WO2021109728A1 - Dispersion reactor - Google Patents

Dispersion reactor Download PDF

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Publication number
WO2021109728A1
WO2021109728A1 PCT/CN2020/121844 CN2020121844W WO2021109728A1 WO 2021109728 A1 WO2021109728 A1 WO 2021109728A1 CN 2020121844 W CN2020121844 W CN 2020121844W WO 2021109728 A1 WO2021109728 A1 WO 2021109728A1
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Prior art keywords
reactor
dispersion
ultrasonic
stirring
stirring blade
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PCT/CN2020/121844
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French (fr)
Chinese (zh)
Inventor
吴斌
景录如
张春琪
崔艺华
马俊锋
徐晓风
张超
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苏州太湖电工新材料股份有限公司
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Publication of WO2021109728A1 publication Critical patent/WO2021109728A1/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/80Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside

Definitions

  • This application belongs to the field of composite material preparation, and in particular relates to a composite modification of inorganic nanomaterials and organic materials, and in particular to a dispersion reactor, which can realize modification with organic materials while uniformly dispersing nanoparticles.
  • Inorganic nano/organic composite materials are widely used because they can combine the toughness, elasticity, ductility, processability of organic materials and the hardness and thermal stability of inorganic materials, resulting in many special properties.
  • due to the high surface energy of the nanoparticles they are prone to agglomeration, and the nanoparticles cannot be uniformly dispersed in the organic matrix.
  • the performance of the composite material will not only not be improved, but will decrease! Therefore, achieving good dispersion of nanoparticles in the resin matrix is a crucial prerequisite for the manufacture of ideal nanocomposite materials.
  • How to completely solve the problem of nanoparticle agglomeration, make the nanoparticles monodisperse, and truly exert the nano effect is one of the hot spots in the field of nano-modified composite materials.
  • nanoparticle dispersing nanoparticles there are many methods for dispersing nanoparticles. According to the different dispersion methods, they can be divided into physical dispersion (sand milling, roller milling, high-pressure homogenization, ultrasound, etc.) and chemical dispersion (coupling agent method, surface modification method, Sol-gel method, etc.).
  • the current popular method of nanoparticle dispersion is the physical-chemical method, that is, the physical method is used to pre-disperse the nanoparticles, and then they are moved into the modification reactor for chemical modification.
  • the problem is that the steps are cumbersome, the process time is long, and because the nanoparticles are pre-dispersed by physical methods, they must be moved into the reactor. During the transfer process, the nanoparticles will partially re-aggregate, which greatly affects the subsequent surface modification effect. Therefore, it is difficult to obtain a well-dispersed nanoparticle solution, and thus an ideal nanocomposite material cannot be prepared.
  • the technical problem to be solved by this application is to overcome the shortcomings of the prior art and provide a new type of dispersion reactor with high-speed stirring shear and ultrasonic dual dispersion function, which can combine the dispersion of inorganic nanoparticles and the improvement of inorganic nanoparticles.
  • the performance is carried out simultaneously, avoiding the incomplete modification caused by the agglomeration effect of inorganic nanoparticles, so that the modified inorganic nanoparticles can achieve monodispersion and truly exert the nano effect.
  • a dispersion reactor comprising a reactor barrel and a stirring device partially arranged inside the reactor barrel.
  • the reactor barrel includes a reactor body and is detachable from the reactor body.
  • a reactor cover connected to the ground and used to cover the reactor body, the stirring device partially penetrates the reactor cover and extends into the reactor body;
  • the dispersion reactor also includes an ultrasonic vibration device
  • the ultrasonic vibration device includes an ultrasonic generator arranged on the cover of the reactor, an ultrasonic transducer connected with the ultrasonic generator, an horn connected with the ultrasonic transducer, and The ultrasonic vibrating rod connected to the horn, the ultrasonic vibrating rod extends into the body of the reactor.
  • the ultrasonic vibrating rod extends in the up and down direction.
  • the ultrasonic vibration device has at least two and is symmetrically distributed around the stirring device.
  • the stirring device includes a driving part fixedly arranged on the reactor cover through a support frame, a coupling that is drivingly connected to the driving part, and is drivingly connected to the coupling And a stirring shaft passing through the reactor cover and extending into the reactor body, and a stirring blade arranged at the lower part of the stirring shaft.
  • the stirring blade has at least two and is sequentially arranged on the stirring shaft along the up and down direction.
  • the stirring blade has a first disc stirring blade arranged at the lower end of the stirring shaft, and a second disc stirring blade arranged above the first disc stirring blade.
  • the first disc stirring blade is located below the ultrasonic vibrating rod, and the ultrasonic vibrating rod is located outside the second disc stirring blade.
  • the first disc-type stirring blade includes a blade body and a plurality of blades formed on the outer periphery of the blade body, and the plurality of blades have a space therebetween.
  • the lower part of the blade body protrudes downward to form an arc-shaped part corresponding to the bottom of the reactor body.
  • the reactor barrel further includes a heat transfer jacket coated on the reactor body, an insulation layer coated on the outer wall of the heat transfer jacket, and the heat transfer clip
  • the jacket has a heat exchange fluid inlet and a heat exchange fluid outlet respectively passing through the insulation layer, the heat exchange fluid inlet is located at the lower part of the heat transfer jacket, and the heat exchange fluid outlet is located at the bottom of the heat transfer jacket Upper part.
  • the reactor barrel further includes a discharge pipe arranged at the bottom of the reactor body and respectively passing through the heat transfer jacket and the insulation layer.
