WO2021109729A1 - Inorganic powder modification system - Google Patents

Inorganic powder modification system Download PDF

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Publication number
WO2021109729A1
WO2021109729A1 PCT/CN2020/121845 CN2020121845W WO2021109729A1 WO 2021109729 A1 WO2021109729 A1 WO 2021109729A1 CN 2020121845 W CN2020121845 W CN 2020121845W WO 2021109729 A1 WO2021109729 A1 WO 2021109729A1
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Prior art keywords
reactor
inorganic powder
modification system
ultrasonic
stirring
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PCT/CN2020/121845
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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 WO2021109729A1 publication Critical patent/WO2021109729A1/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
    • B01F27/90Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80Mixing plants; Combinations of mixers
    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C21/00Disintegrating plant with or without drying of the material

Definitions

  • This application belongs to the field of composite material preparation, in particular to the preparation of an inorganic powder and its composite modification with organic materials, and in particular to an inorganic powder modification system.
  • the mixture of polymer matrix and additives whose at least one dimension is in the nanometer category is called polymer-based nanocomposite.
  • adding a small amount of nano-dispersed phase can significantly improve the performance of the composite material.
  • Research on nano-reinforced polymer-based composites believes that the high specific surface area and high surface activity of the nano-dispersed phase, as well as the exotic physical and chemical properties exhibited by the nanoparticles, strengthen the relationship between the nano-dispersed phase and the polymer matrix.
  • the presence of the phase changes the aggregate structure of the polymer matrix or affects the movement characteristics of the polymer molecules, so that the macroscopic properties of the nanocomposite can be improved.
  • Inorganic powders need to be ultra-refined before they are compounded with polymer materials, that is, they are ground to a smaller particle size by mechanical methods. Most ultra-fine inorganic powders are due to surface hydrophilicity, and most polymer materials are It is hydrophobic and lipophilic, causing inorganic powders to be easily agglomerated, difficult to mix, and poorly modified if they are directly added to polymer materials. Therefore, it is generally necessary to treat inorganic powders and polymers before compounding them. Surface modification of powders, especially nano-sized powders (such as nano-silica, etc.) requires surface treatment to improve its compatibility and dispersion stability with polymer materials.
  • the ultra-fine inorganic powder and its surface modification process are carried out step by step.
  • the first is to use a sand mill to grind to a certain degree of fineness (particle size is 0.3-5 ⁇ m), and the second step is to use ultrasonic equipment.
  • the third step is to move into the reactor for surface hydrophobic modification.
  • the micro-nano solution is solid-liquid separated and filtered to obtain the micro-nano modified powder; however, on the one hand, the above operations are more complicated , And it is a batch operation with low efficiency; on the other hand, due to the transfer of nanoparticles in the batch operation, the nanoparticles will partially reaggregate during the transfer process, which greatly affects the subsequent surface modification effect, and it is difficult to obtain a good dispersion The solution of nano-particles, therefore, it is impossible to prepare an ideal nano-composite material.
  • the technical problem to be solved by this application is to overcome the shortcomings of the prior art and provide a new type of inorganic powder modification system, which can combine the grinding, dispersion and surface integration of inorganic powder, and at the same time, the dispersion and modification are also reduced. It can be carried out synchronously, avoiding the incomplete modification caused by the agglomeration effect of inorganic nanoparticles, making the modified inorganic nanoparticles realize monodispersion, truly exerting the nanometer effect, and basically realizing the continuous effect with high efficiency.
  • an inorganic powder modification system the modification system includes a premixing device, a grinding device, a dispersion reactor and a filtering device connected in sequence; wherein, the The dispersion reactor includes a reactor barrel and a stirring device partially arranged inside the reactor barrel.
  • the reactor barrel includes a reactor body, is detachably connected to the reactor body, and is used to cover the reactor.
  • the dispersion reactor also includes an ultrasonic vibration device, the ultrasonic vibration device includes a set The ultrasonic generator on the cover of the reactor, the ultrasonic transducer connected with the ultrasonic generator, the horn connected with the ultrasonic transducer, and the said horn connected with the ultrasonic transducer
  • 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 connected to the driving part in transmission, and the coupling
  • the device is connected to a stirring shaft which passes through the cover body of the reactor and extends into the body of 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 bottom of the device body passes through the heat transfer jacket and the discharge pipe of the insulation layer, and the heat transfer jacket has a heat exchange fluid inlet and a heat exchange fluid outlet that respectively pass through the insulation layer.
  • the heat exchange fluid inlet is located at the lower part of the heat transfer jacket
  • the heat exchange fluid outlet is located at the upper part of the heat transfer jacket
  • the discharge pipe is in communication with the filter device.
  • the modification system further includes a circulating pipe arranged between the premixing device and the grinding device, and the upper edge of the circulating pipe extends from one end communicating with the grinding device to A circulating pneumatic discharge valve and a laser particle size analyzer are sequentially arranged in the direction of the other end of the communication of the premixing device.
  • the grinding device and the dispersion reactor are connected through an inorganic powder feed pipe, and the inorganic powder feed pipe is provided with a feed pneumatic discharge valve, and the circulation pipe is connected to the The inorganic powder feed pipe is in communication.
  • one of the feed pneumatic discharge valve and the circulating pneumatic discharge valve is in an open state, and the other is in a closed state.
  • the modification system further includes a modifier pre-storage tank, a vacuum system connected to the modifier pre-storage tank, and the modifier pre-storage tank passes through the reactor cover
  • the body is in communication with the reactor body.
