Modified ultrafine powder as well as preparation method and preparation device thereof
The ultrafine powder is modified by EB monomer and EB resin, and the EB electron beam curtain is used to cure it to form a modified structure of polymer organic matter cutting or coating, which solves the problem of poor stability of ultrafine powder modification in the prior art, and realizes the preparation of high-performance powder.
Patent Information
- Application Number
- CN202411917558.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-24
- Publication Date
- 2025-03-28
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The existing ultrafine powder modification methods have problems such as poor stability, poor light transmission, and poor water and solvent resistance, which are difficult to meet the needs of high-performance materials.
The modified ultrafine powder is modified by EB monomer and EB resin, and the atomized particles are cured by using EB electron beam curtains to form a modified or coated modified structure of polymer organic matter cuttings.
It realizes the firm combination of polymer organic matter in ultrafine powder, improves the stability, light transmittance and water resistance of the powder, reduces the probability of agglomeration and water absorption, and is suitable for the preparation of a variety of high-performance materials.
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Figure CN119708548A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of ultrafine powder modification, and in particular to a modified ultrafine powder and a preparation method and a preparation device thereof. Background Art
[0002] Ultrafine powders have excellent properties that are difficult to match with conventional materials and have been widely used in advanced ceramics, microelectronics, aerospace, biopharmaceuticals, optical detection and other fields. Due to problems such as low stability, easy agglomeration and difficulty in dispersion, it is necessary to perform appropriate surface treatment on ultrafine powders to improve the surface characteristics of the particles and enhance their dispersion performance to meet application requirements.
[0003] Surface chemical coating modification is one of the most commonly used methods for powder surface modification. The functional groups in the organic surface modifier molecules are adsorbed or chemically reacted on the particle surface to modify the particle surface. Among them, the surface modifiers mainly include coupling agents (silanes, titanates, aluminates, zirconium aluminates, organic complexes and phosphates, etc.), surfactants (higher fatty acids and their salts, higher amine salts, non-ionic surfactants and silicone oils or silicone resins, etc.), organic oligomers and unsaturated organic acids, etc., as well as organic wax treatment.
[0004] At present, the existing ultrafine powder modification methods basically involve simple adsorption onto the surface of the micropowder, which has the disadvantages of poor stability, poor light transmittance, and poor water and solvent resistance.
[0005] In view of this, the present invention is proposed. Summary of the invention
[0006] The first object of the present invention is to provide a method for preparing a modified ultrafine powder, wherein the ultrafine powder to be modified is modified by using EB monomer and EB resin, and the EB monomer and EB resin on the ultrafine powder can be quickly solidified into high molecular organic matter, thereby forming high molecular organic matter-cutting modified powder and high molecular organic matter-coated modified powder.
[0007] The second object of the present invention is to provide a modified ultrafine powder obtained by the above preparation method.
[0008] The third object of the present invention is to provide a device for preparing the modified ultrafine powder.
[0009] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted:
[0010] The present invention provides a method for preparing a modified ultrafine powder, the preparation method comprising:
[0011] The ultrafine powder to be modified is mixed with EB resin and EB monomer and then atomized to form atomized particles of 1 to 200 μm. The atomized particles are then cured using an EB electron beam curtain to obtain modified ultrafine powder.
[0012] Furthermore, the ultrafine powder to be modified includes organic ultrafine powder and / or inorganic ultrafine powder;
[0013] Preferably, the ultrafine powder to be modified includes at least one of quartz sand, silicon powder, calcium carbonate, kaolin, talc, bentonite, barite, wollastonite, mica, diatomaceous earth, brucite, barium sulfate, dolomite, titanium dioxide, aluminum hydroxide, magnesium hydroxide, and aluminum oxide;
[0014] Preferably, the particle size of the ultrafine powder to be modified is 1 to 200 μm.
[0015] Furthermore, the EB resin is a resin capable of achieving EB curing, and the viscosity of the EB resin is 200-2500CP;
[0016] Preferably, the EB resin includes at least one of a low viscosity UV acrylic resin, a low viscosity UV epoxy acrylic resin, a low viscosity polyester type UV resin, a low viscosity UV prepolymer, and a low viscosity epoxy compound;
[0017] And / or, the EB monomer is an unsaturated monomer capable of EB curing, preferably a monofunctional, difunctional or polyfunctional unsaturated monomer.
[0018] Furthermore, the mass ratio of the ultrafine powder to be modified, the EB resin and the EB monomer is (50-97):(0-20):(3-50).
