second screw rod reactor discharge end is provided with the third feed inlet, the third feed inlet communicates with organic alkali pipeline.
Further, the reactor also comprises a mixing kettle, wherein the feed inlet of the mixing kettle is respectively communicated with the feed pipelines of the aromatic diamine solution and the aromatic acyl chloride, and the discharge outlet of the mixing kettle is communicated with the feed inlet of the first screw reactor through a mixed raw material feed pipeline and is used for introducing mixed raw materials into the first screw reactor for carrying out prepolymerization reaction;
the stirring speed of the mixing kettle is 20-50 r/min, and the cavity temperature is-5-10 ℃;
the mixing kettle is externally provided with an outer jacket, a double-layer double-spiral stirrer is arranged in the mixing kettle, a liquid level meter is arranged on the mixing kettle, and a regulating valve is arranged at a discharge hole.
Further, the device further comprises a first buffer stirring tank, a second buffer stirring tank, a third buffer stirring tank and a fourth buffer stirring tank, wherein the stirring rotation speed of the first buffer stirring tank is 20-50 r/min, the stirring rotation speeds of the second buffer stirring tank, the third buffer stirring tank and the fourth buffer stirring tank are all 15-35 r/min, the feeding port of the first buffer stirring tank is communicated with the discharging port of the first screw reactor, the discharging port of the first buffer stirring tank is communicated with the feeding port of the microchannel reactor, the feeding port of the second buffer stirring tank is communicated with the discharging port of the microchannel reactor, the discharging port of the second buffer stirring tank is communicated with the feeding port of the filter, the feeding port of the third buffer stirring tank is communicated with the discharging port of the filter, the discharging port of the third buffer stirring tank is communicated with the first feeding port of the second screw reactor, and the first feeding port of the fourth buffer stirring tank is communicated with the discharging port of the second screw reactor.
Further, the outside of first buffer memory agitator tank, second buffer memory agitator tank, third buffer memory agitator tank, fourth buffer memory agitator tank all sets up the outer cover, and inside all sets up double-deck double-helical ribbon agitator, all is provided with the level gauge on four buffer memory agitator tanks, and discharge gate department all is provided with the governing valve, a plurality of parallel reation kettle are all adopted to first buffer memory agitator tank, fourth buffer memory agitator tank.
Further, a second feeding port is formed in the fourth buffer stirring tank and is communicated with a feeding pipeline of the aromatic acyl chloride.
Further, the filter comprises a plurality of parallel plate-frame filters, and the plate-frame filters adopt filter cloth with 100-400 meshes.
Further, the first screw reactor and the second screw reactor are both twin screw extruders.
Further, the first screw reactor, the micro-channel reactor and the second screw reactor are connected with cooling heat exchange systems, and on-line dynamic viscometers are arranged on connecting lines of the first screw reactor, the micro-channel reactor, the filter and the second screw reactor.
The invention also provides a method for producing aramid fiber slurry by continuous polymerization with multiple devices, which comprises the following specific steps:
S1: setting the flow rate of an aromatic diamine solution to be 160 kg/h-190 kg/h, mixing the aromatic diamine solution with the molar ratio of 10 (8-9) and aromatic acyl chloride, and then introducing the mixture into a first screw reactor to obtain prepolymer slurry;
the flow rate of the first screw reactor is 185.56 kg/h-227.15 kg/h, the cavity temperature is-5 ℃ to 10 ℃, and the mixed raw materials stay in the first screw reactor for 50 s-100 s;
s2: introducing the prepolymer slurry and a neutralizing agent into a microchannel reactor for a first neutralization reaction to obtain a prepolymer slurry containing insoluble matters;
the flow rate of the microchannel reactor is 185.56 kg/h-227.15 kg/h, and the flow rate of the neutralizer is 4.98-8.1 m solution/h;
s3: passing the prepolymer slurry containing insoluble matter into a filter to obtain transparent prepolymer slurry;
the filtering pressure of the filter is 0.5-1 MPa, and the flow is 190-233.4 kg/h;
s4: introducing the transparent prepolymer slurry and aromatic acyl chloride into a second screw reactor for post-polycondensation reaction to obtain polymerization slurry, introducing organic base into the second screw reactor for secondary neutralization reaction with the polymerization slurry, and obtaining the finished product aramid fiber slurry at a discharge hole of the second screw reactor;
the temperature of the cavity of the second screw reactor is 15-35 ℃, the flow rate of the transparent prepolymer slurry is 183-213.75 kg/h, and the residence time of the transparent prepolymer slurry in the cavity of the second screw reactor is 50-100 s;
The addition amount of the aromatic acyl chloride is 10% -20% of the molar addition amount of the aromatic diamine solution, and the flow rate of the aromatic acyl chloride is 3.3 kg/h-9.273 kg/h;
the flow rate of the organic alkali is 1.74kg/h to 5.13kg/h.
Further, the mass concentration of the aromatic diamine solution is 8% -13%, and a polar organic solvent is adopted, wherein the polar organic solvent comprises at least one of N, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide and dimethyl sulfoxide;
the neutralizer is ammonia gas;
the organic base is methylamine, dimethylamine, ethylamine or diethylamine.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention provides a system for producing aramid fiber slurry by continuous polymerization with multiple devices, which is characterized in that mixed raw materials are continuously introduced into a first screw reactor for continuous reaction, so that the amplification effect of polymerization of a kettle type reactor is avoided, the first screw reactor and a micro-channel reactor both have good heat dissipation systems, and the prepolymerization reaction and the neutralization reaction carried out in the first screw reactor and the micro-channel reactor both release a large amount of heat, so that the temperature of the reaction system can be perfectly controlled by adopting the first screw reactor and the micro-channel reactor, and the heat exchange load of the reaction system is reduced; the filter is connected behind the microchannel reactor, and can filter solid insoluble matters generated by the first neutralization, so that on one hand, the phenomenon that the spinning component is blocked in the spinning process to influence the fiber quality is avoided, and on the other hand, only the filtering is needed for recycling solid wastes, and if the solid wastes are recycled in the spinning process, equipment devices are added, and the cost is increased; the transparent prepolymer slurry filtered by the filter reacts with aromatic acyl chloride in the second screw reactor, the polymerization degree of the second screw reactor can be well controlled, and the finished aramid fiber slurry which meets the requirement and has high viscosity and is suitable for spinning is rapidly generated.
