CN219559622U - Stirred reactor for poly(p-phenylenebenzobisoxazole-polyphosphoric acid) system - Google Patents
Stirred reactor for poly(p-phenylenebenzobisoxazole-polyphosphoric acid) system Download PDFInfo
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- 229920000137 polyphosphoric acid Polymers 0.000 title claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 70
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 125000001140 1,4-phenylene group Chemical group [H]C1=C([H])C([*:2])=C([H])C([H])=C1[*:1] 0.000 claims abstract description 10
- 239000011521 glass Substances 0.000 claims description 5
- 230000008878 coupling Effects 0.000 claims description 3
- 238000010168 coupling process Methods 0.000 claims description 3
- 238000005859 coupling reaction Methods 0.000 claims description 3
- 241000555745 Sciuridae Species 0.000 claims description 2
- 229920000927 poly(p-phenylene benzobisoxazole) Polymers 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 30
- 238000006116 polymerization reaction Methods 0.000 abstract description 11
- 239000012530 fluid Substances 0.000 abstract description 10
- 238000002156 mixing Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 8
- 230000009471 action Effects 0.000 abstract description 7
- 238000009792 diffusion process Methods 0.000 abstract description 4
- 238000010008 shearing Methods 0.000 abstract description 4
- 230000002493 climbing effect Effects 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 229920000642 polymer Polymers 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000009987 spinning Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- ICXAPFWGVRTEKV-UHFFFAOYSA-N 2-[4-(1,3-benzoxazol-2-yl)phenyl]-1,3-benzoxazole Chemical compound C1=CC=C2OC(C3=CC=C(C=C3)C=3OC4=CC=CC=C4N=3)=NC2=C1 ICXAPFWGVRTEKV-UHFFFAOYSA-N 0.000 description 1
- DPYROBMRMXHROQ-UHFFFAOYSA-N 4,6-diaminobenzene-1,3-diol Chemical compound NC1=CC(N)=C(O)C=C1O DPYROBMRMXHROQ-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 125000006615 aromatic heterocyclic group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
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Abstract
Description
技术领域technical field
本实用新型涉及搅拌反应釜技术领域,具体公开了用于聚对苯撑苯并二噁唑-多聚磷酸体系的搅拌反应釜。The utility model relates to the technical field of stirred reactors, in particular disclosing a stirred reactor for poly-p-phenylenebenzobisoxazole-polyphosphoric acid system.
背景技术Background technique
聚对苯撑苯并二噁唑纤维(PBO),是20世纪80年代美国为发展航天航空事业而开发的复合材料用增强材料,是含有杂环芳香族的聚酰胺家族中最有发展前途的一个成员,被誉为21世纪超级纤维。PBO纤维展现出的高强度、高模量、耐高温、耐化学腐蚀等优异性能使其在民用及军用领域具有重要应用价值和广阔的前景。Poly-p-phenylene benzobisoxazole fiber (PBO) is a reinforcing material for composite materials developed by the United States in the 1980s for the development of the aerospace industry. It is the most promising polyamide family containing heterocyclic aromatics. A member, known as the 21st century super fiber. The high strength, high modulus, high temperature resistance, chemical corrosion resistance and other excellent properties of PBO fiber make it have important application value and broad prospects in civil and military fields.