  • the modification system further includes a reflux condensation device that communicates with the reactor body through the reactor cover, and the reflux condensation device includes a fractionation column that communicates with the reactor body.
  • the reflux condensation device includes a fractionation column that communicates with the reactor body.
  • a vertical condenser communicating with the fractionating column, a horizontal condenser communicating with the vertical condenser, an oil-water separator communicating with the horizontal condenser, and a vent communicating with the oil-water separator Tube
  • the vacuum system is in communication with the vent tube.
  • 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.
  • This application realizes the integrated grinding, dispersion and modification of inorganic powder through the pre-mixing device, grinding device, dispersing reactor and filtering device connected in sequence, and basically realizes the continuous effect with high efficiency; especially through the detachable
  • the surface modification is realized while realizing the effective dispersion of inorganic nanoparticles, which not only simplifies the operation steps, but also greatly improves the dispersion and modification effect, avoiding the incomplete modification caused by the agglomeration effect of inorganic nanoparticles, making the modification
  • the latter inorganic nanoparticles realize monodispersion and truly exert the nanometer effect.
  • Figure 1 is a schematic diagram of the overall structure of the inorganic powder modification system of the application.
  • Figure 2 is a schematic diagram of the overall structure of the dispersion reactor included in the inorganic powder modification system of the application;
  • 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 application, "a plurality of” means at least two, such as two, three, etc., unless specifically 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.
  • 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.
  • this example provides an inorganic powder modification system.
  • the modification system includes a premixing device A, a grinding device B, a dispersion reactor C, and a filtering device D that are connected in sequence;
  • the premixing device A, grinding device B, dispersing reactor C and filtering device D realize the integrated grinding, dispersion and modification of inorganic powder, and basically realize the continuous effect, and the work efficiency is high.
  • the dispersion reactor C 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 that is detachably connected to the reactor body 11. And for covering the reactor cover 12 of the reactor body 11, the stirring device partially penetrates the reactor cover 12 and extends into the reactor body 11; the dispersion reactor C also includes an ultrasonic vibration device, the ultrasonic vibration device includes The ultrasonic generator 31 on the reactor cover 12, the ultrasonic transducer (not shown) connected with the ultrasonic generator 31, the horn connected with the ultrasonic transducer, and the ultrasonic vibrating rod connected with the horn 32. 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 parts 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 dispersed extremely well.
  • 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 also includes a discharge pipe 15 arranged at the bottom of the reactor body 11 and respectively passing through the heat transfer jacket 13 and the heat preservation layer 14.
  • the discharge pipe 15 is in communication with the filter device D, and the filter device D Used for solid-liquid separation, that is, to separate the modified inorganic powder from other liquids such as solvents and other substances.
  • 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 combination of the detachable connection of the reactor cover 12 and the reactor body 11, combined with the stirring device and the ultrasonic vibration device provided on the reactor cover 12, achieves the advantages of convenient replacement and adjustment of the entire device.
  • the surface modification can be realized while realizing the effective dispersion of inorganic nanoparticles, 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 resulting incomplete modification makes the modified inorganic nanoparticles achieve monodispersion and truly exert the nanometer effect.
  • the premixing device A can be a commonly used stirring reactor device in the prior art.
  • a structure similar to that of the dispersion reactor C of the present application is adopted, and the ultrasonic vibration device can be omitted on the basis of the dispersion reactor C.
  • the grinding device B may be a pin horizontal sand mill commonly used in the prior art. Specifically, it can be communicated with the premixing device A through a feed pump, and then passed into the intermediate storage tank after grinding, and the intermediate storage tank communicates with the subsequent.
  • the modification system also includes a circulating pipe E arranged between the premixing device A and the grinding device B, that is, the two ends of the circulating pipe E are respectively connected to the premixing device A and the grinding device B, and the upper edge of the circulating pipe E is from A circulating pneumatic discharge valve F, a laser particle analyzer G, a flow meter, etc. are arranged in the direction from one end communicating with the grinding device B to the other end communicating with the premixing device A.
  • the design of the circulation pipe E can make the mixture of inorganic powder and solvent in the premixing device A be ground, and the particle size can be monitored in time. If it does not meet the requirements, the circulation pipe E can be used to make the mixed solution in the premixing device Continuously circulating grinding between A and grinding device B until the particle size requirements are met, laying the foundation for the thorough modification of the subsequent inorganic powder.
  • the grinding device B and the dispersion reactor C are connected through an inorganic powder feed pipe H, and the inorganic powder feed pipe H is provided with a feed pneumatic discharge valve I, a circulation pipe E and the inorganic powder
  • the feed pipe H is connected.
  • one of the feed pneumatic discharge valve I and the circulating pneumatic discharge valve F is in an open state, and the other is in a closed state. This setting can ensure that the inorganic material is passed into the dispersion reactor C.
  • the particle size of the powder is within the required range.
  • the modification system also includes a modifier pre-storage tank J and a vacuum system K connected to the modifier pre-storage tank J.
  • the modifier pre-storage tank J is in communication with the reactor body 11 through the reactor cover 12 .
  • the setting of the vacuum system K can make the modifier be pressed from the storage tank to the modifier pre-storage tank J under negative pressure, reducing the use of the motor.
  • the modification system also includes a reflux condenser connected to the reactor body 11 through the reactor cover 12, and the reflux condenser includes a fractionating column L1 connected to the reactor body 11, and a vertical condenser connected to the fractionating column L1.