The mixing kettle adopted by the invention mainly shows the mixing and stirring effects in the system, a premixing pump is used before a screw reactor in a conventional way, the premixing pump cavity is smaller, the introducing flow is low, the molten aromatic acyl chloride is solidified after contacting with the aromatic diamine solution in the cavity, and meanwhile, partial raw materials are reacted at high temperature without being fully and uniformly mixed, so that on one hand, a pipeline is blocked, and on the other hand, the heat release of the mixer is severe. The mixing kettle adopted by the invention has larger cavity, larger inlet flow and difficult blockage, simultaneously, the raw materials are quickly and uniformly mixed by stirring, and the temperature in the cavity is always controlled at-5-10 ℃ to avoid blockage caused by the reaction of the raw materials at high temperature.
According to the invention, the online dynamic viscometer is arranged on the connecting lines of the first screw reactor, the microchannel reactor, the filter and the second screw reactor, and when the online viscometer observes that the prepolymerization index fluctuates, relevant raw materials are timely supplemented for adjustment, so that the polymerization degree is further controlled, and the product quality stability is improved;
the first screw reactor and the second screw reactor are both double screw extruders, the double screw extruders axially push materials, radially mix the materials uniformly, axially mix the materials back in a small amount, ensure the consistency of molecular weight distribution, ensure the concentration of molecular weight of polymers in post polycondensation, and prevent a large amount of oligomers from separating out in the post spinning process, thereby influencing the fiber performance index.
Drawings
FIG. 1 is a schematic diagram of the front half of the system of the present invention;
FIG. 2 is a schematic diagram of the second half of the system of the present invention;
in the accompanying drawings: 1-a mixing kettle; 2-a first screw reactor; 3-a first reaction kettle; 4-a second reaction kettle; a 5-microchannel reactor; 6-a third reaction kettle; 7-a first plate and frame filter; 8-a second plate and frame filter; 9-a fourth reaction kettle; 10-a second screw reactor; 11-a fifth reaction kettle; 12-a sixth reaction kettle.
Detailed Description
The invention is further described below with reference to the drawings and the detailed description.
As shown in fig. 1-2, the invention provides a system for producing aramid fiber slurry by continuous polymerization with multiple devices, which comprises a mixing kettle 1, a first screw reactor 2, a first buffer stirring tank, a microchannel reactor 5, a second buffer stirring tank, a filter, a third buffer stirring tank, a second screw reactor 10 and a fourth buffer stirring tank, wherein:
the upper end of the mixing kettle 1 is provided with a first feed inlet and a second feed inlet which are respectively communicated with feed pipelines of the aromatic diamine solution and the aromatic acyl chloride and used for realizing uniform mixing of the aromatic diamine solution and the aromatic acyl chloride in the mixing kettle 1;
The lower end discharge port of the mixing kettle 1 is communicated with the feed port of the first screw reactor 2 through a mixed raw material feed pipeline and a pump and is used for conveying the mixed raw material into the first screw reactor 2 for pre-polymerization reaction to obtain prepolymer slurry;
the discharging port of the first screw reactor 2 is communicated with the feeding port at the upper end of the first buffer stirring tank through a pipeline, the discharging port at the lower end of the first buffer stirring tank is communicated with the first feeding port of the micro-channel reactor 5 through a pump, the prepolymer slurry in the first screw reactor 2 is conveyed into the micro-channel reactor 5 for carrying out a first neutralization reaction, and the second feeding port of the micro-channel reactor 5 is communicated with a neutralizer feeding pipeline and is used for introducing neutralizer ammonia gas into the micro-channel reactor 5 to carry out a first neutralization reaction with the prepolymer slurry to obtain prepolymer slurry containing insoluble matters;
the discharge port of the microchannel reactor 5 is communicated with the feed port at the upper end of the second buffer stirring tank, and the discharge port at the lower end of the second buffer stirring tank is communicated with the feed port of the filter through a pipeline and a pump and is used for conveying the prepolymer slurry containing insoluble matters into the filter to filter the insoluble matters to obtain transparent prepolymer slurry;
the discharge port of the filter is communicated with the feed port of the third buffer stirring tank through a pipeline, the discharge port of the third buffer stirring tank is connected with the first feed port of the second screw reactor 10 through a pipeline and a pump, the second feed port of the second screw reactor 10 is communicated with an aromatic acyl chloride feed pipeline and is used for adding aromatic acyl chloride into transparent prepolymer slurry in the second screw reactor 10 to carry out post polycondensation reaction to obtain polymer slurry, the discharge port of the second screw reactor 10 is provided with the third feed port, and the third feed port is communicated with an organic base feed pipeline and is used for carrying out secondary neutralization on the prepared polymer slurry to obtain a finished product aramid fiber slurry;
The discharge port of the second screw reactor 10 is communicated with the first feed port of the fourth buffer stirring tank and is used for storing the finished aramid fiber slurry;
preferably, a second feeding port is arranged on the fourth buffer stirring tank, and the second feeding port is communicated with an aromatic acyl chloride feeding pipeline and is used for adding acyl chloride according to the polymerization state to adjust the viscosity of the finished aramid fiber slurry.
Preferably, the mixing kettle 1, the first buffer stirring tank, the second buffer stirring tank, the third buffer stirring tank and the fourth buffer stirring tank are all provided with liquid level meters, the bottom of each mixing kettle is provided with a regulating valve, and when the liquid level is about 50%, the regulating valves control the solution in the device to be conveyed to the next working procedure.
Preferably, the level gauge is a flange flowmeter or a radar level gauge.
Preferably, the first screw reactor 2 is a twin screw extruder.
