WO2021109729A1 - Système de modification de poudre inorganique - Google Patents

Système de modification de poudre inorganique 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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English (en)
Chinese (zh)
Inventor
吴斌
景录如
张春琪
崔艺华
马俊锋
徐晓风
张超
Original Assignee
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/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C21/00—Disintegrating 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention concerne un système de modification de poudre inorganique, comprenant un dispositif de prémélange (A), un dispositif de broyage (B), un réacteur de dispersion (C) et un dispositif de filtration (D) qui sont mis en communication en séquence. Le réacteur de dispersion (C) comprend un cylindre de réacteur (1), un dispositif d'agitation et un dispositif de vibration ultrasonore, le cylindre de réacteur (1) comprend un corps de réacteur (11) et un couvercle de réacteur (12), et le dispositif d'agitation pénètre partiellement à travers le couvercle de réacteur (12) et s'étend dans le corps de réacteur (11); le dispositif de vibration ultrasonore comprend un générateur d'ultrasons (31) disposé sur le couvercle de réacteur (12), un transducteur ultrasonore connecté au générateur d'ultrasons (31), un émetteur connecté au transducteur ultrasonore, et une tige de vibration ultrasonore (32) connectée à l'émetteur, et la tige de vibration ultrasonore (32) s'étend dans le corps de réacteur (11).
PCT/CN2020/121845 2019-12-06 2020-10-19 Système de modification de poudre inorganique WO2021109729A1 (fr)

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CN201922181197.4U CN211302832U (zh) 2019-12-06 2019-12-06 一种无机粉体改性系统
CN201922181197.4 2019-12-06

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CN114307791A (zh) * 2021-12-31 2022-04-12 无锡东恒新能源科技有限公司 一种碳纳米管的分散系统
CN114789077A (zh) * 2022-05-07 2022-07-26 常州励岸宝机械设备科技有限公司 一种超声波场列管式冷却出料装置
CN114950241A (zh) * 2022-06-08 2022-08-30 包头市开元数码有限公司 一种智能化的稀土纳米级湿磨设备及其加工工艺
CN116943840A (zh) * 2023-08-07 2023-10-27 广州绿徽新材料研究院有限公司 一种压变空化高速三涡流-微波复合超纳研磨植物纤维粉的装置

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CN114307791A (zh) * 2021-12-31 2022-04-12 无锡东恒新能源科技有限公司 一种碳纳米管的分散系统
CN114789077A (zh) * 2022-05-07 2022-07-26 常州励岸宝机械设备科技有限公司 一种超声波场列管式冷却出料装置
CN114789077B (zh) * 2022-05-07 2023-09-01 常州励岸宝机械设备科技有限公司 一种超声波场列管式冷却出料装置
CN114950241A (zh) * 2022-06-08 2022-08-30 包头市开元数码有限公司 一种智能化的稀土纳米级湿磨设备及其加工工艺
CN116943840A (zh) * 2023-08-07 2023-10-27 广州绿徽新材料研究院有限公司 一种压变空化高速三涡流-微波复合超纳研磨植物纤维粉的装置
CN116943840B (zh) * 2023-08-07 2024-04-09 广州绿徽新材料研究院有限公司 一种压变空化高速三涡流-微波复合超纳研磨植物纤维粉的装置

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