  • a hand hole, a material sight glass, a thermometer socket, and a flange for fixing the ultrasonic vibration device are respectively provided on the reactor cover.
  • the present application realizes the advantages of convenient replacement and adjustment of the entire device through the cooperation of the detachably connected reactor cover and the reactor body, combined with the stirring device and the ultrasonic vibration device provided on the reactor cover, and the advantages of convenient replacement and adjustment of the entire device are realized, especially Combining high-speed stirring and shearing and ultrasonic dispersion in one, realizes the effective dispersion of inorganic nanoparticles while realizing surface modification, which not only simplifies the operation steps, but also greatly improves the dispersion and modification effects, and avoids the agglomeration effect of inorganic nanoparticles.
  • the modification is not complete, so that the modified inorganic nanoparticles can achieve monodispersion and truly exert the nanometer effect.
  • Figure 1 is a schematic diagram of the overall structure of the dispersion reactor of this application.
  • Reactor cylinder 11. Reactor body; 12. Reactor cover; 121. Hand hole; 122. Material sight glass; 123. Thermometer socket; 124. Flange; 13. Heat transfer jacket 131. Heat exchange fluid inlet; 132. Heat exchange fluid outlet; 14. Thermal insulation layer; 15. Discharge pipe; 21. Drive parts; 22. Coupling; 23. Stirring shaft; 24. First disc stirring blade Blade; 25. The second disc stirring blade; 31. Ultrasonic generator; 32. Ultrasonic vibrating rod; 4. Ear-type support; 5. Bolt and screw connection.
  • first and second are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of indicated technical features. Therefore, the features defined with “first” and “second” may explicitly or implicitly include at least one of the features. In the description of the present invention, “plurality” means at least two, such as two, three, etc., unless otherwise specifically defined.
  • the first feature “on” or “under” the second feature may be in direct contact with the first and second features, or the first and second features may be indirectly through an intermediary. contact.
  • the "above”, “above” and “above” of the first feature on the second feature may mean that the first feature is directly above or diagonally above the second feature, or it simply means that the level of the first feature is higher than that of the second feature.
  • the “below”, “below” and “below” of the second feature of the first feature may mean that the first feature is directly below or obliquely below the second feature, or it simply means that the level of the first feature is smaller than the second feature.
  • the dispersion reactor includes a reactor barrel 1, a stirring device partially arranged inside the reactor barrel 1, and the reactor barrel 1 includes a reactor body 11,
  • the reactor cover 12 detachably connected with the reactor body 11 and used to cover the reactor body 11, the stirring device partially penetrates the reactor cover 12 and extends into the reactor body 11;
  • the dispersion reactor also includes ultrasonic vibration
  • the ultrasonic vibration device includes an ultrasonic generator 31 arranged on the reactor cover 12, an ultrasonic transducer (not shown) connected to the ultrasonic generator 31, an horn connected to the ultrasonic transducer, and The ultrasonic vibrating rod 32 connected to the horn, the ultrasonic vibrating rod 32 extends into the reactor body 11.
  • the upper part of the reactor body 11 and the reactor cover 12 are detachably connected through the bolt and screw connector 5.
  • the ultrasonic vibration device is a conventional device in the prior art.
  • This application uses the ultrasonic vibration dispersion effect generated after the ultrasonic vibration rod 32 is inserted into the material, so that the inorganic nanoparticles are uniformly dispersed, and then combined with the common stirring device
  • the function integrates the dispersion and surface modification of inorganic nanoparticles, and improves work efficiency and work effect.
  • the frequency of the ultrasonic vibration device may be 2 ⁇ 10 4 to 10 7 Hz, and the power may be 500-3000W.
  • the ultrasonic vibrating rod 32 extends in the up and down direction to facilitate the insertion of the ultrasonic vibrating rod 32 into the material.
  • the ultrasonic vibration device has at least two and is symmetrically distributed around the stirring device, so that all positions in the reactor body 11 can be subjected to the ultrasonic vibration dispersion effect.
  • the stirring device includes a driving part 21 (a conventional variable frequency speed-regulating motor can be used) fixedly arranged on the reactor cover 12 through a support frame, a coupling 22 that is connected to the driving part 21 in transmission, and a coupling 22 is a stirring shaft 23 which is connected in transmission and passes through the reactor cover 12 and extends into the reactor body 11, and a stirring blade arranged at the lower part of the stirring shaft 23.
  • a driving part 21 a conventional variable frequency speed-regulating motor can be used
  • a coupling 22 is a stirring shaft 23 which is connected in transmission and passes through the reactor cover 12 and extends into the reactor body 11, and a stirring blade arranged at the lower part of the stirring shaft 23.
  • the stirring blade has a first disc stirring blade 24 arranged at the lower end of the stirring shaft 23, a second disc stirring blade 25 arranged above the first disc stirring blade 24, and the first disc stirring blade
  • the paddle 24 is located under the ultrasonic vibrating rod 32, and the ultrasonic vibrating rod 32 is located on the outside of the second disc-type stirring blade 25.
  • the purpose of setting two stirring blades is to make the materials inside stir uniformly, and at the same time stir the blades and
  • the mutual positional relationship of the ultrasonic vibrating rods 32 enables the forces of the two to interact, thereby causing internal turbulence to further improve the dispersibility of the material, that is, to further improve the dispersibility of inorganic nanoparticles for thorough modification.
  • the first disc stirring blade 24 includes a blade body and a plurality of blades formed on the outer periphery of the blade body.