Preferably, the first buffer stirring tank at least comprises a first reaction kettle 3 and a second reaction kettle 4 which are connected in parallel, and a plurality of reaction kettles can be arranged between the first reaction kettle 3 and the second reaction kettle 4 for parallel use; the second buffer stirring tank is a third reaction kettle 6; the third buffer stirring tank is a fourth reaction kettle 9; the fourth buffer stirring tank at least comprises a fifth reaction kettle 11 and a sixth reaction kettle 12 which are connected in parallel, and a plurality of reaction kettles can be arranged between the fifth reaction kettle 11 and the sixth reaction kettle 12 for parallel use.
Preferably, the filter is a plate-frame filter, and filter cloth with 100-400 meshes is adopted; the filter at least comprises a first plate frame filter 7 and a second plate frame filter 8 which are connected in parallel, and further, a plurality of plate frame filters can be arranged between the first plate frame filter 7 and the second plate frame filter 8 in parallel.
Preferably, the second screw reactor 10 is a twin screw extruder.
Preferably, the microchannel reactor 5, the first screw reactor 2 and the second screw reactor 10 are connected with a cooling heat exchange system for releasing the reaction heat in the microchannel reactor 5 and the screw reactors.
Preferably, the on-line dynamic viscometer is arranged on the conveying pipeline of the prepolymer slurry and the polymer conveying pipeline, and particularly, the on-line dynamic viscometer is arranged on the pipeline between the first screw reactor 2 and the fourth buffer stirring tank.
Preferably, all material feeding pipelines and conveying pipelines are provided with metering pumps and flow meters;
preferably, the mixing kettle 1, the first reaction kettle 3, the second reaction kettle 4, the third reaction kettle 6, the fourth reaction kettle 9, the fifth reaction kettle 11 and the sixth reaction kettle 12 are all provided with external jackets, a cooling medium or a heating medium is added into the external jackets according to the specific polymerization condition requirement, the lower end of each external jacket is provided with a feed inlet, and the upper end of each external jacket is provided with a discharge outlet;
Preferably, the inside of the mixing kettle 1, the first reaction kettle 3, the second reaction kettle 4, the third reaction kettle 6, the fourth reaction kettle 9, the fifth reaction kettle 11 and the sixth reaction kettle 12 are provided with double-layer double-helical ribbon stirrers, and are all fed from the upper end and discharged from the lower end;
preferably, the first reaction kettle 3, the second reaction kettle 4, the third reaction kettle 6, the fourth reaction kettle 9, the fifth reaction kettle 11 and the sixth reaction kettle 12 can be designed into different specifications according to working condition requirements;
preferably, in the mixing kettle 1, the flow rate of the aromatic diamine solution is 160kg/h to 190kg/h, and the molar ratio of the aromatic diamine solution to the aromatic acyl chloride is 10 (8-9); the stirring rotation speed of the mixing kettle 1 is 20 r/min-50 r/min, and the cavity temperature is-5 ℃ to 10 ℃;
preferably, in the mixing kettle 1, the mass concentration of the input aromatic diamine solution is 8% -13%, preferably 10%, and the solvent is a polar organic solvent, which can be one or more of N, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide, dimethyl sulfoxide and the like;
the neutralizer is ammonia gas;
the organic base is methylamine, dimethylamine, ethylamine or diethylamine, preferably diethylamine;
preferably, the flow rate of the first screw reactor 2 is 185.56 kg-227.15 kg, the cavity temperature is-5 ℃ to 10 ℃, and the materials stay in the first screw reactor 2 for 50 s-100 s;
Preferably, the stirring rotation speed of the first buffer stirring tank is 20 r/min-50 r/min;
preferably, the flow rate of the microchannel reactor 5 is 185.56 kg/h-227.15 kg/h;
preferably, the stirring rotating speed of the second buffer stirring tank is 15 r/min-35 r/min;
preferably, the filtering pressure of the filter is 0.5-1 MPa, and the flow is 190-233.4 kg/h;
preferably, in the second screw reactor 10, the flow rate of the transparent prepolymer slurry is 183 kg/h-213.75 kg/h, and the residence time of the transparent prepolymer slurry in the cavity of the second screw reactor 10 is 50 s-100 s; the addition amount of the aromatic acyl chloride is about 10% -20% of the molar addition amount of the initial aromatic diamine solution, and the flow rate of the aromatic acyl chloride is 3.3 kg/h-9.273 kg/h; the flow rate of the organic alkali is 1.74kg/h to 5.13kg/h, and the PH value is regulated to 7 to 8;
preferably, the stirring rotating speed of the fourth buffer stirring tank is 15 r/min-35 r/min.
According to the invention, continuous polymerization is adopted to realize multi-device serial operation, an aromatic diamine solution, aromatic acyl chloride and corresponding auxiliary raw materials which are added according to requirements are added into a mixing kettle 1 according to initial formula requirements when other functional pulp is prepared, the mixed raw materials are premixed by the mixing kettle 1 and then discharged to a first screw reactor 2 through the lower end of the mixing kettle 1, prepolymer pulp is formed in the first screw reactor 2, the prepolymer pulp is discharged to a first reaction kettle 3 and a second reaction kettle 4, the prepolymer pulp is buffered by the first reaction kettle 3 and the second reaction kettle 4 and then enters a micro-channel reactor 5, meanwhile, ammonia gas and the prepolymer pulp are introduced into the micro-channel reactor 5 to obtain prepolymer pulp containing insoluble substances, the prepolymer pulp which is buffered in the third reaction kettle 6 is conveyed to a first plate-frame filter 7 and a second plate-frame filter 8 through a gear pump, the transparent prepolymer pulp is obtained by filtering, the transparent prepolymer pulp is buffered in a fourth reaction kettle 9, the prepolymer pulp is conveyed to a fifth reaction kettle 10 through a second pump, the pH value of the aramid fiber pulp is obtained by the second screw reactor 10, the pH value of the final product pulp is obtained by adding the aramid fiber pulp into a fifth reaction kettle 11, and finally, and the final product pulp is subjected to the final polycondensation.