目前PBO纤维采用的主要工艺路线为对苯二甲酸法:在多聚磷酸(PPA)溶剂中,主要是以单体4 ,6-二氨基间苯二酚和对苯二甲酸进行聚合反应的合成方法,该反应最终形成具有液晶态的PBO-PPA聚合物体系,经干喷湿纺工艺纺丝、反复水洗、干燥等流程制得PBO纤维。其中PBO预聚合反应在间歇式反应釜中进行,聚合过程体系动力粘度持续升高,直至超过500万cp,如此高黏体系的聚合反应过程对反应釜搅拌器提出了更高的要求。在高分子工业普遍应用的锚式、框式和螺带式搅拌器,在应用于PBO-PPA聚合反应体系时,由于PBO-PPA体系较一般高分子聚合体系,动力粘度甚至高出几个数量级,聚合反应时会出现较严重的爬杆效应的影响,PBO聚合物的品质不易控制,很难制备获得高强的PBO纤维。本实用新型专利对框式搅拌器进行改进,开发出一种更适用于PBO-PPA体系的搅拌反应釜。At present, the main process route used by PBO fiber is the terephthalic acid method: in the polyphosphoric acid (PPA) solvent, the synthesis is mainly carried out by the polymerization reaction of the monomer 4,6-diaminoresorcinol and terephthalic acid. method, the reaction finally forms a PBO-PPA polymer system with a liquid crystal state, and the PBO fiber is prepared through a dry-jet wet spinning process, repeated washing, and drying. Among them, the PBO pre-polymerization reaction is carried out in a batch reactor, and the dynamic viscosity of the system continues to increase during the polymerization process until it exceeds 5 million cp. The polymerization reaction process of such a high-viscosity system puts forward higher requirements for the reactor agitator. The anchor type, frame type and ribbon type agitator commonly used in the polymer industry, when applied to the PBO-PPA polymerization reaction system, the dynamic viscosity of the PBO-PPA system is even several orders of magnitude higher than that of the general polymer polymerization system , There will be a serious climbing effect during the polymerization reaction, the quality of PBO polymer is not easy to control, and it is difficult to prepare high-strength PBO fibers. The utility model patent improves the frame type agitator and develops a stirring reaction kettle more suitable for PBO-PPA system.
实用新型内容Utility model content
本实用新型旨在解决现有技术中搅拌反应釜用于PBO-PPA体系使用时会受到爬杆效应的问题,提供用于聚对苯撑苯并二噁唑-多聚磷酸体系的搅拌反应釜,驱动电机带动搅拌框旋转,使釜内物料大范围总体流动,同时搅拌叶片附近流体在剪切作用下形成局部湍流,加快物料的高效混合,强化分子扩散接触,提高聚合反应的效率;釜体的物料在搅拌框和导流挡板作用下,引导紧贴釜体内壁的物料沿着导流挡板流动,破坏其稳定的离心运动,强化釜壁处流体的分子混合。本实用新型使用能够克服物料的爬杆效应,使得搅拌效果更好,有利于PBO聚合物的一致性得到大幅度提高,继而有利于实现PBO纤维的纺丝工艺稳定性。The utility model aims to solve the problem that the stirred reactor in the prior art will be subjected to the rod-climbing effect when it is used in the PBO-PPA system, and provides a stirred reactor for the poly-p-phenylenebenzobisoxazole-polyphosphoric acid system , the driving motor drives the stirring frame to rotate, so that the material in the kettle can flow in a large range, and at the same time, the fluid near the stirring blade forms a local turbulent flow under the action of shearing, which speeds up the efficient mixing of materials, strengthens the molecular diffusion contact, and improves the efficiency of the polymerization reaction; the kettle body Under the action of the stirring frame and the diversion baffle, the material close to the inner wall of the kettle is guided to flow along the diversion baffle, destroying its stable centrifugal motion and strengthening the molecular mixing of the fluid at the kettle wall. The utility model can overcome the pole-climbing effect of the material, so that the stirring effect is better, and the consistency of the PBO polymer is greatly improved, and then the stability of the spinning process of the PBO fiber is realized.
本实用新型的目的是通过以下技术方案实现的:The purpose of this utility model is achieved by the following technical solutions:
用于聚对苯撑苯并二噁唑-多聚磷酸体系的搅拌反应釜,包括釜体,所述釜体上端设置有投料口和驱动电机,所述驱动电机通过联轴器与搅拌轴相连,所述搅拌轴伸入釜体内与搅拌框相连,所述搅拌框上设置有搅拌叶片,所述釜体内部还设置有导流挡板,所述导流挡板与搅拌框外侧之间形成流动间隙,所述釜体下端设置有出料口。A stirring reaction kettle for poly-p-phenylenebenzobisoxazole-polyphosphoric acid system, including a kettle body, the upper end of the kettle body is provided with a feeding port and a driving motor, and the driving motor is connected to the stirring shaft through a coupling , the stirring shaft extends into the kettle body and connects with the stirring frame, the stirring frame is provided with stirring blades, and the inside of the kettle body is also provided with a diversion baffle, forming a gap between the diversion baffle and the outside of the stirring frame Flow gap, the lower end of the kettle body is provided with a discharge port.
优选的,所述搅拌框为鼠笼式搅拌框。Preferably, the stirring frame is a squirrel-cage stirring frame.
