WO2017181761A1 - 一种对苯二胺的连续溶解装置及方法 - Google Patents

一种对苯二胺的连续溶解装置及方法 Download PDF

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Publication number
WO2017181761A1
WO2017181761A1 PCT/CN2017/073850 CN2017073850W WO2017181761A1 WO 2017181761 A1 WO2017181761 A1 WO 2017181761A1 CN 2017073850 W CN2017073850 W CN 2017073850W WO 2017181761 A1 WO2017181761 A1 WO 2017181761A1
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Prior art keywords
phenylenediamine
continuous dissolution
continuous
dissolution
kettle
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PCT/CN2017/073850
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English (en)
French (fr)
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庹新林
崔庆海
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山东万圣博科技股份有限公司
清华大学
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Publication of WO2017181761A1 publication Critical patent/WO2017181761A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/87—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis the receptacle being divided into superimposed compartments
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F21/00—Dissolving
    • B01F21/10—Dissolving using driven stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
    • B01F27/625—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis the receptacle being divided into compartments, e.g. with porous divisions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
    • B01F27/70—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis with paddles, blades or arms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/80—Forming a predetermined ratio of the substances to be mixed
    • B01F35/88—Forming a predetermined ratio of the substances to be mixed by feeding the materials batchwise
    • B01F35/881—Forming a predetermined ratio of the substances to be mixed by feeding the materials batchwise by weighing, e.g. with automatic discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F35/92—Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners

Definitions

  • the invention belongs to the technical field of polymer synthesis, and relates to a continuous dissolution device and method for p-phenylenediamine, in particular to a method A continuous dissolution apparatus and method for monomeric p-phenylenediamine in a continuous polymerization process of a para-aramid fiber resin.
  • Para-aramid fiber is a high-performance fiber with many properties such as high strength, high modulus, high temperature resistance and solvent resistance, and has important applications in defense and civil applications.
  • PPTA polyparaphenylene terephthalamide
  • the polymerization method is a low temperature solution polycondensation method. That is, low temperature polymerization of monomeric terephthaloyl chloride (TPC) and p-phenylenediamine (PPD) in a suitable solvent system.
  • TPC monomeric terephthaloyl chloride
  • PPD p-phenylenediamine
  • the dissolution of the monomer p-phenylenediamine and the manner of adding the reaction are very important for achieving continuous stable polymerization of PPTA.
  • PPD The activity is high and easy to oxidize, and the oxidation products have strong dyeing properties. Therefore, the dissolution mode of PPD is unreasonable, which not only affects the polymer PPTA.
  • the present invention proposes a new apparatus and method for continuously dissolving p-phenylenediamine, that is, continuous dissolution of PPD instead of the usual intermittent dissolution, thereby All processes of PPTA polymerization are continuous operation, and by continuously dissolving PPD, the effect of PPD oxidative discoloration on the quality stability of PPTA is eliminated, thereby ensuring PPTA. Quality stability.
  • a continuous dissolution device for p-phenylenediamine comprising a weighing system, a dissolution system, a cooling system and a storage system;
  • the weighing system includes a silo; Weighing system All silos and pipelines are protected by high-purity nitrogen; the weighing system is capable of continuously and accurately measuring the weight of the PPD, preferably a high-precision weightless scale.
  • the dissolution system comprises a continuous dissolution kettle, a continuous dissolution kettle is provided with a feed port, a gas inlet, a discharge port and a gas outlet; the continuous dissolution kettle is provided with a stirring device and a grid; the stirring device comprises a motor, Mixing shaft and stirring blade; said The grille is a porous disc fixed on the wall of the kettle; the stirring shaft passes through the center of the grille and maintains a gap of 1-10 mm with the grille;
  • the silo is connected to the feed port through a pipeline
  • the discharge port is sequentially connected to the cooling system and the storage system through a pipeline.
  • the continuous dissolution vessel may be vertical or horizontal, preferably horizontal.