  • the setting of the reflux condensing device can cause too much solvent in the modified system to affect the filtration efficiency in the later stage.
  • the internal solvent can be evaporated by heating the reactor body 11, and then processed and recycled through the condensing reflux device, and the vacuum system
  • the function of K communication is to keep the oil-water separator L4 in a negative pressure state, so that the solvent can be collected smoothly.
  • the inorganic powder and solvent are initially mixed in the premixing device A, and then passed into the grinding device B for grinding.
  • the circulating pneumatic discharge valve F is in an open state
  • the feed pneumatic discharge valve I is in the closed state.
  • the laser particle size analyzer G detects that the particle size of the inorganic powder in the system meets the requirements, adjust the circulating pneumatic discharge valve F to the closed state, and open the feed pneumatic discharge valve I to feed into the dispersion reactor C.
  • the modifier is added accordingly (that is, the discharge valve of the modifier pre-storage tank J is opened to feed the dispersion reactor C), and the frequency of the driving part 21 is adjusted as needed to make the inorganic powder
  • the body is well dispersed in the dispersion reactor C and modified at the same time.
  • the heat transfer medium in the heat transfer jacket 13 can be a thermal fluid, etc.; when the inorganic particles are materials such as boron nitride, mica or montmorillonite, the transfer The heat transfer medium in the heat jacket 13 is set to alternate between freezing liquid and hot fluid to achieve freezing and thawing, combined with high-speed stirring and shearing and ultrasonic dispersion, to obtain exfoliated two-dimensional nanomaterials, and then perform modification operations As well as other corresponding subsequent operations, the above-mentioned heat transfer medium can be produced by the heat transfer medium production device M.
  • the thermal fluid can be hot water, thermal oil, etc.
  • the refrigerant can be liquid nitrogen, and so on.
  • this application realizes the integrated grinding, dispersion and modification of inorganic powder through the pre-mixing device A, grinding device B, dispersing reactor C, and filtering device D that are connected in sequence, and basically realizes the continuous effect and efficiency High; especially 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, to realize the convenient replacement and adjustment of the entire device
  • it combines high-speed stirring and shearing and ultrasonic dispersion to achieve surface modification while achieving effective dispersion of inorganic nanoparticles, 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 makes the modified inorganic nanoparticles achieve monodispersion and truly exert the nanometer effect.

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Abstract

An inorganic powder modification system, comprising a premixing device (A), a grinding device (B), a dispersion reactor (C), and a filtering device (D) which are communicated in sequence. The dispersion reactor (C) comprises a reactor cylinder (1), a stirring device, and an ultrasonic vibration device, the reactor cylinder (1) comprises a reactor body (11) and a reactor cover (12), and the stirring device partially penetrates through the reactor cover (12) and extends into the reactor body (11); the ultrasonic vibration device comprises an ultrasonic generator (31) arranged on the reactor cover (12), an ultrasonic transducer connected to the ultrasonic generator (31), a horn connected to the ultrasonic transducer, and an ultrasonic vibration rod (32) connected to the horn, and the ultrasonic vibration rod (32) extends into the reactor body (11).

Description

一种无机粉体改性系统An inorganic powder modification system
本申请要求申请号为:CN201922181197.4、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 CN201922181197.4 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,尤其涉及一种无机粉体的制备及其与有机材料的复合改性,具体涉及一种无机粉体改性系统。This application belongs to the field of composite material preparation, in particular to the preparation of an inorganic powder and its composite modification with organic materials, and in particular to an inorganic powder modification system.
背景技术Background technique
聚合物基体与至少一维是纳米范畴的添加剂所组成的混合物称之为聚合物基纳米复合材料。通常少量添加纳米分散相,即可使复合材料的性能得到明显改善。纳米增强聚合物基复合材料的研究认为,纳米分散相的高比表面积与高表面活性,以及纳米粒子所表现出的奇异理化特性使得纳米分散相与聚合物基体之间的联系得以加强,纳米分散相的存在改变了聚合物基的聚集态结构或影响了聚合物分子的运动特性,使得纳米复合材料的宏观性能得以改善。The mixture of polymer matrix and additives whose at least one dimension is in the nanometer category is called polymer-based nanocomposite. Generally, adding a small amount of nano-dispersed phase can significantly improve the performance of the composite material. Research on nano-reinforced polymer-based composites believes that the high specific surface area and high surface activity of the nano-dispersed phase, as well as the exotic physical and chemical properties exhibited by the nanoparticles, strengthen the relationship between the nano-dispersed phase and the polymer matrix. The presence of the phase changes the aggregate structure of the polymer matrix or affects the movement characteristics of the polymer molecules, so that the macroscopic properties of the nanocomposite can be improved.
无机粉体在与高分子材料复合前需要进行超细化处理,即采用机械法研磨至较小的粒径,大多数超细化无机粉体由于表面亲水性,而大多数高分子材料又是疏水亲油的,导致无机粉体如直接添加到高分子材料中,易发生团聚、混合困难、改性效果差;因此,一般在将无机粉体与高分子复合前,往往需要先对无机粉体进行表面改性,特别是纳米级粉体(如纳米二氧化硅等)更需进行表面处理,提高其与高分子材料的相容性和分散稳定性。Inorganic powders need to be ultra-refined before they are compounded with polymer materials, that is, they are ground to a smaller particle size by mechanical methods. Most ultra-fine inorganic powders are due to surface hydrophilicity, and most polymer materials are It is hydrophobic and lipophilic, causing inorganic powders to be easily agglomerated, difficult to mix, and poorly modified if they are directly added to polymer materials. Therefore, it is generally necessary to treat inorganic powders and polymers before compounding them. Surface modification of powders, especially nano-sized powders (such as nano-silica, etc.) requires surface treatment to improve its compatibility and dispersion stability with polymer materials.