  • the corresponding arc-shaped part at the bottom of the reactor body 11 can be arranged at intervals to increase the force generated by the materials in different directions during the stirring process, and the materials will further collide with each other, so that the materials are excellently dispersed.
  • the reactor barrel 1 also includes a heat transfer jacket 13 (which can be passed through a cooling or heating medium) coated on the reactor body 11, and an insulation layer 14 coated on the outer wall of the heat transfer jacket 13.
  • the heat jacket 13 has a heat exchange fluid inlet 131 and a heat exchange fluid outlet 132 respectively passing through the thermal insulation layer 14.
  • the heat exchange fluid inlet 131 is located at the lower part of the heat transfer jacket 13, and the heat exchange fluid outlet 132 is located at the bottom of the heat transfer jacket 13 Upper part.
  • the reactor barrel 1 further includes a discharge pipe 15 arranged at the bottom of the reactor body 11 and passing through the heat transfer jacket 13 and the insulation layer 14 respectively.
  • the reactor cover 12 is provided with a hand hole 121, a material sight glass 122, a thermometer socket 123, and a flange 124 for fixing the ultrasonic vibration device.
  • the reactor barrel 1 includes a plurality of ear supports 4 arranged on the reactor body 11 and passing through the heat transfer jacket 13 and the insulation layer 14.
  • the present application realizes the easy replacement of the entire device through the cooperation of the detachably connected reactor cover 12 and the reactor body 11, combined with the stirring device and the ultrasonic vibration device provided on the reactor cover 12,
  • the advantages of adjustment especially the combination of high-speed stirring and shearing and ultrasonic dispersion, can realize the effective dispersion of inorganic nanoparticles while realizing surface modification, which not only simplifies the operation steps, but also greatly improves the dispersion and modification effects, and avoids inorganic nanoparticles.
  • the incomplete modification caused by the agglomeration effect of nanoparticles makes the modified inorganic nanoparticles achieve monodispersion and truly exert the nanometer effect.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

Disclosed is a dispersion reactor. The dispersion reactor comprises a reactor cylinder (1) and a stirring device partially arranged inside the reactor cylinder (1), wherein the reactor cylinder (1) comprises a reactor body (11), and a reactor cover (12) detachably connected to the reactor body (11) and used for covering the reactor body (11), and a portion of the stirring device penetrates the reactor cover (12) and extends into the reactor body (11); and the dispersion reactor further comprises an ultrasonic vibration device, wherein the ultrasonic vibration device comprises an ultrasonic generator (31) arranged on the reactor cover (12), an ultrasonic transducer connected to the ultrasonic generator (31), an amplitude-transforming pole connected to the ultrasonic transducer, and an ultrasonic vibration rod (32) connected to the amplitude-transforming pole, and the ultrasonic vibration rod (32) extends into the reactor body (11).

Description

一种分散反应器Dispersion reactor
本申请要求申请号为:CN201922180916.0、申请日为2019.12.6的中国国家知识产权局的在先专利申请为优先权,该在先专利申请文本中的内容通过引用而完全加入本专利申请中。This application requires the prior patent application of the State Intellectual Property Office of China with the application number of CN201922180916.0 and the filing date of 2019.12.6 as priority, and the content of the prior patent application text is fully incorporated into this patent application by reference .
技术领域Technical field
本申请属于复合材料制备领域,尤其涉及一种无机纳米材料与有机材料的复合改性,具体涉及一种分散反应器,其能够在均匀分散纳米颗粒的同时实现与有机材料的改性。This application belongs to the field of composite material preparation, and in particular relates to a composite modification of inorganic nanomaterials and organic materials, and in particular to a dispersion reactor, which can realize modification with organic materials while uniformly dispersing nanoparticles.
背景技术Background technique
无机纳米/有机复合材料由于可以结合有机材料的韧性、弹性、延展性、可加工性和无机材料的硬度及热稳定性等性能而得到广泛的应用,从而产生许多特殊的性能。但由于纳米粒子具有较高的表面能,容易发生团聚,纳米粒子在有机基体中无法分散均匀,导致复合材料的性能不仅得不到提高,反而会下降!因此,实现纳米颗粒在树脂基体中的良好分散是制造理想的纳米复合材料的一个至关重要的前提。如何彻底解决纳米粒子团聚问题,使得纳米粒子实现单分散,真正发挥纳米效应,是目前纳米改性复合材料领域的热点技术之一。Inorganic nano/organic composite materials are widely used because they can combine the toughness, elasticity, ductility, processability of organic materials and the hardness and thermal stability of inorganic materials, resulting in many special properties. However, due to the high surface energy of the nanoparticles, they are prone to agglomeration, and the nanoparticles cannot be uniformly dispersed in the organic matrix. As a result, the performance of the composite material will not only not be improved, but will decrease! Therefore, achieving good dispersion of nanoparticles in the resin matrix is a crucial prerequisite for the manufacture of ideal nanocomposite materials. How to completely solve the problem of nanoparticle agglomeration, make the nanoparticles monodisperse, and truly exert the nano effect, is one of the hot spots in the field of nano-modified composite materials.