  • the gap between the paddle and the continuous dissolution kettle wall is maintained at 1-10mm to enable solids PPD It is better to stir without rubbing against the wall.
  • the continuous dissolution vessel may be cooled by an outer jacket or may be omitted, which is not preferred.
  • the continuous dissolution kettle is protected by high purity nitrogen gas.
  • the feed port is located at the top of the continuous dissolution vessel near the side of the motor, and the discharge port is located at the bottom or side wall of the other end of the continuous dissolution vessel, preferably the side wall is discharged to reduce solids. The risk of PPD being brought out.
  • the main unit is still composed of a stirring device and a grid, except that the feed port and the high-purity nitrogen vent are changed to the top.
  • the continuous dissolution kettle has an aspect ratio of 5:1 to 10:1.
  • the cooling system of the present invention may be a vertical or horizontal heat exchanger commonly used in the industry.
  • the amount of cooling is controlled to continuously cool the dissolved material to a specified temperature.
  • Nitrogen gas is introduced into the whole device through the air inlet, the p-phenylenediamine powder is added to the silo of the weighing system, and the weighing system is continuously and stably added to the continuous dissolution kettle to add p-phenylenediamine; at the same time, Prepared with high precision metering pump
  • the N-methylpyrrolidone/calcium chloride solution is continuously and stably delivered to the continuous dissolution vessel through the feed port; the stirring of the continuous dissolution vessel is started, and the rotation speed is controlled at 10-150 rpm. Open the discharge pump to deliver the dissolved material to the cooling system and cool it to -5-5 °C, then store the dissolved and cooled material in the storage system for later use.
  • the apparatus and method for continuously dissolving monomer p-phenylenediamine in a continuous polymerization process of a para-aramid fiber resin proposed by the present invention have the following advantages: PPD eliminates the influence of PPD oxidation on the quality of PPTA resin in a continuous dissolution mode, and achieves the stability of PPD dissolution quality, which not only ensures the stability of PPTA molecular weight, but also ensures PPTA resin color consistency, which lays a solid foundation for the subsequent aramid fiber quality stability.
  • Figure 1 is a schematic view showing the structure of a continuous dissolution apparatus of p-phenylenediamine according to the present invention
  • a continuous dissolution device for p-phenylenediamine comprising a weighing system, a dissolution system, a cooling system and a storage system;
  • the weighing system includes a silo 1;
  • the dissolution system comprises a continuous dissolution kettle 2, and the continuous dissolution kettle 2 is provided with a feed port 3, a gas inlet 4, and a discharge port 5 And a gas outlet 6; a continuous stirring tank 2 is provided with a stirring device and a grid 7; the stirring device comprises a motor 8, a stirring shaft 9 and a stirring blade 10; a porous disc fixed to the wall of the kettle; the agitating shaft 9 passes through the center of the grid 7 and maintains a gap of 1 mm with the grid 7;
  • the silo 1 is connected to the feed port 3 through a pipeline;
  • the discharge port 5 is connected to the cooling system 11 and the storage system 12 in sequence via a pipeline.
  • the continuous dissolution kettle 2 has an aspect ratio of 5:1.
  • the gap between the stirring paddle 1 and the continuous dissolution kettle wall was kept at 1 mm.
  • Nitrogen gas is introduced into the entire apparatus through the gas inlet 3, and the p-phenylenediamine powder is added to the silo of the weighing system.
  • the weighing system is continuously and stably added to the continuous dissolution kettle 2 with p-phenylenediamine; at the same time, the prepared N-methylpyrrolidone/calcium chloride solution is passed through the feed port by using a high-precision metering pump 3 Continuously and stably delivered to the continuous dissolution tank 2; the stirring of the continuous dissolution tank 2 is started, the rotation speed is controlled at 10 rpm; the discharge delivery pump is turned on, 13 and the dissolved material is sent to the cooling system 11 to be cooled to At -5 °C, the dissolved and cooled material is then stored in storage system 12 for later use.
  • the dissolved and cooled PPD solution is described in the continuous polymerization method described in the patent ZL201210485817.3 with another monomer.