[0019] The present invention provides a modified ultrafine powder, wherein the modified ultrafine powder has a macromolecular organic matter cutting modification structure;
[0020] Alternatively, the modified ultrafine powder has a polymer organic matter-coated modified structure.
[0021] The present invention provides a device for preparing the modified ultrafine powder, which comprises: a raw material discharge bin, a flat square powder solidification pipeline and a powder collecting device;
[0022] The feed inlet of the flat square powder solidification pipeline is communicated with the discharge port of the raw material discharge bin, and the discharge port of the flat square powder solidification pipeline is communicated with the feed inlet of the powder collecting device.
[0023] The flat square powder curing pipeline is provided with a high-pressure nitrogen scatterer and an EB electron beam curtain generator;
[0024] The high-pressure nitrogen disperser is used to disperse the powder into powder mist, and the powder mist is strip-shaped powder mist in the flat square powder curing pipeline;
[0025] The electron beam curtain generated by the EB electron beam curtain generator is arranged to be perpendicular to the flow direction of the strip-shaped powder mist.
[0026] Furthermore, the raw material discharging bin is a quantitative discharging bin, and the quantitative discharging is achieved by a quantitative screw.
[0027] Furthermore, the powder collecting device includes a powder collector and a packaging machine;
[0028] Wherein: the powder collector is connected to the discharge pipe of the flat square powder curing pipe; the packaging machine is arranged at the powder outlet of the powder collector;
[0029] Preferably, the powder collector is also provided with an induced draft fan.
[0030] The present invention provides an application of the modified ultrafine powder in the preparation of coating inks, engineering plastics, rubber, films, electronic products, cosmetics, advanced ceramics, microelectronics, aerospace, biopharmaceuticals and optical detection products.
[0031] Compared with the prior art, the present invention has the following beneficial effects:
[0032] The present invention provides a method for preparing a modified ultrafine powder. The method firstly mixes the ultrafine powder to be modified, EB resin and EB monomer, and then atomizes the mixture to form atomized particles of 1 to 200 μm. The atomized particles are then cured by an EB electron beam curtain to obtain the modified ultrafine powder. The above-mentioned preparation method modifies the ultrafine powder to be modified by EB monomer and EB resin. After the 1 to 200 μm atomized particles formed by the ultrafine powder, EB resin and EB monomer are cured by the EB electron beam curtain, the EB monomer and EB resin on the powder can be quickly cured into a high molecular organic matter in 0.0005-0.1 seconds. The high molecular organic matter is firmly combined with the ultrafine powder, thereby forming a high molecular organic matter cutting modified powder and a high molecular organic matter coated modified powder.
[0033] The modified ultrafine powder provided by the present invention is determined by the above-mentioned modification method, and the modified ultrafine powder has a macromolecular organic matter cutting modification structure or a macromolecular organic matter coating modification structure.
[0034] The present invention provides a preparation device for modified ultrafine powders, the preparation device includes a raw material discharge bin, a flat square powder curing pipeline and a powder collecting device; the feed port of the flat square powder curing pipeline is connected to the discharge port of the raw material discharge bin, and the discharge port of the flat square powder curing pipeline is connected to the feed port of the powder collecting device; the flat square powder curing pipeline is provided with a high-pressure nitrogen scatterer and an EB electron beam curtain generator, wherein: the high-pressure nitrogen scatterer is used to scatter the powder to form a strip-shaped powder mist, the EB electron beam curtain generator is below the high-pressure nitrogen scatterer and at the lower end of the flat square powder curing pipeline, and the EB electron beam curtain generated by the generator is used to solidify the ultrafine powder to be modified in the strip-shaped powder mist. The present invention realizes ultrafine powders with a polymer organic cutting / coating modified structure through the coordinated cooperation of the various components in the above-mentioned modified ultrafine powder preparation device, and the above-mentioned preparation method has the advantages of simple preparation process flow, high efficiency, and suitability for factory production.
[0035] The modified ultrafine powder provided by the present invention can be widely used in the preparation process of coating inks, engineering plastics, rubber, films, electronic products, cosmetics, advanced ceramics, microelectronics, aerospace, biopharmaceuticals and optical detection products. BRIEF DESCRIPTION OF THE DRAWINGS
[0036] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0037] Figure 1 A schematic diagram of the structure of the ultrafine powder EB electron beam curing modification device provided in Example 1 of the present invention;
[0038] Figure 2 A top view of the EB electron beam curing pipeline provided in Example 1 of the present invention.