优选的,所述搅拌叶片为框式结构。Preferably, the stirring blade is a frame structure.
优选的,所述搅拌叶片设置在搅拌框中下段。Preferably, the stirring blades are arranged in the lower part of the stirring frame.
优选的,所述导流挡板设置有多个。Preferably, there are multiple guide baffles.
优选的,多个导流挡板均匀设置在釜体内壁下端。Preferably, a plurality of guide baffles are uniformly arranged at the lower end of the inner wall of the kettle.
优选的,所述流动间隙为25-50mm。Preferably, the flow gap is 25-50mm.
优选的,所述釜体上设置有视镜。Preferably, a sight glass is arranged on the kettle body.
优选的,所述出料口处设置有单螺杆挤出机。Preferably, a single-screw extruder is provided at the outlet.
优选的,所述釜体外还设置有换热夹套。Preferably, a heat exchange jacket is provided outside the kettle body.
本技术方案的有益效果如下:The beneficial effects of this technical solution are as follows:
一、本实用新型提供的用于聚对苯撑苯并二噁唑-多聚磷酸体系的搅拌反应釜,驱动电机带动搅拌框旋转,釜内物料大范围总体流动,同时搅拌叶片附近流体在剪切作用下形成局部湍流,加快物料的高效混合,强化分子扩散接触,提高聚合反应的效率;釜体的物料在搅拌框和导流挡板作用下,引导紧贴釜体内壁的物料沿着导流挡板流动,破坏其稳定的离心运动,强化釜壁处流体的分子混合。本实用新型的应用能够克服物料的爬杆效应,使得搅拌效果更好,有利于PBO聚合物的一致性得到大幅度提高,继而有利于实现PBO纤维的纺丝工艺稳定性。1. The stirring reaction kettle for poly(p-phenylenebenzobisoxazole-polyphosphoric acid system) provided by the utility model, the driving motor drives the stirring frame to rotate, and the materials in the kettle flow in a large range as a whole, and at the same time, the fluid near the stirring blade is shearing The local turbulent flow is formed under the action of cutting, the efficient mixing of materials is accelerated, the molecular diffusion contact is strengthened, and the efficiency of polymerization reaction is improved; The flow of the flow baffle disrupts its stable centrifugal motion and strengthens the molecular mixing of the fluid at the wall of the kettle. The application of the utility model can overcome the pole-climbing effect of the material, so that the stirring effect is better, which is beneficial to greatly improving the consistency of the PBO polymer, and then is beneficial to realizing the stability of the spinning process of the PBO fiber.
二、本实用新型提供的用于聚对苯撑苯并二噁唑-多聚磷酸体系的搅拌反应釜,鼠笼式搅拌框和框式结构的设置进一步克服了物料搅拌过程中的爬杆效应。2. The stirred reactor for poly(p-phenylenebenzobisoxazole-polyphosphoric acid) system provided by the utility model, the setting of the squirrel-cage stirring frame and the frame structure further overcomes the pole-climbing effect in the material stirring process .
三、本实用新型提供的用于聚对苯撑苯并二噁唑-多聚磷酸体系的搅拌反应釜,流动间隙为25-50mm,使得釜体内物料最大范围的整体流动。3. The stirring reaction kettle for the poly(p-phenylenebenzobisoxazole-polyphosphoric acid system) provided by the utility model has a flow gap of 25-50mm, so that the materials in the kettle body can flow as a whole in the largest range.
四、本实用新型提供的用于聚对苯撑苯并二噁唑-多聚磷酸体系的搅拌反应釜,视镜的设置方便查看釜体的物料情况,单螺杆挤出机的设置使得物料出料更顺畅,换热夹套的设置满足物料反应的温度。4. The agitated reactor for the poly(p-phenylenebenzobisoxazole-polyphosphoric acid system) provided by the utility model, the setting of the sight glass is convenient to check the material situation of the kettle body, and the setting of the single-screw extruder makes the material go out The material is smoother, and the setting of the heat exchange jacket meets the temperature of the material reaction.
五、本实用新型提供的用于聚对苯撑苯并二噁唑-多聚磷酸体系的搅拌反应釜,本搅拌反应釜不仅仅能用于聚对苯撑苯并二噁唑-多聚磷酸体系使用,还能适用于高粘度体系或非牛顿流体体系使用。5. The stirred reactor for poly(p-phenylenebenzobisoxazole-polyphosphoric acid) system provided by the utility model, this stirred reactor can not only be used for poly(p-phenylenebenzobisoxazole-polyphosphoric acid) It can also be used in high-viscosity systems or non-Newtonian fluid systems.