  • the TPC is continuously polymerized, and the final PPTA powder is measured by a Ubbelohde viscometer with a logarithmic viscosity of 6.20.
  • the precision color difference meter continuously detects the PPTA resin powder, and the color difference does not exceed 0.02. .
  • a continuous dissolution device for p-phenylenediamine comprising a weighing system, a dissolution system, a cooling system and a storage system;
  • the weighing system includes a silo 1;
  • the dissolution system comprises a continuous dissolution kettle 2, and the continuous dissolution kettle 2 is provided with a feed port 3, a gas inlet 4, and a discharge port 5 And a gas outlet 6; a continuous stirring tank 2 is provided with a stirring device and a grid 7; the stirring device comprises a motor 8, a stirring shaft 9 and a stirring blade 10; a porous disc fixed to the wall of the kettle; the agitating shaft 9 passes through the center of the grid 7 and maintains a gap of 10 mm with the grid 7;
  • the silo 1 is connected to the feed port 3 through a pipeline;
  • the discharge port 5 is connected to the cooling system 11 and the storage system 12 in sequence via a pipeline.
  • the continuous dissolution kettle 2 has an aspect ratio of 10:1.
  • the gap between the stirring blade 1 and the continuous dissolution kettle wall was kept at 10 mm.
  • Nitrogen gas is introduced into the entire apparatus through the gas inlet 3, and the p-phenylenediamine powder is added to the silo of the weighing system.
  • the weighing system is continuously and stably added to the continuous dissolution kettle 2 with p-phenylenediamine; at the same time, the prepared N-methylpyrrolidone/calcium chloride solution is passed through the feed port by using a high-precision metering pump 3 Continuously and stably transported to the continuous dissolution tank 2; the stirring of the continuous dissolution tank 2 is started, the rotation speed is controlled at 150 rpm; the discharge delivery pump is turned on, 13 and the dissolved material is sent to the cooling system 11 to be cooled to At 5 °C, the dissolved and cooled material is then stored in storage system 12 for later use.
  • the dissolved and cooled PPD solution is described in the continuous polymerization method described in the patent ZL201210485817.3 with another monomer.
  • the TPC was continuously polymerized, and the final PPTA powder was measured by an Ubbelohde viscometer with a logarithmic viscosity of 5.5.
  • the precision color difference meter continuously detected the PPTA resin powder, and the color difference did not exceed 0.02.
  • a continuous dissolution device for p-phenylenediamine comprising a weighing system, a dissolution system, a cooling system and a storage system;
  • the weighing system includes a silo 1;
  • the dissolution system comprises a continuous dissolution kettle 2, and the continuous dissolution kettle 2 is provided with a feed port 3, a gas inlet 4, and a discharge port 5 And a gas outlet 6; a continuous stirring tank 2 is provided with a stirring device and a grid 7; the stirring device comprises a motor 8, a stirring shaft 9 and a stirring blade 10; a porous disc fixed to the wall of the kettle; the agitating shaft 9 passes through the center of the grid 7 and maintains a gap of 5 mm with the grid 7;
  • the silo 1 is connected to the feed port 3 through a pipeline;
  • the discharge port 5 is connected to the cooling system 11 and the storage system 12 in sequence via a pipeline.
  • the continuous dissolution kettle 2 has an aspect ratio of 8:1.
  • the gap between the stirring blade 1 and the continuous dissolution kettle wall was kept at 5 mm.
  • Nitrogen gas is introduced into the entire apparatus through the gas inlet 3, and the p-phenylenediamine powder is added to the silo of the weighing system.
  • the weighing system is continuously and stably added to the continuous dissolution kettle 2 with p-phenylenediamine; at the same time, the prepared N-methylpyrrolidone/calcium chloride solution is passed through the feed port by using a high-precision metering pump 3 Continuously and stably transported to the continuous dissolution tank 2; the agitation of the continuous dissolution tank 2 is started, the rotation speed is controlled at 100 rpm; the discharge delivery pump is turned on, 13 and the dissolved material is sent to the cooling system 11 to be cooled to At 0 °C, the dissolved and cooled material is then stored in storage system 12 for later use.