目前,分散纳米颗粒的方法有很多种,根据分散方法的不同,可分为物理分散(砂磨、辊磨、高压均质法、超声等)和化学分散(偶联剂法、表面修饰法、溶胶-凝胶法等)。现行流行的纳米颗粒方法分散是物理-化学法,即先采用物理法进行纳米颗粒的预分散,然后移入改性反应器中进行化学改性。存在的问题就是步骤繁琐、工艺时间长,且由于物理法进行纳米颗粒的预分散后要移入反应器中,在这转移过程中,纳米粒子会部分的重新团聚,大大影响后面的表面改性效果,难以得到良好分散的纳米颗粒溶液,因而无法制备理想的纳米复合材料。At present, there are many methods for dispersing nanoparticles. According to the different dispersion methods, they can be divided into physical dispersion (sand milling, roller milling, high-pressure homogenization, ultrasound, etc.) and chemical dispersion (coupling agent method, surface modification method, Sol-gel method, etc.). The current popular method of nanoparticle dispersion is the physical-chemical method, that is, the physical method is used to pre-disperse the nanoparticles, and then they are moved into the modification reactor for chemical modification. The problem is that the steps are cumbersome, the process time is long, and because the nanoparticles are pre-dispersed by physical methods, they must be moved into the reactor. During the transfer process, the nanoparticles will partially re-aggregate, which greatly affects the subsequent surface modification effect. Therefore, it is difficult to obtain a well-dispersed nanoparticle solution, and thus an ideal nanocomposite material cannot be prepared.
申请内容Application content
本申请所要解决的技术问题是克服现有技术的不足,提供一种新型的分散反应器,具有高速搅拌剪切与超声双重分散功能,其能够兼具无机纳米粒子的分散与无机纳米粒子的改性同步进行,避免了无机纳米粒子团聚效应造成的改性不彻底,使得改性后的无机纳米粒子实现单分散,真正发挥纳米效应。The technical problem to be solved by this application is to overcome the shortcomings of the prior art and provide a new type of dispersion reactor with high-speed stirring shear and ultrasonic dual dispersion function, which can combine the dispersion of inorganic nanoparticles and the improvement of inorganic nanoparticles. The performance is carried out simultaneously, avoiding the incomplete modification caused by the agglomeration effect of inorganic nanoparticles, so that the modified inorganic nanoparticles can achieve monodispersion and truly exert the nano effect.
为解决以上技术问题,本申请采取的技术方案如下:In order to solve the above technical problems, the technical solutions adopted by this application are as follows:
一种分散反应器,所述分散反应器包括反应器筒体、部分设置在所述反应器筒体内部的搅拌装置,所述反应器筒体包括反应器本体、与所述反应器本体可拆卸地连接且用于盖合所述反应器本体的反应器盖体,所述搅拌装置部分穿过所述反应器盖体伸入所述反应器本体内;所述分散反应器还包括超声波振动装置,所述超声波振动装置包括设置在所述反应器盖体上的超声波发生器、与所述超声波发生器连接的超声波换能器、与所述超声波换能器连接的变幅杆,以及与所述变幅杆连接的所述超声波振动棒,所述超声波振动棒伸入所述反应器本体内。A dispersion reactor comprising a reactor barrel and a stirring device partially arranged inside the reactor barrel. The reactor barrel includes a reactor body and is detachable from the reactor body. A reactor cover connected to the ground and used to cover the reactor body, the stirring device partially penetrates the reactor cover and extends into the reactor body; the dispersion reactor also includes an ultrasonic vibration device The ultrasonic vibration device includes an ultrasonic generator arranged on the cover of the reactor, an ultrasonic transducer connected with the ultrasonic generator, an horn connected with the ultrasonic transducer, and The ultrasonic vibrating rod connected to the horn, the ultrasonic vibrating rod extends into the body of the reactor.
根据本申请的一些具体且优选的方面,所述超声波振动棒沿上下方向延伸。According to some specific and preferred aspects of the present application, the ultrasonic vibrating rod extends in the up and down direction.
根据本申请的一些具体且优选的方面,所述超声波振动装置具有至少两个且绕着所述搅拌装置对称分布。According to some specific and preferred aspects of the present application, the ultrasonic vibration device has at least two and is symmetrically distributed around the stirring device.
根据本申请的一些具体方面,所述搅拌装置包括通过支撑架固定设置在所述反应器盖体上的驱动部件、与所述驱动部件传动连接的联轴器、与所述联轴器传动连接且穿过所述反应器盖体并伸入所述反应器本体内的搅拌轴,以及设置在所述搅拌轴下部的搅拌桨叶。According to some specific aspects of the present application, the stirring device includes a driving part fixedly arranged on the reactor cover through a support frame, a coupling that is drivingly connected to the driving part, and is drivingly connected to the coupling And a stirring shaft passing through the reactor cover and extending into the reactor body, and a stirring blade arranged at the lower part of the stirring shaft.
根据本申请的一些优选方面,所述搅拌桨叶具有至少两个且沿上下方向依次设置在所述搅拌轴上。According to some preferred aspects of the present application, the stirring blade has at least two and is sequentially arranged on the stirring shaft along the up and down direction.
根据本申请的一些优选方面,所述搅拌桨叶具有设置在所述搅拌轴下端部的第一盘式搅拌桨叶、设置在所述第一盘式搅拌桨叶上方的第二盘式搅拌桨叶,所述第一盘 式搅拌桨叶位于所述超声波振动棒下方,且所述超声波振动棒位于所述第二盘式搅拌桨叶的外侧。According to some preferred aspects of the present application, the stirring blade has a first disc stirring blade arranged at the lower end of the stirring shaft, and a second disc stirring blade arranged above the first disc stirring blade. The first disc stirring blade is located below the ultrasonic vibrating rod, and the ultrasonic vibrating rod is located outside the second disc stirring blade.