The pre-polycondensation is carried out in the first screw reactor 2, 80% -90% of the total raw materials are subjected to the pre-polymerization reaction at the moment, a large amount of heat can be released, the heat exchange efficiency of the first screw reactor 2 is high, the heat generated in the polymerization reaction process can be rapidly dissipated, the rest 10% -20% of the raw materials react with the prepolymer slurry with certain viscosity in the second screw reactor 10 to rapidly generate the finished aramid fiber slurry with high viscosity suitable for spinning, and the advantage of stirring and mixing the high-viscosity polymerization slurry by adopting the second screw reactor 10 is reflected at the moment;
when the system for producing aramid fiber slurry by continuous polymerization with multiple devices is used, the concrete steps are as follows:
1. proportioning and feeding:
the method comprises the steps of (1) injecting an aromatic diamine solution and aromatic acyl chloride with a molar ratio of 10 (8-9) into a mixing kettle 1 through respective raw material pipelines by respective feeding flow meters, wherein the flow rate of the aromatic diamine solution in the mixing kettle 1 is 160 kg/h-190 kg/h, the stirring rotation speed is 20 r/min-50 r/min, the mixing kettle 1 is stirred after raw material injection is started, the cavity temperature of the mixing kettle 1 is controlled to be minus 5 ℃ to 10 ℃ through jacket refrigerants, and after the liquid level of the mixing kettle 1 reaches 50%, the mixed solution is transferred into a first screw reactor 2 through a gear pump at a flow rate of 185.56 kg/h-227.15 kg/h for pre-polycondensation.
2. Pre-polycondensation
Controlling the mixed solution to stay for 50-100 s in the first screw reactor 2, controlling the temperature of the cavity of the first screw reactor 2 to be-5-10 ℃, primarily obtaining prepolymer slurry through the first screw reactor 2, storing the prepolymer slurry in a first buffer stirring tank, wherein the first buffer stirring tank has a buffer function on one hand, and continuously reacting in the stay process if the prepolymer slurry does not completely react after entering the first buffer stirring tank on the other hand;
3. neutralization reaction
Injecting the prepolymer slurry in the first buffer stirring tank into the microchannel reactor 5 through a gear pump according to the flow rate of 185.56 kg/h-227.15 kg/h, and simultaneously introducing ammonia gas of 4.98 m/h-8.1 m/h into the microchannel reactor 5 to neutralize the prepolymer slurry to obtain prepolymer slurry containing insoluble matters, and storing the prepolymer slurry containing insoluble matters in the second buffer stirring tank;
4. filtration
Continuously stirring the prepolymer slurry containing insoluble matters in the second buffer stirring tank to prevent sedimentation and layering, injecting the prepolymer slurry containing insoluble matters in the second buffer stirring tank into a filter through a gear pump at the stirring speed of 15-35 r/min, filtering out the generated insoluble matters at the filtering pressure of 0.5-1 MPa and the flow rate of 190-233.4 kg/h to obtain transparent prepolymer slurry, and storing the transparent prepolymer slurry in a third buffer stirring tank;
5. Finished aramid fiber slurry
The transparent prepolymer slurry in the third buffer stirring tank is fed into a second screw reactor 10 through a gear pump, the flow rate of the second screw reactor 10 is 183 kg/h-226.18 kg/h, the cavity temperature is 15-35 ℃, at this time, aromatic acyl chloride is fed into the second screw reactor 10 through a second feed inlet, the adding amount of the aromatic acyl chloride is 10-20% of the molar adding amount of the aromatic diamine solution, the flow rate of the aromatic acyl chloride is 3.3 kg/h-9.273 kg/h, the transparent prepolymer slurry and the aromatic acyl chloride are subjected to post polycondensation, finally, organic alkali is fed into the second screw reactor 10 through a third feed inlet for carrying out a second neutralization reaction, and finally, the finished aramid fiber slurry is stored in a fourth buffer stirring tank, the flow rate of the organic alkali is 1.74 kg/h-5.13 kg/h, and the residence time of the transparent slurry in the cavity of the second screw reactor 10 is 50 s-100 s.
Example 1
M-phenylenediamine is dissolved in N, N-dimethylacetamide DMAC to prepare a 10% m-phenylenediamine solution. M-phenylenediamine and isophthaloyl dichloride with the molar ratio of 10:8 are respectively injected into a mixing kettle 1 through a feeding pipeline according to the ratio by a metering pump, the flow rate of the m-phenylenediamine solution is 190kg/h, the flow rate of the molten isophthaloyl dichloride is 28.58kg/h, the stirring speed of the mixing kettle 1 is 50r/min, the injection flow rate of the mixing kettle 1 is 218.58kg/h, and the temperature of the mixing kettle 1 is controlled at-5 ℃. After the liquid level of the mixing tank 1 reached 50%, a gear pump was started to feed the mixed liquid into the first screw reactor 2 at a flow rate of 218.58 kg/h.
The axial pushing speed of the first screw reactor 2 is regulated, so that the mixed solution from the mixing kettle 1 stays in the screw cavity for 100s, the cavity temperature is 10 ℃, the mixed solution enters the first reaction kettle 3 and the second reaction kettle 4 for storage, the stirring rotating speed of the reaction kettle is 20r/min, and the viscosity value of the polymer solution is 10Po.
After the liquid level of the first reaction kettle 3 reaches 50%, the liquid is conveyed into the micro-channel reactor 5 through a tank bottom pipeline by a centrifugal pump, the flow of the micro-channel reactor 5 is 218.58kg/h, and meanwhile, 6.23 m/h ammonia gas is input into the micro-channel reactor 5 through a feed pipe for neutralization.
The neutralized prepolymer slurry was stored in a third reactor 6, the stirring rotation speed of the third reactor 6 was 35r/min, after the liquid level in the third reactor 6 reached 50%, the valve at the bottom of the tank was opened, and the prepolymer slurry was pressed into a plate-and-frame filter using 300 mesh filter cloth by means of a gear pump flow rate 223.96kg/h, at a pressure of 1MPa. Finally, the fourth reaction kettle 9 obtains clear and transparent prepolymer slurry, and the stirring rotating speed is 35r/min.