  • the dissolved and cooled PPD solution is described in the continuous polymerization method described in the patent ZL201210485817.3 with another monomer.
  • the TPC is continuously polymerized, and the final PPTA powder is measured by an Ubbelohde viscometer with a logarithmic viscosity of 7.07.
  • the precision colorimeter continuously detects the PPTA resin powder, and the color difference does not exceed 0.02. .

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polyamides (AREA)

Abstract

一种对苯二胺的连续溶解装置和方法，该装置包括称量系统，溶解系统，冷却系统（11）和储存系统（12）；称量系统包括料仓（1）；溶解系统包括连续溶解釜（2），连续溶解釜（2）上设有进料口（3）、气体进口（4）、出料口（5）以及气体出口（6）；连续溶解釜（2）内设有搅拌装置和格栅（7）；搅拌装置包括电机（8）、搅拌轴（9）和搅拌桨叶（10）；格栅（7）为多孔圆盘，固定在釜壁上；搅拌轴（9）穿过格栅（7）中心，与格栅（7）保持1-10mm间隙；料仓（1）通过管路与进料口（3）连接；出料口（5）通过管路依次与冷却系统（11）和储存系统（12）连接。

Description

一种对苯二胺的连续溶解装置及方法 一种对苯二胺的连续溶解装置及方法
技术领域
本发明属 高分子合成技术领域 ，涉及一种 对苯二胺的连续溶解装置及方法 ，特别涉及一种 对位芳纶纤维用树脂连续聚合过程中单体对苯二胺的连续溶解装置及方法 。
背景技术
对位芳纶纤维是一种高性能纤维，具有高强度、高模量、耐高温和耐溶剂等许多优异性能并在国防及民用领域有重要的应用。 其中连续稳定生产对位芳纶纤维用聚对苯二甲酰对苯二胺（ PPTA ）树脂是其中的关键之一。工业上常用的 PPTA 聚合方法是低温溶液缩聚法。即将单体对苯二甲酰氯（ TPC ）与对苯二胺（ PPD ）在合适的溶剂体系中进行低温聚合反应。到目前为止已有大量的有关 PPTA 低温溶液聚合的报道。但是，如何实现大规模稳定批量聚合生产的报道并不多。
其中，单体对苯二胺的溶解及加入反应的方式对实现 PPTA 连续稳定聚合非常重要。因为 PPD 活性高极易氧化，氧化产物又都具有较强的染色性，所以 PPD 溶解方式不合理，不仅会影响聚合物 PPTA 的分子量，而且会影响聚合产物的色泽，进而会影响对位芳纶纤维的品质。目前常用的 PPD 溶解及处理方式有两种：一是将高纯度 PPD 先搅拌溶解于溶剂 N- 甲基吡咯烷酮（ NMP ）中，然后降温与另一个单体对苯二甲酰氯继续聚合反应；二是将 PPD 加热熔化，然后以喷射或其他方式分散溶解到 NMP 中。这两种方法对于小批量生产来说问题不大，但是对于大批量聚合生产来说就会有问题。因为这两种方法都是间歇溶解 PPD ， PPD 溶解后经过长时间存放会逐渐变色，即使有高纯氮气保护也会发生变色。所以间歇式溶解 PPD 对于保持大批量连续稳定生产的 PPTA 树脂的稳定性不利。