目前,无机粉体超细化及其表面改性工艺都是分步进行的,第一是采用砂磨机研磨至一定细度(粒径在0.3~5μm),第二步是在超声波设备中进行超声分散处理,第三步是移入到反应器中进行表面疏水改性,改性完成后对微纳米溶液进行固液分离,过滤得到微纳米改性粉体;但是,一方面上述操作较为复杂,且是间歇式操作,效率较低;另一方面由于间歇式操作存在纳米颗粒转移,而在转移过程中,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, the ultra-fine inorganic powder and its surface modification process are carried out step by step. The first is to use a sand mill to grind to a certain degree of fineness (particle size is 0.3-5μm), and the second step is to use ultrasonic equipment. For ultrasonic dispersion treatment, the third step is to move into the reactor for surface hydrophobic modification. After the modification is completed, the micro-nano solution is solid-liquid separated and filtered to obtain the micro-nano modified powder; however, on the one hand, the above operations are more complicated , And it is a batch operation with low efficiency; on the other hand, due to the transfer of nanoparticles in the batch operation, the nanoparticles will partially reaggregate during the transfer process, which greatly affects the subsequent surface modification effect, and it is difficult to obtain a good dispersion The solution of nano-particles, therefore, it is impossible to prepare an ideal nano-composite material.
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,提供一种新型的无机粉体改性系统,其能够兼具无机粉体的研磨、分散以及表面一体化进行,同时分散与改性还能同步进行,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,且基本实现连续化作用,效率高。The technical problem to be solved by this application is to overcome the shortcomings of the prior art and provide a new type of inorganic powder modification system, which can combine the grinding, dispersion and surface integration of inorganic powder, and at the same time, the dispersion and modification are also reduced. It can be carried out synchronously, avoiding the incomplete modification caused by the agglomeration effect of inorganic nanoparticles, making the modified inorganic nanoparticles realize monodispersion, truly exerting the nanometer effect, and basically realizing the continuous effect with high efficiency.
为解决以上技术问题,本申请采取的技术方案如下:一种无机粉体改性系统,所述改性系统包括依次连通的预混装置、研磨装置、分散反应器和过滤装置;其中,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。In order to solve the above technical problems, the technical solution adopted by this application is as follows: an inorganic powder modification system, the modification system includes a premixing device, a grinding device, a dispersion reactor and a filtering device connected in sequence; wherein, the The dispersion reactor includes a reactor barrel and a stirring device partially arranged inside the reactor barrel. The reactor barrel includes a reactor body, is detachably connected to the reactor body, and is used to cover the reactor. The reactor cover of 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 a set The ultrasonic generator on the cover of the reactor, the ultrasonic transducer connected with the ultrasonic generator, the horn connected with the ultrasonic transducer, and the said horn connected with the ultrasonic transducer The ultrasonic vibrating rod extends into the body of the reactor.
根据本申请的一些优选方面,所述超声波振动棒沿上下方向延伸。According to some preferred aspects of the present application, the ultrasonic vibrating rod extends in the up and down direction.
根据本申请的一些优选方面,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 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且优选的方面,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 and preferred aspects of the present application, the stirring device includes a driving part fixedly arranged on the reactor cover through a support frame, a coupling connected to the driving part in transmission, and the coupling The device is connected to a stirring shaft which passes through the cover body of the reactor and extends into the body of 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以及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,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,所述出料管与所述过滤装置连通。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 bottom of the device body passes through the heat transfer jacket and the discharge pipe of the insulation layer, and the heat transfer jacket has a heat exchange fluid inlet and a heat exchange fluid outlet that respectively pass through the insulation layer. The heat exchange fluid inlet is located at the lower part of the heat transfer jacket, the heat exchange fluid outlet is located at the upper part of the heat transfer jacket, and the discharge pipe is in communication with the filter device.
根据本申请的一些优选方面,所述改性系统还包括设置在所述预混装置与所述研磨装置之间的循环管,所述循环管上沿从与所述研磨装置连通的一端至与所述预混装置连通的另一端方向依次设置有循环气动放料阀、激光粒度仪。According to some preferred aspects of the present application, the modification system further includes a circulating pipe arranged between the premixing device and the grinding device, and the upper edge of the circulating pipe extends from one end communicating with the grinding device to A circulating pneumatic discharge valve and a laser particle size analyzer are sequentially arranged in the direction of the other end of the communication of the premixing device.
根据本申请的一些优选方面,所述研磨装置与所述分散反应器通过无机粉体进料管连通,所述无机粉体进料管上设置有进料气动放料阀,所述循环管与所述无机粉体进料管连通。According to some preferred aspects of the present application, the grinding device and the dispersion reactor are connected through an inorganic powder feed pipe, and the inorganic powder feed pipe is provided with a feed pneumatic discharge valve, and the circulation pipe is connected to the The inorganic powder feed pipe is in communication.
根据本申请的一些具体方面,在所述改性系统工作中,所述进料气动放料阀与所述循环气动放料阀中的一个处于打开状态,另一个则处于关闭状态。According to some specific aspects of the present application, during the operation of the modification system, one of the feed pneumatic discharge valve and the circulating pneumatic discharge valve is in an open state, and the other is in a closed state.