After the liquid level of the fourth reaction kettle 9 reaches 50%, a tank bottom valve is opened, the prepolymer slurry is pressed into the second screw reactor 10 through a screw pump at a flow rate of 207kg/h, the prepolymer slurry stays in the cavity of the second screw reactor 10 for 50s, the cavity temperature is 15 ℃, isophthaloyl dichloride required for finishing polycondensation is added into the second screw reactor 10, the flow rate is 7.13kg/h, after the reaction is completed, the neutralization is performed through adding diethylamine, the flow rate is 5.13kg/h, and finally the neutralized polymer enters the fifth reaction kettle 11 for storage, and the fifth reaction kettle 11 is opened with a stirring paddle at a stirring speed of 15r/min. The final polymer had a ph=7.0 measured by a PH meter, a viscosity 697Po measured at room temperature by a rotational viscometer, a molecular weight of 19.6w measured by a gel chromatograph GPC, and a polymerization efficiency of 80%.
Example 2
M-phenylenediamine is dissolved in DMAC to prepare a 10% m-phenylenediamine solution. M-phenylenediamine and isophthaloyl dichloride with the molar ratio of 10:9 are respectively injected into a mixing kettle 1 through a feeding pipeline according to the ratio by a metering pump, the flow rate of the m-phenylenediamine solution is 175kg/h, the flow rate of the molten isophthaloyl dichloride is 29.6kg/h, the stirring rotating speed of the mixing kettle 1 is 35r/min, the injection flow rate of the mixing kettle 1 is 194.6kg/h, and the temperature of the mixing kettle 1 is controlled at 10 ℃. After the liquid level of the mixing kettle 1 reached 50%, a gear pump was started to deliver the mixed liquid into the double screw reactor at a flow rate of 194.6 kg/h.
The axial pushing speed of the first screw reactor 2 is regulated, so that the mixed solution from the mixing kettle 1 stays in the screw cavity for 75 seconds, the cavity temperature is minus 5 ℃, the mixed solution enters the first reaction kettle 3 and the second reaction kettle 4 for storage, the stirring rotating speed of the reaction kettle is 40r/min, and the viscosity value of the polymer solution is conveyed out of the reaction kettle to be 3Po.
After the liquid level of the first reaction kettle 3 reaches 50%, the liquid is conveyed into the micro-channel reactor 5 through a tank bottom pipeline by a centrifugal pump, the flow of the micro-channel reactor 5 is 194.6kg/h, and meanwhile, 6.45 m/h ammonia gas is input into the micro-channel reactor 5 through a feed pipe for neutralization.
The neutralized prepolymer slurry was stored in a third reactor 6, the stirring rotation speed of the third reactor 6 was 20r/min, after the liquid level in the third reactor 6 reached 50%, the bottom valve was opened, and the prepolymer slurry was pressed into a plate-and-frame filter using 100 mesh filter cloth by using a gear pump flow rate of 206.28kg/h, at a pressure of 0.5MPa. Finally, the fourth reaction kettle 9 obtains clear and transparent prepolymer slurry, and the stirring rotating speed is 20r/min.
After the liquid level of the fourth reaction kettle 9 reaches 50%, a tank bottom valve is opened, and the prepolymer slurry is pressed into the second screw reactor 10 by a screw pump at a flow rate of 190kg/h, so that the prepolymer slurry stays in the cavity of the second screw reactor 10 for 75s, the cavity temperature is 21 ℃, the isophthaloyl dichloride required for the post polycondensation is added into the second screw reactor 10, and the flow rate is 3.3kg/h. After the reaction is completed, diethylamine is added for neutralization, the flow is 2.375kg/h, and finally the neutralized polymer enters a fifth reaction kettle 11 for storage, and the fifth reaction kettle 11 is started with a stirring paddle, and the stirring speed is 20r/min. The final polymer had a ph=8.0 measured by a PH meter, a viscosity 732Po measured at room temperature by a rotational viscometer, a molecular weight of 18.9w measured by a gel chromatograph GPC, and a polymerization efficiency of 78%.
Example 3
M-phenylenediamine is dissolved in DMAC to prepare a 10% m-phenylenediamine solution. M-phenylenediamine and isophthaloyl dichloride with the molar ratio of 10:8.5 are respectively injected into a mixing kettle 1 through a feeding pipeline according to the ratio by a metering pump, the flow of the m-phenylenediamine solution is 160kg/h, the flow of the molten isophthaloyl dichloride is 25.56kg/h, the stirring rotating speed of the mixing kettle 1 is 20r/min, the injection flow of the mixing kettle 1 is 185.56kg/h, and the temperature of the mixing kettle 1 is controlled at 0 ℃. After the liquid level of the mixing tank 1 reached 50%, a gear pump was started to feed the mixed liquid into the first screw reactor 2 at a flow rate of 185.56 kg/h.
The axial pushing speed of the first screw reactor 2 is regulated, so that the mixed solution from the mixing kettle 1 stays in the screw cavity for 50s, the cavity temperature is 0 ℃, the mixed solution enters the first reaction kettle 3 and the second C2 for storage, the stirring rotating speed of the reaction kettle is 50r/min, and the viscosity value of the polymer solution is conveyed out of the reaction kettle to be 1Po.
After the liquid level of the first reaction kettle 3 reaches 50%, the liquid is conveyed into the micro-channel reactor 5 through a tank bottom pipeline by a centrifugal pump, the flow of the micro-channel reactor 5 is 185.56kg/h, and meanwhile, ammonia gas with the flow of 5.56 m/h is input into the micro-channel reactor 5 through a feed pipe for neutralization.
The prepolymer slurry after neutralization is stored in a third reaction kettle 6, the stirring rotation speed of the third reaction kettle 6 is 15r/min, after the liquid level in the third reaction kettle 6 reaches 50%, a valve at the bottom of the kettle is opened, and the prepolymer slurry is pressed into a plate-and-frame filter using 400-mesh filter cloth by using a gear pump with the flow rate of 190.1kg/h, and the pressure is 0.75MPa. Finally, the fourth reaction kettle 9 obtains clear and transparent prepolymer slurry, and the stirring rotating speed is 15r/min.