发明内容
为此，本发明提出了一种新的对苯二胺连续溶解装置及方法，即以 PPD 连续溶解来代替常用的间歇式溶解，从而使 PPTA 聚合的所有过程都是连续操作，而且通过将 PPD 连续溶解，消除了 PPD 氧化变色对 PPTA 质量稳定性的影响，进而保证了 PPTA 质量的稳定性。
本发明所述的一种 对苯二胺的连续溶解装置，包括称量系统，溶解系统，冷却系统和储存系统；
所述的称量系统包括料仓； 称量系统所有料仓和管道用高纯度氮气保护；称量系统能够连续稳定准确计量PPD重量，优选高精度失重秤。
所述的溶解系统包括连续溶解釜，连续溶解釜上设有进料口，气体进口，出料口以及气体出口；连续溶解釜内设有搅拌装置和格栅；所述的搅拌装置包括电机、搅拌轴和搅拌桨叶；所述的 格栅为多孔圆盘，固定在釜壁上；搅拌轴穿过格栅中心，与格栅保持 1-10mm 间隙；
所述的料仓通过管路与进料口连接；
所述的出料口通过管路依次与冷却系统和储存系统连接。
连续溶解釜可以是立式，也可以是卧式，优选卧式。桨叶与连续溶解釜壁间隙保持在 1-10mm ，以能够将固体 PPD 搅动而又不会发生与器壁摩擦为宜。为了控制溶解温度，连续溶解釜可以外带夹套降温，也可以不用，以不用为优选。连续溶解釜内通高纯氮气保护。进料口位于靠近电机一侧的连续溶解釜顶端，而出料口位于连续溶解釜另一端的釜底或侧壁，优选侧壁出料以降低固体 PPD 被带出的风险。如果是立式溶解釜，主体装置依然由搅拌装置和格栅组成，只是进料口和高纯氮通气口改到顶端。
为了保证 PPD 的完全溶解，所述的 连续溶解釜长径比为 5:1-10:1 。
本发明所述的冷却系统采用工业上常用的立式或卧式换热器即可。控制制冷量将溶解后的物料连续冷却到规定的温度。
采用本发明所述的装置可以实现 对苯二胺的连续溶解，其具体步骤为：
将氮气通过进气口通入整个装置中，将对苯二胺粉料加入到称重系统的料仓中，开启称重系统连续稳定向连续溶解釜中加入 对苯二胺 ；与此同时，利用高精度计量泵将配制好的 N- 甲基吡咯烷酮 / 氯化钙溶液通过进料口连续稳定输送到连续溶解釜中；开启连续溶解釜的搅拌，控制转速在 10-150rpm ；开启出料输送泵将溶解好的物料输送到冷却系统中冷却到 -5-5 ℃，然后将溶解冷却好的物料储存到 储存系统 中备用。
综上所述，本发明提出的一种对位芳纶纤维用树脂连续聚合过程中单体对苯二胺连续溶解的装置及方法，其优点是： PPD 以连续溶解的方式消除了 PPD 氧化对 PPTA 树脂质量的影响，实现了 PPD 溶解质量的稳定性，不仅可以保证 PPTA 分子量的稳定，而且可以保证 PPTA 树脂色泽一致性，从而为后续芳纶纤维质量稳定性打下坚实基础。
附图说明
图 1 为本发明所述的 对苯二胺的连续溶解装置 结构示意图；
图中： 1 、料仓， 2 、连续溶解釜， 3 、进料口， 4 、气体进口， 5 、出料口， 6 、气体出口， 7 、 格栅，8、 电机， 9 、搅拌轴， 10 、搅拌桨叶， 11 、冷却系统， 12 、储存系统， 13 、出料输送泵。
具体实施方式
下面通过实例对本发明进行进一步说明，但并不因此而限制本发明的内容。
实施例 1
一种 对苯二胺的连续溶解装置，该装置包括称量系统，溶解系统，冷却系统和储存系统；
所述的称量系统包括料仓 1 ；