根据本申请的一些优选方面,所述改性系统还包括改性剂预储罐、与所述改性剂预储罐连通的真空系统,所述改性剂预储罐通过所述反应器盖体与所述反应器本体连通。According to some preferred aspects of the application, the modification system further includes a modifier pre-storage tank, a vacuum system connected to the modifier pre-storage tank, and the modifier pre-storage tank passes through the reactor cover The body is in communication with the reactor body.
根据本申请的一些优选方面,所述改性系统还包括通过所述反应器盖体与所述反应器本体连通的回流冷凝装置,所述回流冷凝装置包括与所述反应器本体连通的分馏柱、与所述分馏柱连通的立式冷凝器、与所述立式冷凝器连通的卧式冷凝器、与所述卧式冷凝器连通的油水分离器、与所述油水分离器连通的放空管,所述真空系统与所述放空管连通。According to some preferred aspects of the present application, the modification system further includes a reflux condensation device that communicates with the reactor body through the reactor cover, and the reflux condensation device includes a fractionation column that communicates with the reactor body. , A vertical condenser communicating with the fractionating column, a horizontal condenser communicating with the vertical condenser, an oil-water separator communicating with the horizontal condenser, and a vent communicating with the oil-water separator Tube, the vacuum system is in communication with the vent tube.
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:
本申请通过依次连通的预混装置、研磨装置、分散反应器和过滤装置实现了无机粉体的研磨、分散以及改性一体化进行,且基本实现连续化作用,效率高;尤其是通过可拆卸连接地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,同时结合高速搅拌与超声分散于一体,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。This application realizes the integrated grinding, dispersion and modification of inorganic powder through the pre-mixing device, grinding device, dispersing reactor and filtering device connected in sequence, and basically realizes the continuous effect with high efficiency; especially through the detachable The cooperation between the connected reactor cover and the reactor body, combined with the stirring device and the ultrasonic vibration device arranged on the reactor cover, realizes the advantages of convenient replacement and adjustment of the entire device, and combines high-speed stirring and ultrasonic dispersion. In one, the surface modification is realized while realizing the effective dispersion of inorganic nanoparticles, which not only simplifies the operation steps, but also greatly improves the dispersion and modification effect, avoiding the incomplete modification caused by the agglomeration effect of inorganic nanoparticles, making the modification The latter inorganic nanoparticles realize monodispersion and truly exert the nanometer effect.
附图说明Description of the drawings
图1为本申请无机粉体改性系统的整体结构示意图;Figure 1 is a schematic diagram of the overall structure of the inorganic powder modification system of the application;
图2为本申请无机粉体改性系统包含的分散反应器的整体结构示意图;Figure 2 is a schematic diagram of the overall structure of the dispersion reactor included in the inorganic powder modification system of the application;
其中,A、预混装置;B、研磨装置;C、分散反应器;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;D、过滤装置;E、循环管;F、循环气动放料阀;G、激光粒度仪;H、无机粉体进料管;I、进料气动放料阀;J、改性剂预储罐;K、真空系统;L1、分馏柱;L2、立式冷凝器;L3、卧式冷凝器;L4、油水分离器;L5、放空管;M、传热介质生产装置。Among them, A. Premixing device; B. Grinding device; C. Dispersion reactor; 1. Reactor cylinder; 11. Reactor body; 12. Reactor cover; 121. Hand hole; 122. Material sight glass; 123. Thermometer jack; 124. Flange; 13. Heat transfer jacket; 131. Heat exchange fluid inlet; 132. Heat exchange fluid outlet; 14. Insulation layer; 15. Discharge pipe; 21. Drive parts; 22. Coupling; 23. Stirring shaft; 24. The first disc stirring blade; 25. The second disc stirring blade; 31. Ultrasonic generator; 32. Ultrasonic vibrating rod; 4. Ear support; 5. Bolt screw connection; D, filter device; E, circulating pipe; F, circulating pneumatic discharge valve; G, laser particle size analyzer; H, inorganic powder feeding pipe; I, feeding pneumatic discharge valve; J, modification Sexual agent pre-storage tank; K, vacuum system; L1, fractionating column; L2, vertical condenser; L3, horizontal condenser; L4, oil-water separator; L5, vent pipe; M, heat transfer medium production device.
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。在本申请的描述中,“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 application, "a plurality of" means at least two, such as two, three, etc., unless specifically defined otherwise.
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1-2所示,本例提供了一种无机粉体改性系统,改性系统包括依次连通的预混装置A、研磨装置B、分散反应器C和过滤装置D;通过上述依次连通的预混装置A、研磨装置B、分散反应器C和过滤装置D实现了无机粉体的研磨、分散以及改性一体化进行,且基本实现连续化作用,工作效率高。As shown in Figure 1-2, this example provides an inorganic powder modification system. The modification system includes a premixing device A, a grinding device B, a dispersion reactor C, and a filtering device D that are connected in sequence; The premixing device A, grinding device B, dispersing reactor C and filtering device D realize the integrated grinding, dispersion and modification of inorganic powder, and basically realize the continuous effect, and the work efficiency is high.