After the liquid level of the fourth reaction kettle 9 reaches 50%, a tank bottom valve is opened, and the prepolymer slurry is pressed into the second screw reactor 10 by a screw pump at a flow rate of 183kg/h, so that the prepolymer slurry stays in the cavity of the second screw reactor 10 for 100s, the cavity temperature is 35 ℃, and the isophthaloyl dichloride required for post polycondensation is added into the second screw reactor 10 at a flow rate of 4.52kg/h. After the reaction is completed, diethylamine is added for neutralization, the flow is 3.26kg/h, and finally the neutralized polymer enters a fifth reaction kettle 11 for storage, and the fifth reaction kettle 11 is started with a stirring paddle, and the stirring speed is 35r/min. The final polymer had a ph=7.5 measured by a PH meter, a viscosity 721Po measured by a rotational viscometer, a molecular weight of 19.4w measured by a gel chromatograph GPC, and a polymerization efficiency of 84%.
Example 4
M-phenylenediamine is dissolved in N-methyl pyrrolidone NMP to prepare m-phenylenediamine solution with the concentration of 8 percent. M-phenylenediamine and isophthaloyl dichloride with the molar ratio of 10:8 are respectively injected into a mixing kettle 1 through a feeding pipeline according to the ratio by a metering pump, the flow rate of the m-phenylenediamine solution is 190kg/h, the flow rate of the molten isophthaloyl dichloride is 22.86kg/h, the stirring rotating speed of the mixing kettle 1 is 40r/min, the injection flow rate of the mixing kettle 1 is 212.86kg/h, and the temperature of the mixing kettle 1 is controlled at-1 ℃. After the liquid level of the mixing tank 1 reached 50%, a gear pump was started to feed the mixed liquid into the first screw reactor 2 at a flow rate of 212.86 kg/h.
The axial pushing speed of the first screw reactor 2 is regulated, so that the mixed solution from the mixing kettle 1 stays in the screw cavity for 80s, the cavity temperature is 8 ℃, the mixed solution enters the first reaction kettle 3 and the second reaction kettle 4 for storage, the stirring rotating speed of the reaction kettle is 22r/min, and the viscosity value of the polymer solution is 7Po.
After the liquid level of the first reaction kettle 3 reaches 50%, the liquid is conveyed into the micro-channel reactor 5 through a tank bottom pipeline by a centrifugal pump, the flow of the micro-channel reactor 5 is 212.86kg/h, and meanwhile, ammonia gas with the flow of 4.98 m/h is input into the micro-channel reactor 5 through a feed pipe for neutralization.
The neutralized prepolymer slurry was stored in a third reactor 6, the stirring rotation speed of the third reactor 6 was 35r/min, after the liquid level in the third reactor 6 reached 50%, the valve at the bottom of the tank was opened, and the prepolymer slurry was pressed into a plate-and-frame filter using 200 mesh filter cloth by means of a gear pump flow rate 179.17kg/h, at a pressure of 0.8MPa. Finally, the fourth reaction kettle 9 obtains clear and transparent prepolymer slurry, and the stirring rotating speed is 35r/min.
After the liquid level of the fourth reaction kettle 9 reaches 50%, a tank bottom valve is opened, the prepolymer slurry is pressed into the second screw reactor 10 through a screw pump at a flow rate of 165.6kg/h, the prepolymer slurry stays in the cavity of the second screw reactor 10 for 55s, the cavity temperature is 18 ℃, isophthaloyl dichloride required for finishing polycondensation is added into the second screw reactor 10, the flow rate is 5.7kg/h, after the reaction is completed, the neutralization is performed by adding methylamine, the flow rate is 1.74kg/h, and finally the neutralized polymer enters the fifth reaction kettle 11 for storage, and the fifth reaction kettle 11 is opened with a stirring paddle at a stirring speed of 15r/min. The final polymer had a ph=7.2 measured by a PH meter, a viscosity 703Po measured at room temperature by a rotational viscometer, a molecular weight of 19.9w measured by a gel chromatograph GPC, and a polymerization efficiency of 85%.
Example 5
M-phenylenediamine is dissolved in N, N-dimethylformamide DMF to prepare a 13% m-phenylenediamine solution. M-phenylenediamine and isophthaloyl dichloride with the molar ratio of 10:8 are respectively injected into a mixing kettle 1 through a feeding pipeline according to the ratio by a metering pump, the flow rate of the m-phenylenediamine solution is 190kg/h, the flow rate of the molten isophthaloyl dichloride is 37.15kg/h, the stirring rotating speed of the mixing kettle 1 is 43r/min, the injection flow rate of the mixing kettle 1 is 227.15kg/h, and the temperature of the mixing kettle 1 is controlled at 5 ℃. After the liquid level of the mixing tank 1 reached 50%, a gear pump was started to feed the mixed liquid into the first screw reactor 2 at a flow rate of 227.15 kg/h.
The axial pushing speed of the first screw reactor 2 is regulated, so that the mixed solution from the mixing kettle 1 stays in the screw cavity for 90s, the cavity temperature is 8 ℃, the mixed solution enters the first reaction kettle 3 and the second reaction kettle 4 for storage, the stirring rotating speed of the reaction kettle is 25r/min, and the viscosity value of the polymer solution is conveyed out of the reaction kettle to be 6Po.
After the liquid level of the first reaction kettle 3 reaches 50%, the liquid is conveyed into the micro-channel reactor 5 through a tank bottom pipeline by a centrifugal pump, the flow of the micro-channel reactor 5 is 227.15kg/h, and meanwhile, 8.1 m/h ammonia gas is input into the micro-channel reactor 5 through a feed pipe for neutralization.
The neutralized prepolymer slurry was stored in a third reactor 6, the stirring rotation speed of the third reactor 6 was 35r/min, after the liquid level in the third reactor 6 reached 50%, the valve at the bottom of the tank was opened, and the prepolymer slurry was pressed into a plate-and-frame filter using 300 mesh filter cloth by means of a gear pump flow rate 233.4kg/h, at a pressure of 1MPa. Finally, the fourth reaction kettle 9 obtains clear and transparent prepolymer slurry, and the stirring rotating speed is 35r/min.