所述的溶解系统包括连续溶解釜 2 ，连续溶解釜 2 上设有进料口 3 ，气体进口 4 ，出料口 5 以及气体出口 6 ；连续溶解釜 2 内设有搅拌装置和格栅 7 ；所述的搅拌装置包括电机 8 、搅拌轴 9 和搅拌桨叶 10 ；所述的 格栅 7 为多孔圆盘，固定在釜壁上；搅拌轴 9 穿过格栅 7 中心，与格栅 7 保持 1mm 间隙；
所述的料仓 1 通过管路与进料口 3 连接；
所述的出料口 5 通过管路依次与冷却系统 11 和储存系统 12 连接。
所述的 连续溶解釜 2 长径比为 5:1 。
所述的 搅拌 桨叶 1 与 连续溶解釜 壁间隙保持在 1mm 。
利用上述的 对苯二胺的连续溶解装置连续溶解对苯二胺的方法，其具体步骤为：
将氮气通过进气口 3 通入整个装置中，将对苯二胺粉料加入到称重系统的料仓 1 中，开启称重系统连续稳定向连续溶解釜 2 中加入 对苯二胺 ；与此同时，利用高精度计量泵将配制好的 N- 甲基吡咯烷酮 / 氯化钙溶液通过进料口 3 连续稳定输送到连续溶解釜 2 中；开启连续溶解釜 2 的搅拌，控制转速在 10rpm ；开启出料输送泵 13 将溶解好的物料输送到冷却系统 11 中冷却到 -5 ℃，然后将溶解冷却好的物料储存到 储存系统12 中备用。
溶解并冷却后的 PPD 溶液参照专利 ZL201210485817.3 中所述的的连续聚合方法与另一个单体 TPC 连续聚合，最终得到的 PPTA 粉末用乌氏粘度计测定对数比浓粘度为 6.20 ，精密色差仪连续检测 PPTA 树脂粉末，色差不超过 0.02 。
实施例 2
一种 对苯二胺的连续溶解装置，该装置包括称量系统，溶解系统，冷却系统和储存系统；
所述的称量系统包括料仓 1 ；
所述的溶解系统包括连续溶解釜 2 ，连续溶解釜 2 上设有进料口 3 ，气体进口 4 ，出料口 5 以及气体出口 6 ；连续溶解釜 2 内设有搅拌装置和格栅 7 ；所述的搅拌装置包括电机 8 、搅拌轴 9 和搅拌桨叶 10 ；所述的 格栅 7 为多孔圆盘，固定在釜壁上；搅拌轴 9 穿过格栅 7 中心，与格栅 7 保持 10mm 间隙；
所述的料仓 1 通过管路与进料口 3 连接；
所述的出料口 5 通过管路依次与冷却系统 11 和储存系统 12 连接。
所述的 连续溶解釜 2 长径比为 10:1 。
所述的 搅拌 桨叶 1 与 连续溶解釜 壁间隙保持在 10mm 。
利用上述的 对苯二胺的连续溶解装置连续溶解对苯二胺的方法，其具体步骤为：
将氮气通过进气口 3 通入整个装置中，将对苯二胺粉料加入到称重系统的料仓 1 中，开启称重系统连续稳定向连续溶解釜 2 中加入 对苯二胺 ；与此同时，利用高精度计量泵将配制好的 N- 甲基吡咯烷酮 / 氯化钙溶液通过进料口 3 连续稳定输送到连续溶解釜 2 中；开启连续溶解釜 2 的搅拌，控制转速在 150rpm ；开启出料输送泵 13 将溶解好的物料输送到冷却系统 11 中冷却到 5 ℃，然后将溶解冷却好的物料储存到 储存系统12 中备用。
溶解并冷却后的 PPD 溶液参照专利 ZL201210485817.3 中所述的的连续聚合方法与另一个单体 TPC 连续聚合，最终得到的 PPTA 粉末用乌氏粘度计测定对数比浓粘度为 5.5 ，精密色差仪连续检测 PPTA 树脂粉末，色差不超过 0.02 。
实施例 3
一种 对苯二胺的连续溶解装置，该装置包括称量系统，溶解系统，冷却系统和储存系统；
所述的称量系统包括料仓 1 ；