附图说明Description of drawings
图1为本实用新型的结构示意图;Fig. 1 is the structural representation of the utility model;
图2为图1中A-A处的剖视图;Fig. 2 is the sectional view of A-A place in Fig. 1;
其中:1、釜体;2、换热夹套;3、搅拌框;4、搅拌叶片;5、导流挡板;6、投料口;7、视镜;8、单螺杆挤出机;9、驱动电机;10、出料口;11、流动间隙。Among them: 1. Kettle body; 2. Heat exchange jacket; 3. Stirring frame; 4. Stirring blade; 5. Guide baffle; 6. Feeding port; 7. Sight glass; , Drive motor; 10, discharge port; 11, flow gap.
具体实施方式Detailed ways
下面结合实施例对本实用新型作进一步地详细说明,但本实用新型的实施方式不限于此。The utility model will be described in further detail below in conjunction with the examples, but the implementation of the utility model is not limited thereto.
需要说明的是,当部件被称为“装设于”、“固定于”或“设置于”另一个部件上,它可以直接在另一个部件上或者可能同时存在居中部件。当一个部件被称为是“连接于”另一个部件,它可以是直接连接到另一个部件或者可能同时存在居中部件。It should be noted that, when an element is referred to as being “mounted on”, “fixed on” or “disposed on” another element, it may be directly on the other element or there may be an intervening element at the same time. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or intervening elements may also be present.
还需要说明的是,本实用新型实施例中的左、右、上、下等方位用语,仅是互为相对概念或是以产品的正常使用状态为参考的,而不应该认为是具有限制性的。It should also be noted that the orientation terms such as left, right, up, and down in the embodiments of the present utility model are only relative concepts or refer to the normal use state of the product, and should not be regarded as restrictive of.
实施例1Example 1
如图1和图2所示,用于聚对苯撑苯并二噁唑-多聚磷酸体系的搅拌反应釜,包括釜体1,所述釜体1上端设置有投料口6和驱动电机9,所述驱动电机9通过联轴器与搅拌轴相连,所述搅拌轴伸入釜体1内与搅拌框3相连,所述搅拌框3上设置有搅拌叶片4,所述釜体1内部还设置有导流挡板5,所述导流挡板5与搅拌框3外侧之间形成流动间隙11,所述釜体1下端设置有出料口10。驱动电机9带动搅拌框3旋转,釜内物料大范围总体流动,同时搅拌叶片4附近流体在剪切作用下形成局部湍流,加快物料的高效混合,强化分子扩散接触,提高聚合反应的效率;釜体1的物料在搅拌框3和导流挡板5作用下,引导紧贴釜体1内壁的物料沿着导流挡板5流动,破坏其稳定的离心运动,强化釜壁处流体的分子混合。As shown in Figure 1 and Figure 2, the stirred reactor for poly-p-phenylenebenzobisoxazole-polyphosphoric acid system includes a kettle body 1, and the upper end of the kettle body 1 is provided with a feeding port 6 and a drive motor 9 , the drive motor 9 is connected to the stirring shaft through a coupling, and the stirring shaft extends into the still body 1 and is connected to the stirring frame 3. The stirring frame 3 is provided with stirring blades 4, and the inside of the kettle body 1 is also A flow guide baffle 5 is provided, and a flow gap 11 is formed between the flow guide baffle 5 and the outside of the stirring frame 3 , and a discharge port 10 is provided at the lower end of the kettle body 1 . The driving motor 9 drives the stirring frame 3 to rotate, and the materials in the kettle flow in a large area. At the same time, the fluid near the stirring blade 4 forms a local turbulent flow under the action of shearing, which speeds up the efficient mixing of materials, strengthens the molecular diffusion contact, and improves the efficiency of the polymerization reaction; Under the action of the stirring frame 3 and the diversion baffle 5, the material in the body 1 guides the material close to the inner wall of the kettle body 1 to flow along the diversion baffle 5, destroying its stable centrifugal motion and strengthening the molecular mixing of the fluid at the kettle wall .