After the liquid level of the fourth reaction kettle 9 reaches 50%, a tank bottom valve is opened, the prepolymer slurry is pressed into the second screw reactor 10 through a screw pump at a flow rate of 213.75kg/h, the prepolymer slurry stays in the cavity of the second screw reactor 10 for 50s, the cavity temperature is 15 ℃, isophthaloyl dichloride required for finishing polycondensation is added into the second screw reactor 10, the flow rate is 9.273kg/h, after the reaction is completed, the neutralization is performed by adding dimethylamine, the flow rate is 3.16kg/h, and finally the neutralized polymer enters the fifth reaction kettle 11 for storage, and the fifth reaction kettle 11 is opened with a stirring paddle at a stirring speed of 15r/min. The final polymer had a ph=7.0 measured by a PH meter, a viscosity 732Po measured at room temperature by a rotational viscometer, and a molecular weight 19.2w measured by a gel chromatograph GPC, and a polymerization efficiency of 83%.
Example 6
M-phenylenediamine is dissolved in dimethyl sulfoxide to prepare a 10% m-phenylenediamine solution. M-phenylenediamine and isophthaloyl dichloride with the molar ratio of 10:8 are respectively injected into a mixing kettle 1 through a feeding pipeline according to the ratio by a metering pump, the flow rate of the m-phenylenediamine solution is 190kg/h, the flow rate of the molten isophthaloyl dichloride is 28.58kg/h, the stirring speed of the mixing kettle 1 is 50r/min, the injection flow rate of the mixing kettle 1 is 218.58kg/h, and the temperature of the mixing kettle 1 is controlled at 3 ℃. After the liquid level of the mixing tank 1 reached 50%, a gear pump was started to feed the mixed liquid into the first screw reactor 2 at a flow rate of 218.58 kg/h.
The axial pushing speed of the first screw reactor 2 is regulated, so that the mixed solution from the mixing kettle 1 stays in the screw cavity for 95s, the cavity temperature is 7 ℃, the mixed solution enters the first reaction kettle 3 and the second reaction kettle 4 for storage, the stirring rotating speed of the reaction kettle is 50r/min, and the viscosity value of the polymer solution is conveyed out of the reaction kettle to be 9Po.
After the liquid level of the first reaction kettle 3 reaches 50%, the liquid is conveyed into the micro-channel reactor 5 through a tank bottom pipeline by a centrifugal pump, the flow of the micro-channel reactor 5 is 218.58kg/h, and meanwhile, 6.23 m/h ammonia gas is input into the micro-channel reactor 5 through a feed pipe for neutralization.
The neutralized prepolymer slurry was stored in a third reactor 6, the stirring rotation speed of the third reactor 6 was 35r/min, after the liquid level in the third reactor 6 reached 50%, the valve at the bottom of the tank was opened, and the prepolymer slurry was pressed into a plate-and-frame filter using 300 mesh filter cloth by means of a gear pump flow rate 223.96kg/h, at a pressure of 1MPa. Finally, the fourth reaction kettle 9 obtains clear and transparent prepolymer slurry, and the stirring rotating speed is 33r/min.
After the liquid level of the fourth reaction kettle 9 reaches 50%, a tank bottom valve is opened, the prepolymer slurry is pressed into the second screw reactor 10 through a screw pump at a flow rate of 207kg/h, the prepolymer slurry stays in the cavity of the second screw reactor 10 for 50s, the cavity temperature is 15 ℃, isophthaloyl dichloride required for finishing polycondensation is added into the second screw reactor 10, the flow rate is 7.13kg/h, after the reaction is completed, the neutralization is performed through adding ethylamine, the flow rate is 3.16kg/h, and finally the neutralized polymer enters the fifth reaction kettle 11 for storage, and the fifth reaction kettle 11 is opened with a stirring paddle at a stirring rotating speed of 15r/min. The final polymer had a ph=7.0 measured by a PH meter, a viscosity 655Po measured at room temperature by a rotational viscometer, a molecular weight 19.1w measured by a gel chromatograph GPC, and a polymerization efficiency 83%.
Comparative example batch polymerization
M-phenylenediamine is dissolved in DMAC to prepare a 10% m-phenylenediamine solution. The m-phenylenediamine and the m-phthaloyl chloride with the molar ratio of 10:9 are respectively input into a reaction kettle A through a feed pipeline, 290kg of m-phenylenediamine solution is directly added into the reaction kettle A for prepolymerization, the temperature is controlled at 0 ℃, the stirring speed is 28r/min, 10m of ammonia gas is added for neutralization, after the neutralization is finished, the prepolymer solution is filtered through a 100-mesh plate frame under the pressure of 0.5MPa, the filtered prepolymer is transferred to a reaction kettle B, then 5.51kg of m-phthaloyl chloride is added for finishing polycondensation, the temperature is controlled at 15 ℃, the stirring speed is 28r/min, and then 3.96kg of diethylamine is added for neutralization, so that the polymerization slurry with the PH=7.1, the viscosity 698Po, the molecular weight of 17.8w and the polymerization efficiency of 65% are finally obtained.
The batch polymerization reaction is carried out in stages, the reaction mixture enters a reaction kettle B after the reaction of the reaction kettle A is finished, the conventional production time is about 20 hours for one batch, and about 300kg of slurry is prepared; in the preparation process, a certain link is different, so that the quality of the final polymerization slurry is easy to fluctuate, the continuous polymerization of the invention is to continuously introduce raw materials into a system, continuously introduce continuous reaction, calculate by introducing 160kg/h m-phenylenediamine solution at the lowest, and produce 3584kg of slurry in 20 hours, and the single reaction efficiency is much higher. In addition, each batch of continuous polymerization has no stop, and the reaction process can be regulated according to the state of the intermediate process, so that the stability of the quality of the final polymerization slurry is ensured.
In summary, the system and the method for producing aramid fiber slurry by continuous polymerization with the combination of multiple devices, which are disclosed by the invention, have the advantages that the devices continuously work in the reaction process, the continuous operation is realized without shutdown, and the production efficiency is improved. In the polymerization process, the polymer index in each reaction kettle is effectively controlled, so that the polymerization efficiency can be obviously improved and the product index can be timely adjusted.