根据本申请的一些优选方面,所述第一盘式搅拌桨叶包括桨叶本体以及形成在所述桨叶本体外周的多个叶片,所述的多个叶片两两之间具有间隔,所述桨叶本体的下部向下凸起形成与所述反应器本体底部相适应的弧形部。According to some preferred aspects of the present application, the first disc-type stirring blade includes a blade body and a plurality of blades formed on the outer periphery of the blade body, and the plurality of blades have a space therebetween. The lower part of the blade body protrudes downward to form an arc-shaped part corresponding to the bottom of the reactor body.
根据本申请的一些优选方面,所述反应器筒体还包括包覆在所述反应器本体上的传热夹套、包覆在所述传热夹套外壁的保温层,所述传热夹套具有分别穿过所述保温层的换热流体进口和换热流体出口,所述换热流体进口位于所述传热夹套的下部,所述换热流体出口位于所述传热夹套的上部。According to some preferred aspects of the present application, the reactor barrel further includes a heat transfer jacket coated on the reactor body, an insulation layer coated on the outer wall of the heat transfer jacket, and the heat transfer clip The jacket has a heat exchange fluid inlet and a heat exchange fluid outlet respectively passing through the insulation layer, the heat exchange fluid inlet is located at the lower part of the heat transfer jacket, and the heat exchange fluid outlet is located at the bottom of the heat transfer jacket Upper part.
根据本申请的一些具体方面,所述反应器筒体还包括设置在所述反应器本体底部且分别穿过所述传热夹套、所述保温层的出料管。According to some specific aspects of the present application, the reactor barrel further includes a discharge pipe arranged at the bottom of the reactor body and respectively passing through the heat transfer jacket and the insulation layer.
根据本申请的一些具体且优选的方面,所述反应器盖体上分别设置有手孔、物料视镜、温度计插孔以及用于固定所述超声波振动装置的法兰。According to some specific and preferred aspects of the present application, a hand hole, a material sight glass, a thermometer socket, and a flange for fixing the ultrasonic vibration device are respectively provided on the reactor cover.
由于以上技术方案的采用,本申请与现有技术相比具有如下优点:Due to the adoption of the above technical solutions, compared with the prior art, this application has the following advantages:
本申请通过可拆卸连接的反应器盖体与反应器本体的配合,并结合搅拌装置、设置在反应器盖体上的超声波振动装置共同作用,实现了整个装置方便更换、调整的优点,尤其是结合高速搅拌剪切与超声分散于一体,在实现无机纳米粒子有效分散的同时实现表面改性,不仅简化了操作步骤,而且大大提高了分散以及改性效果,避免了无机纳米粒子团聚效应造成的改性不彻底,使得改性后的无机纳米粒子实现单分散,真正发挥纳米效应。The present application realizes the advantages of convenient replacement and adjustment of the entire device through the cooperation of the detachably connected reactor cover and the reactor body, combined with the stirring device and the ultrasonic vibration device provided on the reactor cover, and the advantages of convenient replacement and adjustment of the entire device are realized, especially Combining high-speed stirring and shearing and ultrasonic dispersion in one, realizes the effective dispersion of inorganic nanoparticles while realizing surface modification, which not only simplifies the operation steps, but also greatly improves the dispersion and modification effects, and avoids the agglomeration effect of inorganic nanoparticles. The modification is not complete, so that the modified inorganic nanoparticles can achieve monodispersion and truly exert the nanometer effect.
附图说明Description of the drawings
图1为本申请分散反应器的整体结构示意图;Figure 1 is a schematic diagram of the overall structure of the dispersion reactor of this application;
其中,1、反应器筒体;11、反应器本体;12、反应器盖体;121、手孔;122、物料视镜;123、温度计插孔;124、法兰;13、传热夹套;131、换热流体进口;132、换热流体出口;14、保温层;15、出料管;21、驱动部件;22、联轴器;23、搅拌轴;24、第一盘式搅拌桨叶;25、第二盘式搅拌桨叶;31、超声波发生器;32、超声波振动棒;4、耳式支座;5、螺栓螺杆连接件。Among them, 1. Reactor cylinder; 11. Reactor body; 12. Reactor cover; 121. Hand hole; 122. Material sight glass; 123. Thermometer socket; 124. Flange; 13. Heat transfer jacket 131. Heat exchange fluid inlet; 132. Heat exchange fluid outlet; 14. Thermal insulation layer; 15. Discharge pipe; 21. Drive parts; 22. Coupling; 23. Stirring shaft; 24. First disc stirring blade Blade; 25. The second disc stirring blade; 31. Ultrasonic generator; 32. Ultrasonic vibrating rod; 4. Ear-type support; 5. Bolt and screw connection.
具体实施方式Detailed ways
以下结合具体实施例对上述方案做进一步说明;应理解,这些实施例是用于说明本申请的基本原理、主要特征和优点,而本申请不受以下实施例的范围限制。The above solutions are further described below in conjunction with specific embodiments; it should be understood that these embodiments are used to illustrate the basic principles, main features, and advantages of the present application, and the present application is not limited by the scope of the following embodiments.
此外,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此,限定有“第一”、“第二”的特征可以明示或者隐含地包括至少一个该特征。在本发明的描述中,“多个”的含义是至少两个,例如两个,三个等,除非另有明确具体的限定。In addition, the terms "first" and "second" are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of indicated technical features. Therefore, the features defined with "first" and "second" may explicitly or implicitly include at least one of the features. In the description of the present invention, "plurality" means at least two, such as two, three, etc., unless otherwise specifically defined.