如图2所示,分散反应器C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C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 2, the dispersion reactor C 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 that is detachably connected to the reactor body 11. And for covering the reactor cover 12 of the reactor body 11, the stirring device partially penetrates the reactor cover 12 and extends into the reactor body 11; the dispersion reactor C also includes an ultrasonic vibration device, the ultrasonic vibration device includes The ultrasonic generator 31 on the reactor cover 12, the ultrasonic transducer (not shown) connected with the ultrasonic generator 31, the horn connected with the ultrasonic transducer, and the ultrasonic vibrating rod connected with the horn 32. 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地分散。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 parts 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 dispersed extremely well.
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,出料管15与过滤装置D连通,过滤装置D用于固液分离,即分离出改性后的无机粉体与其它液体例如溶剂等物质。In this example, the reactor barrel 1 also includes a discharge pipe 15 arranged at the bottom of the reactor body 11 and respectively passing through the heat transfer jacket 13 and the heat preservation layer 14. The discharge pipe 15 is in communication with the filter device D, and the filter device D Used for solid-liquid separation, that is, to separate the modified inorganic powder from other liquids such as solvents and other substances.
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.
上述通过可拆卸连接的反应器盖体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。The combination of the detachable connection of the reactor cover 12 and the reactor body 11, combined with the stirring device and the ultrasonic vibration device provided on the reactor cover 12, achieves the advantages of convenient replacement and adjustment of the entire device. Especially by combining high-speed stirring and shearing and ultrasonic dispersion, the surface modification can be realized while realizing the effective dispersion of inorganic nanoparticles, 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 resulting incomplete modification makes the modified inorganic nanoparticles achieve monodispersion and truly exert the nanometer effect.
本例中,预混装置A可以为现有技术中常用的搅拌反应釜装置。优选地采用与本申请分散反应器C的类似结构,可以在分散反应器C的基础上省略超声波振动装置即可。In this example, the premixing device A can be a commonly used stirring reactor device in the prior art. Preferably, a structure similar to that of the dispersion reactor C of the present application is adopted, and the ultrasonic vibration device can be omitted on the basis of the dispersion reactor C.
本例中,研磨装置B可以为现有技术中常用的棒销卧式砂磨机。具体地,其可以通过进料泵与预混装置A连通,然后研磨之后通入中间储罐,由中间储罐与后续连通。In this example, the grinding device B may be a pin horizontal sand mill commonly used in the prior art. Specifically, it can be communicated with the premixing device A through a feed pump, and then passed into the intermediate storage tank after grinding, and the intermediate storage tank communicates with the subsequent.
进一步地,改性系统还包括设置在预混装置A与研磨装置B之间的循环管E,即循环管E的两端分别与预混装置A、研磨装置B连通,循环管E上沿从与研磨装置B连通的一端至与预混装置A连通的另一端方向依次设置有循环气动放料阀F、激光粒度仪G、流量计等等。此处循环管E的设计可以使得预混装置A中的无机粉体与溶剂的混合液经过研磨之后,及时监测粒度,若不符合要求,则可以通过此循环管E使混合液在预混装置A与研磨装置B之间持续循环研磨直至符合粒度要求,为后续无机粉体的彻底改性奠定基础。Further, the modification system also includes a circulating pipe E arranged between the premixing device A and the grinding device B, that is, the two ends of the circulating pipe E are respectively connected to the premixing device A and the grinding device B, and the upper edge of the circulating pipe E is from A circulating pneumatic discharge valve F, a laser particle analyzer G, a flow meter, etc. are arranged in the direction from one end communicating with the grinding device B to the other end communicating with the premixing device A. Here, the design of the circulation pipe E can make the mixture of inorganic powder and solvent in the premixing device A be ground, and the particle size can be monitored in time. If it does not meet the requirements, the circulation pipe E can be used to make the mixed solution in the premixing device Continuously circulating grinding between A and grinding device B until the particle size requirements are met, laying the foundation for the thorough modification of the subsequent inorganic powder.
进一步地,本例中,研磨装置B与分散反应器C通过无机粉体进料管H连通,无机粉体进料管H上设置有进料气动放料阀I,循环管E与无机粉体进料管H连通。其中,在改性系统工作中,进料气动放料阀I与循环气动放料阀F中的一个处于打开状态,另一个则处于关闭状态,此设置可以确保通入分散反应器C中的无机粉体的粒度在要求范围内。Further, in this example, the grinding device B and the dispersion reactor C are connected through an inorganic powder feed pipe H, and the inorganic powder feed pipe H is provided with a feed pneumatic discharge valve I, a circulation pipe E and the inorganic powder The feed pipe H is connected. Among them, in the work of the modification system, one of the feed pneumatic discharge valve I and the circulating pneumatic discharge valve F is in an open state, and the other is in a closed state. This setting can ensure that the inorganic material is passed into the dispersion reactor C. The particle size of the powder is within the required range.
本例中,改性系统还包括改性剂预储罐J、与改性剂预储罐J连通的真空系统K,改性剂预储罐J通过反应器盖体12与反应器本体11连通。真空系统K的设置可以使得改性剂在负压状态下从储存罐内被压向改性剂预储罐J,减少电机的使用。In this example, the modification system also includes a modifier pre-storage tank J and a vacuum system K connected to the modifier pre-storage tank J. The modifier pre-storage tank J is in communication with the reactor body 11 through the reactor cover 12 . The setting of the vacuum system K can make the modifier be pressed from the storage tank to the modifier pre-storage tank J under negative pressure, reducing the use of the motor.