Claims (10)
1. A method for producing aramid fiber slurry by continuous polymerization with multiple devices is characterized by comprising the following specific steps:
s1: setting the flow rate of an aromatic diamine solution to be 160 kg/h-190 kg/h, mixing the aromatic diamine solution and aromatic acyl chloride with the molar ratio of 10:8-9, and then introducing the mixture into a first screw reactor (2) to obtain prepolymer slurry;
the flow rate of the first screw reactor (2) is 185.56 kg/h-227.15 kg/h, the cavity temperature is-5 ℃ to 10 ℃, and the mixed raw materials stay in the first screw reactor (2) for 50 s-100 s;
s2: introducing the prepolymer slurry and a neutralizing agent into a microchannel reactor (5) for a first neutralization reaction to obtain a prepolymer slurry containing insoluble matters;
the flow of the micro-channel reactor (5) is 185.56 kg/h-227.15 kg/h, and the flux of the neutralizer is 4.98-8.1 m-bar;
s3: introducing the prepolymer slurry containing insoluble matters into a filter for filtering to obtain transparent prepolymer slurry;
The filtering pressure of the filter is 0.5-1 MPa, and the flow is 190-233.4 kg/h;
s4: introducing transparent prepolymer slurry and aromatic acyl chloride into a second screw reactor (10) for post-polycondensation reaction to obtain polymerization slurry, introducing organic alkali into the second screw reactor (10) for secondary neutralization reaction with the polymerization slurry, and obtaining the finished aramid fiber slurry at a discharge port of the second screw reactor (10);
the cavity temperature of the second screw reactor (10) is 15-35 ℃, the flow rate of the transparent prepolymer slurry is 183-213.75 kg/h, and the residence time of the transparent prepolymer slurry in the cavity of the second screw reactor (10) is 50-100 s;
the addition amount of the aromatic acyl chloride is 10% -20% of the molar addition amount of the aromatic diamine solution, and the flow rate of the aromatic acyl chloride is 3.3 kg/h-9.273 kg/h;
the flow rate of the organic alkali is 1.74kg/h to 5.13kg/h.
2. The method for producing aramid fiber slurry by continuous polymerization with multi-device combination according to claim 1, wherein the mass concentration of the aromatic diamine solution is 8% -13%, and a polar organic solvent is adopted, including at least one of N, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide and dimethyl sulfoxide;
The neutralizer is ammonia gas;
the organic base is methylamine, dimethylamine, ethylamine or diethylamine.
3. The system for using the method for producing aramid fiber slurry by continuous polymerization of any one of claims 1-2 in combination, which is characterized by comprising a first screw reactor (2), a microchannel reactor (5), a filter and a second screw reactor (10), wherein a feed port of the first screw reactor (2) is communicated with a mixed raw material feed line for introducing a mixed liquid of an aromatic diamine solution and an aromatic acyl chloride, a discharge port of the first screw reactor (2) is communicated with a first feed port of the microchannel reactor (5), a second feed port of the microchannel reactor (5) is communicated with a neutralizer feed line, a discharge port of the microchannel reactor (5) is communicated with a feed port of the filter, a feed port of the second screw reactor (10) is provided with a first feed port and a second feed port, a discharge port of the filter is communicated with a first feed port of the second screw reactor (10), a discharge port of the second screw reactor (10) is communicated with a second feed port of the third screw reactor, and a feed port of the third screw reactor is provided with a feed port of the aromatic acyl chloride.
4. A system according to claim 3, further comprising a mixing kettle (1), wherein the feed inlet of the mixing kettle (1) is respectively communicated with the feed lines of the aromatic diamine solution and the aromatic acyl chloride, and the discharge outlet of the mixing kettle (1) is communicated with the feed inlet of the first screw reactor (2) through a mixed raw material feed line for introducing mixed raw materials into the first screw reactor (2) for carrying out a prepolymerization reaction;
the stirring rotating speed of the mixing kettle (1) is 20-50 r/min, and the cavity temperature is-5-10 ℃;
the mixing kettle (1) is externally provided with an outer jacket, a double-layer double-spiral stirrer is arranged in the mixing kettle, a liquid level meter is arranged on the mixing kettle (1), and a regulating valve is arranged at a discharge hole.
5. The system of claim 3, further comprising a first buffer agitator tank, a second buffer agitator tank, a third buffer agitator tank, and a fourth buffer agitator tank, wherein the agitation speed of the first buffer agitator tank is 20r/min to 50r/min, the agitation speeds of the second buffer agitator tank, the third buffer agitator tank, and the fourth buffer agitator tank are all 15r/min to 35r/min, the feed port of the first buffer agitator tank is in communication with the discharge port of the first screw reactor (2), the discharge port of the first buffer agitator tank is in communication with the feed port of the microchannel reactor (5), the feed port of the second buffer agitator tank is in communication with the feed port of the filter, the feed port of the third buffer agitator tank is in communication with the discharge port of the filter, the feed port of the third buffer agitator tank is in communication with the first feed port of the second screw reactor (10), and the feed port of the fourth buffer agitator tank is in communication with the discharge port of the second screw reactor (10).
6. The system of claim 5, wherein the first buffer stirring tank, the second buffer stirring tank, the third buffer stirring tank and the fourth buffer stirring tank are all externally provided with an outer jacket, the inside is all provided with double-layer double-helical ribbon stirrers, the four buffer stirring tanks are all provided with liquid level meters, the discharge ports are all provided with regulating valves, and the first buffer stirring tank and the fourth buffer stirring tank are all a plurality of parallel reaction kettles.
7. The system of claim 6, wherein the fourth buffer agitator tank is provided with a second feed port, the second feed port being in communication with an aromatic acid chloride feed line.
8. A system according to claim 3, wherein the filter comprises a plurality of parallel plate and frame filters, the plate and frame filters using 100 mesh to 400 mesh filter cloth.
9. A system according to claim 3, characterized in that the first screw reactor (2) and the second screw reactor (10) are both twin screw extruders.
10. A system according to claim 3, characterized in that the first screw reactor (2), the microchannel reactor (5) and the second screw reactor (10) are connected with cooling heat exchange systems, and the connecting lines of the first screw reactor (2), the microchannel reactor (5), the filter and the second screw reactor (10) are provided with on-line dynamic viscosimeters.
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