在本申请中,除非另有明确的规定和限定,第一特征在第二特征“上”或“下”可以是第一和第二特征直接接触,或第一和第二特征通过中间媒介间接接触。而且,第一特征在第二特征“之上”、“上方”和“上面”可是第一特征在第二特征正上方或斜上方,或仅仅表示第一特征水平高度高于第二特征。第一特征在第二特征“之下”、“下方”和“下面”可以是第一特征在第二特征正下方或斜下方,或仅仅表示第一特征水平高度小于第二特征。In this application, unless expressly stipulated and defined otherwise, the first feature “on” or “under” the second feature may be in direct contact with the first and second features, or the first and second features may be indirectly through an intermediary. contact. Moreover, the "above", "above" and "above" of the first feature on the second feature may mean that the first feature is directly above or diagonally above the second feature, or it simply means that the level of the first feature is higher than that of the second feature. The “below”, “below” and “below” of the second feature of the first feature may mean that the first feature is directly below or obliquely below the second feature, or it simply means that the level of the first feature is smaller than the second feature.
下面结合附图及本申请的优选实施例对本申请作进一步描述。The application will be further described below in conjunction with the drawings and preferred embodiments of the application.
如图1所示,本例提供了一种分散反应器,分散反应器包括反应器筒体1、部分设置在反应器筒体1内部的搅拌装置,反应器筒体1包括反应器本体11、与反应器本体11可拆卸地连接且用于盖合反应器本体11的反应器盖体12,搅拌装置部分穿过反应器盖体12伸入反应器本体11内;分散反应器还包括超声波振动装置,超声波振动装置包括设置在反应器盖体12上的超声波发生器31、与超声波发生器31连接的超声波换能器(未示出)、与超声波换能器连接的变幅杆,以及与变幅杆连接的超声波振动棒32,超声波振动棒32伸入反应器本体11内。As shown in Figure 1, this example provides a dispersion reactor. The dispersion reactor includes a reactor barrel 1, a stirring device partially arranged inside the reactor barrel 1, and the reactor barrel 1 includes a reactor body 11, The reactor cover 12 detachably connected with the reactor body 11 and used to cover the reactor body 11, the stirring device partially penetrates the reactor cover 12 and extends into the reactor body 11; the dispersion reactor also includes ultrasonic vibration The ultrasonic vibration device includes an ultrasonic generator 31 arranged on the reactor cover 12, an ultrasonic transducer (not shown) connected to the ultrasonic generator 31, an horn connected to the ultrasonic transducer, and The ultrasonic vibrating rod 32 connected to the horn, the ultrasonic vibrating rod 32 extends into the reactor body 11.
本例中,反应器本体11的上部与反应器盖体12通过螺栓螺杆连接件5实现可拆卸地连接。In this example, the upper part of the reactor body 11 and the reactor cover 12 are detachably connected through the bolt and screw connector 5.
本例中,超声波振动装置是现有技术中的常规设备,本申请利用的是其超声波振动棒32插入物料内部后产生的超声振动分散作用,使得无机纳米粒子分散均匀,进而结合搅拌装置的共同作用,使得无机纳米粒子的分散与表面改性集于一体,提升工作效率以及工作效果。具体地,超声波振动装置的频率可以为2×10 4~10 7Hz,功率为500-3000W。In this example, the ultrasonic vibration device is a conventional device in the prior art. This application uses the ultrasonic vibration dispersion effect generated after the ultrasonic vibration rod 32 is inserted into the material, so that the inorganic nanoparticles are uniformly dispersed, and then combined with the common stirring device The function integrates the dispersion and surface modification of inorganic nanoparticles, and improves work efficiency and work effect. Specifically, the frequency of the ultrasonic vibration device may be 2×10 4 to 10 7 Hz, and the power may be 500-3000W.
本例中,超声波振动棒32沿上下方向延伸,方便超声波振动棒32插入物料内部。具体地,超声波振动装置具有至少两个且绕着搅拌装置对称分布,可以使得反应器本体11内所有位置均能受到超声振动分散作用。In this example, the ultrasonic vibrating rod 32 extends in the up and down direction to facilitate the insertion of the ultrasonic vibrating rod 32 into the material. Specifically, the ultrasonic vibration device has at least two and is symmetrically distributed around the stirring device, so that all positions in the reactor body 11 can be subjected to the ultrasonic vibration dispersion effect.
本例中,搅拌装置包括通过支撑架固定设置在反应器盖体12上的驱动部件21(可以采用常规的变频调速马达)、与驱动部件21传动连接的联轴器22、与联轴器22传动连接且穿过反应器盖体12并伸入反应器本体11内的搅拌轴23,以及设置在搅拌轴23下部的搅拌桨叶。In this example, the stirring device includes a driving part 21 (a conventional variable frequency speed-regulating motor can be used) fixedly arranged on the reactor cover 12 through a support frame, a coupling 22 that is connected to the driving part 21 in transmission, and a coupling 22 is a stirring shaft 23 which is connected in transmission and passes through the reactor cover 12 and extends into the reactor body 11, and a stirring blade arranged at the lower part of the stirring shaft 23.