实施例2Example 2
本实施例与实施例1的区别点在于:所述搅拌框3为鼠笼式搅拌框。The difference between this embodiment and embodiment 1 is that the stirring frame 3 is a squirrel cage type stirring frame.
其中,所述搅拌叶片4为框式结构。鼠笼式搅拌框和框式结构的设置进一步克服了物料搅拌过程中的爬杆效应。Wherein, the stirring blade 4 is a frame structure. The setting of the squirrel-cage mixing frame and the frame structure further overcomes the pole-climbing effect during the material mixing process.
其中,所述搅拌叶片4设置在搅拌框3中下段。Wherein, the stirring blade 4 is arranged in the lower part of the stirring frame 3 .
其中,所述导流挡板5设置有多个。Wherein, there are multiple guide baffles 5 .
其中,多个导流挡板5均匀设置在釜体1内壁下端。Wherein, a plurality of guide baffles 5 are evenly arranged on the lower end of the inner wall of the kettle body 1 .
其中,所述流动间隙11为25-50mm。流动间隙11为25-50mm,使得釜体1内物料最大范围的整体流动。Wherein, the flow gap 11 is 25-50 mm. The flow gap 11 is 25-50 mm, so that the materials in the still body 1 can flow as a whole in the largest range.
其中,所述釜体1上设置有视镜7。Wherein, the kettle body 1 is provided with a viewing mirror 7 .
其中,所述出料口10处设置有单螺杆挤出机8。Wherein, the discharge port 10 is provided with a single-screw extruder 8 .
其中,所述釜体1外还设置有换热夹套2。视镜7的设置方便查看釜体1的物料情况,单螺杆挤出机8的设置使得物料出料更顺畅,换热夹套2的设置满足物料反应的温度。Wherein, a heat exchange jacket 2 is provided outside the kettle body 1 . The setting of sight glass 7 is convenient to check the material condition of kettle body 1, the setting of single screw extruder 8 makes material discharge more smoothly, and the setting of heat exchange jacket 2 satisfies the temperature of material reaction.
本搅拌反应釜不仅仅能用于聚对苯撑苯并二噁唑-多聚磷酸体系使用,还能适用于高粘度体系或非牛顿流体体系使用。This stirred reactor can not only be used for poly(p-phenylene benzobisoxazole-polyphosphoric acid system), but also suitable for high viscosity system or non-Newtonian fluid system.
本装置使用时,物料通过投料口6进入釜体1内部,换热夹套2中通入满足物料反应要求的换热介质,启动驱动电机9,驱动电机9转动带动釜体1的搅拌框3和设置在搅拌框3上的搅拌叶片4进行搅拌,物料在釜体1搅拌反应完成后,通过单螺杆挤出机8将反应完毕的物料从出料口10处排出釜体1。When the device is in use, the material enters the interior of the kettle body 1 through the feeding port 6, and the heat exchange medium that meets the requirements of the material reaction is introduced into the heat exchange jacket 2, and the driving motor 9 is started, and the driving motor 9 rotates to drive the stirring frame 3 of the kettle body 1 Stir with the stirring blade 4 arranged on the stirring frame 3. After the material is stirred and reacted in the kettle body 1, the reacted material is discharged from the kettle body 1 through the single-screw extruder 8 from the discharge port 10.
以上所述,仅是本实用新型的较佳实施例,并非对本实用新型做任何形式上的限制,凡是依据本实用新型的技术实质对以上实施例所作的任何简单修改、等同变化,均落入本实用新型的保护范围之内。The above is only a preferred embodiment of the utility model, and does not limit the utility model in any form. Any simple modification or equivalent change made to the above embodiments according to the technical essence of the utility model falls within the scope of the present utility model. Within the protection scope of the present utility model.
Claims (10)
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| CN202321883031.7U CN219559622U (en) | 2023-07-18 | 2023-07-18 | Stirred reactor for poly(p-phenylenebenzobisoxazole-polyphosphoric acid) system |
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| CN120169301A (en) * | 2025-05-21 | 2025-06-20 | 福建省德旭新材料有限公司 | A reaction separation device for preparing phosphorus oxyfluoride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN120169301A (en) * | 2025-05-21 | 2025-06-20 | 福建省德旭新材料有限公司 | A reaction separation device for preparing phosphorus oxyfluoride |
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