所述的溶解系统包括连续溶解釜 2 ，连续溶解釜 2 上设有进料口 3 ，气体进口 4 ，出料口 5 以及气体出口 6 ；连续溶解釜 2 内设有搅拌装置和格栅 7 ；所述的搅拌装置包括电机 8 、搅拌轴 9 和搅拌桨叶 10 ；所述的 格栅 7 为多孔圆盘，固定在釜壁上；搅拌轴 9 穿过格栅 7 中心，与格栅 7 保持 5mm 间隙；
所述的料仓 1 通过管路与进料口 3 连接；
所述的出料口 5 通过管路依次与冷却系统 11 和储存系统 12 连接。
所述的 连续溶解釜 2 长径比为 8:1 。
所述的 搅拌 桨叶 1 与 连续溶解釜 壁间隙保持在 5mm 。
利用上述的 对苯二胺的连续溶解装置连续溶解对苯二胺的方法，其具体步骤为：
将氮气通过进气口 3 通入整个装置中，将对苯二胺粉料加入到称重系统的料仓 1 中，开启称重系统连续稳定向连续溶解釜 2 中加入 对苯二胺 ；与此同时，利用高精度计量泵将配制好的 N- 甲基吡咯烷酮 / 氯化钙溶液通过进料口 3 连续稳定输送到连续溶解釜 2 中；开启连续溶解釜 2 的搅拌，控制转速在 100rpm ；开启出料输送泵 13 将溶解好的物料输送到冷却系统 11 中冷却到 0 ℃，然后将溶解冷却好的物料储存到 储存系统12 中备用。
溶解并冷却后的 PPD 溶液参照专利 ZL201210485817.3 中所述的的连续聚合方法与另一个单体 TPC 连续聚合，最终得到的 PPTA 粉末用乌氏粘度计测定对数比浓粘度为 7.07 ，精密色差仪连续检测 PPTA 树脂粉末，色差不超过 0.02 。

Claims (4)

1 、一种 对苯二胺的连续溶解装置，其特征在于：该装置包括称量系统，溶解系统，冷却系统和储存系统；
所述的称量系统包括料仓（ 1 ）；
所述的溶解系统包括连续溶解釜（ 2 ），连续溶解釜（ 2 ）上设有进料口（ 3 ），气体进口（ 4 ），出料口（ 5 ）以及气体出口（ 6 ）；连续溶解釜（ 2 ）内设有搅拌装置和格栅（ 7 ）；所述的搅拌装置包括电机（ 8 ）、搅拌轴（ 9 ）和搅拌桨叶（ 10 ）；所述的 格栅 （ 7 ） 为多孔圆盘，固定在釜壁上；搅拌轴 （ 9 ） 穿过格栅 （ 7 ） 中心，与格栅 （ 7 ） 保持 1-10mm 间隙；
所述的料仓（ 1 ）通过管路与进料口（ 3 ）连接；
所述的出料口（ 5 ）通过管路依次与冷却系统（ 11 ）和储存系统（ 12 ）连接。
2 、根据权利要求 1 所述的一种 对苯二胺的连续溶解装置，其特征在于：所述的 连续溶解釜（ 2 ）长径比为 5:1-10:1 。
3 、根据权利要求 1 或 2 所述的一种 对苯二胺的连续溶解装置，其特征在于：所述的 搅拌 桨叶 （ 1 ） 与 连续溶解釜 壁间隙保持在 1-10mm 。
4 、利用权利要求 1 所述的 对苯二胺的连续溶解装置连续溶解对苯二胺的方法，其特征在于：其具体步骤为：
将氮气通过进气口（ 3 ）通入整个装置中，将对苯二胺粉料加入到称重系统的料仓（ 1 ）中，开启称重系统连续稳定向连续溶解釜（ 2 ）中加入 对苯二胺 ；与此同时，利用高精度计量泵将配制好的 N- 甲基吡咯烷酮 / 氯化钙溶液通过进料口（ 3 ）连续稳定输送到连续溶解釜（ 2 ）中；开启连续溶解釜（ 2 ）的搅拌，控制转速在 10-150rpm ；开启出料输送泵（ 13 ）将溶解好的物料输送到冷却系统（ 11 ）中冷却到 -5-5 ℃，然后将溶解冷却好的物料储存到 储存系统（12） 中备用。
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