本例中,搅拌桨叶具有至少两个且沿上下方向依次设置在搅拌轴23上。具体地,搅拌桨叶具有设置在搅拌轴23下端部的第一盘式搅拌桨叶24、设置在第一盘式搅拌桨叶24上方的第二盘式搅拌桨叶25,第一盘式搅拌桨叶24位于超声波振动棒32下方,且超声波振动棒32位于第二盘式搅拌桨叶25的外侧,设置两个搅拌桨叶的目的是为了使得内部的物料能够搅拌均匀,同时搅拌桨叶与超声振动棒32的相互位置关系设置使得两者的作用力能够相互作用,进而使得内部产生扰流作用,进一步提升物料的分散性,即进一步提升无机纳米粒子的分散性,以便改性彻底。In this example, there are at least two stirring blades, which are sequentially arranged on the stirring shaft 23 in the vertical direction. Specifically, the stirring blade has a first disc stirring blade 24 arranged at the lower end of the stirring shaft 23, a second disc stirring blade 25 arranged above the first disc stirring blade 24, and the first disc stirring blade The paddle 24 is located under the ultrasonic vibrating rod 32, and the ultrasonic vibrating rod 32 is located on the outside of the second disc-type stirring blade 25. The purpose of setting two stirring blades is to make the materials inside stir uniformly, and at the same time stir the blades and The mutual positional relationship of the ultrasonic vibrating rods 32 enables the forces of the two to interact, thereby causing internal turbulence to further improve the dispersibility of the material, that is, to further improve the dispersibility of inorganic nanoparticles for thorough modification.
本例中,第一盘式搅拌桨叶24包括桨叶本体以及形成在桨叶本体外周的多个叶片,上述多个叶片两两之间具有间隔,桨叶本体的下部向下凸起形成与反应器本体11底部相适应的弧形部,间隔的设置可以增加物料在搅拌过程中产生不同方向的作用力,进而物料相互之间会进一步发生碰撞,从而使得物料被极好的分散。In this example, the first disc stirring blade 24 includes a blade body and a plurality of blades formed on the outer periphery of the blade body. The corresponding arc-shaped part at the bottom of the reactor body 11 can be arranged at intervals to increase the force generated by the materials in different directions during the stirring process, and the materials will further collide with each other, so that the materials are excellently dispersed.
本例中,反应器筒体1还包括包覆在反应器本体11上的传热夹套13(可以通入冷却或加热介质)、包覆在传热夹套13外壁的保温层14,传热夹套13具有分别穿过保温层14的换热流体进口131和换热流体出口132,换热流体进口131位于传热夹套13的下部,换热流体出口132位于传热夹套13的上部。In this example, the reactor barrel 1 also includes a heat transfer jacket 13 (which can be passed through a cooling or heating medium) coated on the reactor body 11, and an insulation layer 14 coated on the outer wall of the heat transfer jacket 13. The heat jacket 13 has a heat exchange fluid inlet 131 and a heat exchange fluid outlet 132 respectively passing through the thermal insulation layer 14. The heat exchange fluid inlet 131 is located at the lower part of the heat transfer jacket 13, and the heat exchange fluid outlet 132 is located at the bottom of the heat transfer jacket 13 Upper part.
本例中,反应器筒体1还包括设置在反应器本体11底部且分别穿过传热夹套13、保温层14的出料管15。In this example, the reactor barrel 1 further includes a discharge pipe 15 arranged at the bottom of the reactor body 11 and passing through the heat transfer jacket 13 and the insulation layer 14 respectively.
本例中,反应器盖体12上分别设置有手孔121、物料视镜122、温度计插孔123以及用于固定超声波振动装置的法兰124。In this example, the reactor cover 12 is provided with a hand hole 121, a material sight glass 122, a thermometer socket 123, and a flange 124 for fixing the ultrasonic vibration device.
本例中,反应器筒体1包括设置在反应器本体11上且穿过传热夹套13以及保温层14的多个耳式支座4。In this example, the reactor barrel 1 includes a plurality of ear supports 4 arranged on the reactor body 11 and passing through the heat transfer jacket 13 and the insulation layer 14.
综上,本申请通过可拆卸连接地反应器盖体12与反应器本体11的配合,并结合搅拌装置、设置在反应器盖体12上的超声波振动装置共同作用,实现了整个装置方便更换、调整的优点,尤其是结合高速搅拌剪切与超声分散于一体,在实现无机纳米粒子有效分散的同时实现表面改性,不仅简化了操作步骤,而且大大提高了分散以及改性效果,避免了无机纳米粒子团聚效应造成的改性不彻底,使得改性后的无机纳米粒子实现单分散,真正发挥纳米效应。In summary, the present application realizes the easy replacement of the entire device through the cooperation of the detachably connected reactor cover 12 and the reactor body 11, combined with the stirring device and the ultrasonic vibration device provided on the reactor cover 12, The advantages of adjustment, especially the combination of high-speed stirring and shearing and ultrasonic dispersion, can realize the effective dispersion of inorganic nanoparticles while realizing surface modification, which not only simplifies the operation steps, but also greatly improves the dispersion and modification effects, and avoids inorganic nanoparticles. The incomplete modification caused by the agglomeration effect of nanoparticles makes the modified inorganic nanoparticles achieve monodispersion and truly exert the nanometer effect.
上述实施例只为说明本申请的技术构思及特点,其目的在于让熟悉此项技术的人士能够了解本申请的内容并据以实施,并不能以此限制本申请的保护范围,凡根据本申请精神实质所作的等效变化或修饰,都应涵盖在本申请的保护范围之内。The above embodiments are only to illustrate the technical ideas and features of this application, and their purpose is to enable those familiar with this technology to understand the content of this application and implement it accordingly, and cannot limit the scope of protection of this application. Equivalent changes or modifications made to the spirit and substance shall be covered by the scope of protection of this application.