本例中,改性系统还包括通过反应器盖体12与反应器本体11连通的回流冷凝装置,回流冷凝装置包括与反应器本体11连通的分馏柱L1、与分馏柱L1连通的立式冷凝器L2、与立式冷凝器L2连通的卧式冷凝器L3、与卧式冷凝器L3连通的油水分离器L4、与油水分离器L4连通的放空管L5,真空系统K与放空管L5连通。此冷凝回流装 置的设置可以使得在改性后体系中溶剂过多影响后期过滤效率,因此,可以通过加热反应器本体11以使得内部的溶剂蒸发,然后经由冷凝回流装置处理回收利用,与真空系统K连通的作用是可以保持油水分离器L4处于负压状态,使得溶剂能够顺利被收集。In this example, the modification system also includes a reflux condenser connected to the reactor body 11 through the reactor cover 12, and the reflux condenser includes a fractionating column L1 connected to the reactor body 11, and a vertical condenser connected to the fractionating column L1. L2, horizontal condenser L3 connected with vertical condenser L2, oil-water separator L4 connected with horizontal condenser L3, vent pipe L5 connected with oil-water separator L4, vacuum system K and vent pipe L5 Connected. The setting of the reflux condensing device can cause too much solvent in the modified system to affect the filtration efficiency in the later stage. Therefore, the internal solvent can be evaporated by heating the reactor body 11, and then processed and recycled through the condensing reflux device, and the vacuum system The function of K communication is to keep the oil-water separator L4 in a negative pressure state, so that the solvent can be collected smoothly.
工作过程:首先使无机粉体与溶剂在预混装置A中初步混合后,然后通入研磨装置B中研磨,此过程中,循环气动放料阀F处于打开状态,而进料气动放料阀I处于关闭状态,当激光粒度仪G检测到体系中无机粉体的粒度符合要求后,调整循环气动放料阀F至关闭状态,同时打开进料气动放料阀I向分散反应器C内进料,并根据进料量相应添加改性剂的添加量(即打开改性剂预储罐J的出料阀向分散反应器C内加料),根据需要调整驱动部件21的频率,使得无机粉体在分散反应器C内被较好分散的同时被改性,改性完成后根据内部溶剂的多寡进行选择是否需要通过回流冷凝装置进行回收溶剂,然后放料进入过滤装置,分离出改性后的无机粒子;Working process: Firstly, the inorganic powder and solvent are initially mixed in the premixing device A, and then passed into the grinding device B for grinding. During this process, the circulating pneumatic discharge valve F is in an open state, and the feed pneumatic discharge valve I is in the closed state. When the laser particle size analyzer G detects that the particle size of the inorganic powder in the system meets the requirements, adjust the circulating pneumatic discharge valve F to the closed state, and open the feed pneumatic discharge valve I to feed into the dispersion reactor C. According to the feed quantity, the modifier is added accordingly (that is, the discharge valve of the modifier pre-storage tank J is opened to feed the dispersion reactor C), and the frequency of the driving part 21 is adjusted as needed to make the inorganic powder The body is well dispersed in the dispersion reactor C and modified at the same time. After the modification is completed, it is determined whether the solvent needs to be recovered through the reflux condensing device according to the amount of internal solvent, and then the material is discharged into the filtering device to separate the modified Of inorganic particles;
其中,针对不同的无机粒子,例如颗粒状的,传热夹套13内的传热介质可以为热流体等等;当无机粒子为氮化硼、云母或蒙脱土等材料时,可以将传热夹套13内的传热介质设置为冷冻液与热流体交替进行以实现冻融、解冻处理,并结合高速搅拌剪切和超声分散,获得剥离的二维纳米材料,然后再进行改性操作以及其它相应后续操作,上述传热介质均可通过传热介质生产装置M产生,例如热流体可以为热水、热油等,冷冻液可以为液态氮等等。Among them, for different inorganic particles, such as granular, the heat transfer medium in the heat transfer jacket 13 can be a thermal fluid, etc.; when the inorganic particles are materials such as boron nitride, mica or montmorillonite, the transfer The heat transfer medium in the heat jacket 13 is set to alternate between freezing liquid and hot fluid to achieve freezing and thawing, combined with high-speed stirring and shearing and ultrasonic dispersion, to obtain exfoliated two-dimensional nanomaterials, and then perform modification operations As well as other corresponding subsequent operations, the above-mentioned heat transfer medium can be produced by the heat transfer medium production device M. For example, the thermal fluid can be hot water, thermal oil, etc., and the refrigerant can be liquid nitrogen, and so on.
综上,本申请通过依次连通的预混装置A、研磨装置B、分散反应器C和过滤装置D实现了无机粉体的研磨、分散以及改性一体化进行,且基本实现连续化作用,效率高;尤其是通过可拆卸连接的反应器盖体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,同时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, this application realizes the integrated grinding, dispersion and modification of inorganic powder through the pre-mixing device A, grinding device B, dispersing reactor C, and filtering device D that are connected in sequence, and basically realizes the continuous effect and efficiency High; especially 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, to realize the convenient replacement and adjustment of the entire device At the same time, it combines high-speed stirring and shearing and ultrasonic dispersion to achieve surface modification while achieving effective dispersion of inorganic nanoparticles, 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 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. 一种无机粉体改性系统,其特征在于,所述改性系统包括依次连通的预混装置、研磨装置、分散反应器和过滤装置;其中,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超声波振动棒,所述超声波振动棒伸入所述反应器本体内。An inorganic powder modification system, characterized in that the modification system includes a premixing device, a grinding device, a dispersion reactor, and a filtering device that are connected in sequence; wherein, the dispersion reactor includes a reactor cylinder and a part A stirring device arranged inside the reactor barrel, the reactor barrel including a reactor body, a reactor cover detachably connected to the reactor body and used for covering the reactor body, The stirring device partially penetrates the reactor cover and extends into the reactor body; the dispersion reactor further includes an ultrasonic vibration device, and the ultrasonic vibration device includes an ultrasonic wave arranged on the reactor cover. A generator, an ultrasonic transducer connected to the ultrasonic generator, an horn connected to the ultrasonic transducer, and an ultrasonic vibrating rod connected to the horn, the ultrasonic vibrating rod extends into the The reactor body.