Claims (10)

  1. 一种分散反应器,所述分散反应器包括反应器筒体、部分设置在所述反应器筒体内部的搅拌装置,其特征在于,所述反应器筒体包括反应器本体、与所述反应器本体可拆卸地连接且用于盖合所述反应器本体的反应器盖体,所述搅拌装置部分穿过所述反应器盖体伸入所述反应器本体内;所述分散反应器还包括超声波振动装置,所述超声波振动装置包括设置在所述反应器盖体上的超声波发生器、与所述超声波发生器连接的超声波换能器、与所述超声波换能器连接的变幅杆,以及与所述变幅杆连接的超声波振动棒,所述超声波振动棒伸入所述反应器本体内。A dispersion reactor comprising a reactor cylinder and a stirring device partially arranged inside the reactor cylinder, characterized in that the reactor cylinder includes a reactor body and is The reactor body is detachably connected and used to cover the reactor body of the reactor body, and the stirring device partially penetrates the reactor body to extend into the reactor body; the dispersion reactor also Including an ultrasonic vibrating device, the ultrasonic vibrating device including an ultrasonic generator arranged on the reactor cover, an ultrasonic transducer connected to the ultrasonic generator, and an horn connected to the ultrasonic transducer , And an ultrasonic vibrating rod connected to the horn, the ultrasonic vibrating rod extends into the reactor body.
  2. 根据权利要求1所述的分散反应器,其特征在于,所述超声波振动棒沿上下方向延伸。The dispersion reactor according to claim 1, wherein the ultrasonic vibrating rod extends in a vertical direction.
  3. 根据权利要求1或2所述的分散反应器,其特征在于,所述超声波振动装置具有至少两个且绕着所述搅拌装置对称分布。The dispersion reactor according to claim 1 or 2, wherein the ultrasonic vibration device has at least two and is symmetrically distributed around the stirring device.
  4. 根据权利要求1所述的分散反应器,其特征在于,所述搅拌装置包括通过支撑架固定设置在所述反应器盖体上的驱动部件、与所述驱动部件传动连接的联轴器、与所述联轴器传动连接且穿过所述反应器盖体并伸入所述反应器本体内的搅拌轴,以及设置在所述搅拌轴下部的搅拌桨叶。The dispersion reactor according to claim 1, wherein the stirring device comprises a driving part fixedly arranged on the cover of the reactor through a support frame, a coupling connected with the driving part, and The coupling is drivingly connected to a stirring shaft that passes through the reactor cover and extends into the reactor body, and a stirring blade arranged at the lower part of the stirring shaft.
  5. 根据权利要求4所述的分散反应器,其特征在于,所述搅拌桨叶具有至少两个且沿上下方向依次设置在所述搅拌轴上。The dispersion reactor according to claim 4, wherein the stirring blade has at least two and is sequentially arranged on the stirring shaft in an up and down direction.
  6. 根据权利要求5所述的分散反应器,其特征在于,所述搅拌桨叶具有设置在所述搅拌轴下端部的第一盘式搅拌桨叶、设置在所述第一盘式搅拌桨叶上方的第二盘式搅拌桨叶,所述第一盘式搅拌桨叶位于所述超声波振动棒下方,且所述超声波振动棒位于所述第二盘式搅拌桨叶的外侧。The dispersion reactor according to claim 5, wherein the stirring blade has a first disc stirring blade arranged at the lower end of the stirring shaft, and is arranged above the first disc stirring blade The second disc stirring blade, the first disc stirring blade is located below the ultrasonic vibrating rod, and the ultrasonic vibrating rod is located outside the second disc stirring blade.
  7. 根据权利要求6所述的分散反应器,其特征在于,所述第一盘式搅拌桨叶包括桨叶本体以及形成在所述桨叶本体外周的多个叶片,所述的多个叶片两两之间具有间隔,所述桨叶本体的下部向下凸起形成与所述反应器本体底部相适应的弧形部。The dispersion reactor according to claim 6, wherein the first disc stirring blade comprises a blade body and a plurality of blades formed on the outer periphery of the blade body, and the plurality of blades are paired by two. There is a gap therebetween, and the lower part of the blade body protrudes downward to form an arc-shaped part that is compatible with the bottom of the reactor body.
  8. 根据权利要求1所述的分散反应器,其特征在于,所述反应器筒体还包括包覆在所述反应器本体上的传热夹套、包覆在所述传热夹套外壁的保温层,所述传热夹套具有分别穿过所述保温层的换热流体进口和换热流体出口,所述换热流体进口位于所述传热夹套的下部,所述换热流体出口位于所述传热夹套的上部。The dispersion reactor according to claim 1, wherein the reactor barrel further comprises a heat transfer jacket coated on the reactor body, and a heat preservation jacket coated on the outer wall of the heat transfer jacket Layer, the heat transfer jacket has a heat exchange fluid inlet and a heat exchange fluid outlet respectively passing through the insulation layer, the heat exchange fluid inlet is located at the lower part of the heat transfer jacket, and the heat exchange fluid outlet is located at The upper part of the heat transfer jacket.
  9. 根据权利要求8所述的分散反应器,其特征在于,所述反应器筒体还包括设置在所述反应器本体底部且分别穿过所述传热夹套、所述保温层的出料管。The dispersion reactor according to claim 8, wherein the reactor barrel further comprises a discharge pipe arranged at the bottom of the reactor body and respectively passing through the heat transfer jacket and the insulation layer .
  10. 根据权利要求1所述的分散反应器,其特征在于,所述反应器盖体上分别设置有手孔、物料视镜、温度计插孔以及用于固定所述超声波振动装置的法兰。The dispersion reactor according to claim 1, wherein a hand hole, a material sight glass, a thermometer socket, and a flange for fixing the ultrasonic vibration device are respectively provided on the reactor cover.
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