  2. 根据权利要求1所述的无机粉体改性系统,其特征在于,所述超声波振动棒沿上下方向延伸;和/或,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 inorganic powder modification system according to claim 1, wherein the ultrasonic vibrating rod extends in a vertical direction; and/or the ultrasonic vibrating device has at least two and is symmetrically distributed around the stirring device .
  3. 根据权利要求1所述的无机粉体改性系统,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,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 inorganic powder modification system according to claim 1, wherein the stirring device comprises a driving part fixedly arranged on the reactor cover through a support frame, and a coupling connected to the driving part in transmission. , A stirring shaft which is connected to the coupling in transmission and passes through the reactor cover and extends into the reactor body, and a stirring blade arranged at the lower part of the stirring shaft, the stirring blade There are at least two and are sequentially arranged on the stirring shaft along the up and down direction.
  4. 根据权利要求3所述的无机粉体改性系统,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 inorganic powder modification system according to claim 3, wherein the stirring blade has a first disc stirring blade arranged at the lower end of the stirring shaft, and the first disc stirring blade is arranged on the first disc stirring blade. The second disc stirring blade above the 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.
  5. 根据权利要求4所述的无机粉体改性系统,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 inorganic powder modification system according to claim 4, 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 There is an interval between the two blades, and the lower part of the blade body protrudes downward to form an arc-shaped part corresponding to the bottom of the reactor body.
  6. 根据权利要求1所述的无机粉体改性系统,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以及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,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,所述出料管与所述过滤装置连通。The inorganic powder modification system according to claim 1, wherein the reactor barrel further comprises a heat transfer jacket coated on the reactor body, and a heat transfer jacket coated on the heat transfer jacket The heat preservation layer of the outer wall and the discharge pipe which are arranged at the bottom of the reactor body and respectively pass through the heat transfer jacket and the heat preservation layer, and the heat transfer jacket has heat exchange that respectively passes through the heat preservation layer. Fluid inlet and heat exchange fluid outlet, the heat exchange fluid inlet is located at the lower part of the heat transfer jacket, the heat exchange fluid outlet is located on the upper part of the heat transfer jacket, the discharge pipe and the filter device Connected.
  7. 根据权利要求1所述的无机粉体改性系统,其特征在于,所述改性系统还包括设置在所述预混装置与所述研磨装置之间的循环管,所述循环管上沿从与所述研磨装置连通的一端至与所述预混装置连通的另一端方向依次设置有循环气动放料阀、激光粒度仪。The inorganic powder modification system according to claim 1, wherein the modification system further comprises a circulation pipe arranged between the premixing device and the grinding device, and the upper edge of the circulation pipe is from A circulating pneumatic discharge valve and a laser particle size analyzer are sequentially arranged from one end communicating with the grinding device to the other end communicating with the premixing device.
  8. 根据权利要求7所述的无机粉体改性系统,其特征在于,所述研磨装置与所述分散反应器通过无机粉体进料管连通,所述无机粉体进料管上设置有进料气动放料阀,所述循环管与所述无机粉体进料管连通。The inorganic powder modification system according to claim 7, wherein the grinding device and the dispersion reactor are connected through an inorganic powder feed pipe, and the inorganic powder feed pipe is provided with a feed Pneumatic discharge valve, the circulation pipe is in communication with the inorganic powder feeding pipe.
  9. 根据权利要求1所述的无机粉体改性系统,其特征在于,所述改性系统还包括改性剂预储罐、与所述改性剂预储罐连通的真空系统,所述改性剂预储罐通过所述反应器盖体与所述反应器本体连通。The inorganic powder modification system according to claim 1, wherein the modification system further comprises a modifier pre-storage tank, a vacuum system connected with the modifier pre-storage tank, and the modification system The agent pre-storage tank is in communication with the reactor body through the reactor cover.
  10. 根据权利要求9所述的无机粉体改性系统,其特征在于,所述改性系统还包括通过所述反应器盖体与所述反应器本体连通的回流冷凝装置,所述回流冷凝装置包括与所述反应器本体连通的分馏柱、与所述分馏柱连通的立式冷凝器、与所述立式冷凝器连通的卧式冷凝器、与所述卧式冷凝器连通的油水分离器、与所述油水分离器连通的放空管,所述真空系统与所述放空管连通。The inorganic powder modification system according to claim 9, wherein the modification system further comprises a reflux condensing device communicating with the reactor body through the reactor cover, and the reflux condensing device comprises A fractionating column communicating with the reactor body, a vertical condenser communicating with the fractionating column, a horizontal condenser communicating with the vertical condenser, an oil-water separator communicating with the horizontal condenser, A vent pipe communicating with the oil-water separator, and the vacuum system is in communication with the vent pipe.
PCT/CN2020/121845 2019-12-06 2020-10-19 Inorganic powder modification system WO2021109729A1 (en)

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