[0039] Icons: 1-Raw material discharge bin; 2-Flat square powder curing pipeline; 21-High pressure nitrogen disperser; 22-EB electron beam curtain generator; 3-Powder collection device; 31-Powder collector; 32-Packaging machine; 33-Draught fan. DETAILED DESCRIPTION
[0040] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0041] According to one aspect of the present invention, a method for preparing a modified ultrafine powder comprises:
[0042] The ultrafine powder to be modified is mixed with EB resin and EB monomer and then atomized to form atomized particles of 1 to 200 μm. The atomized particles are then cured using an EB electron beam curtain to obtain modified ultrafine powder.
[0043] The present invention provides a method for preparing a modified ultrafine powder. The method firstly mixes the ultrafine powder to be modified with EB resin and EB monomer, and then atomizes the mixture to form atomized particles of 1 to 200 μm. The atomized particles are then cured by an EB electron beam curtain to obtain the modified ultrafine powder. The above-mentioned preparation method modifies the ultrafine powder to be modified by EB monomer and EB resin. The atomized particles of 1 to 200 μm formed by the ultrafine powder, EB resin and EB monomer are cured by an EB electron beam curtain. The EB monomer and EB resin on the powder can be quickly cured into a high molecular organic matter in 0.0005-0.1 seconds. The high molecular organic matter is firmly combined with the ultrafine powder, thereby forming a high molecular organic matter cutting modified powder and a high molecular organic matter coated modified powder.
[0044] The modified ultrafine powder has the following advantages:
[0045] (1) After the ultrafine powder is modified into high molecular organic cutting modified powder and high molecular organic coated modified powder, the modified ultrafine powder reacts completely with the unsaturated bonds of EB monomer and EB resin, and the formed high molecular organic matter is firmly combined with the powder. The formed powder is a composite material with low water and oil absorption, no interface with organic resins, and can be easily dispersed into resins, plastics, rubber and other products, and the powder has the advantage of not being easy to agglomerate.
[0046] (2) After modification, the hardness of silica, alumina and other ultrafine powders increases, and the scratch resistance is good;
[0047] (3) The modified ultrafine powder can be stably dispersed into coatings, inks, resins, rubber and plastics as a pigment without the need for a dispersant, and has excellent color development properties;
[0048] (4) The present application uses EB electron beam to solidify and modify the ultrafine powder, which can maintain the original particle size distribution and morphology of the ultrafine powder.
[0049] (5) The raw materials for modifying the ultrafine powder of the present invention are easily available, and the production energy consumption is low. The EB curing method has no VOC emissions and no wastewater generation. It is environmentally friendly and economical, and can meet the current industrial demand for high-performance materials.
[0050] In a preferred embodiment of the present invention, the ultrafine powder to be modified includes organic ultrafine powder and / or inorganic ultrafine powder;
[0051] Preferably, the ultrafine powder to be modified includes at least one of quartz sand, silicon powder, calcium carbonate, kaolin, talc, bentonite, barite, wollastonite, mica, diatomaceous earth, brucite, barium sulfate, dolomite, titanium dioxide, aluminum hydroxide, magnesium hydroxide, and aluminum oxide;
[0052] In a preferred embodiment of the present invention, the particle size of the ultrafine powder to be modified is 1 to 200 μm.
[0053] In a preferred embodiment of the present invention, the EB resin is a resin capable of EB curing;
[0054] In the above preferred embodiment, the EB resin includes at least one of a low viscosity UV acrylic resin, a low viscosity UV epoxy acrylic resin, a low viscosity polyester type UV resin, a low viscosity UV prepolymer, and a low viscosity epoxy compound resin;
[0055] In the above preferred embodiment, the EB monomer is an unsaturated monomer capable of EB curing, preferably a monofunctional, difunctional or polyfunctional unsaturated monomer.
[0056] It should be noted that the present application uses EB resin and EB monomer to modify the ultrafine powder. The EB monomer and low-viscosity EB resin can be adsorbed into the interior of the powder due to their low viscosity and small molecular weight. At the same time, the outside of the powder is also coated with EB monomer and EB resin. The EB monomer and EB resin on the powder are then cured by an EB electron beam curtain curing device to become high-molecular organic matter. The high-molecular organic matter and the ultrafine powder are firmly combined to become high-molecular organic matter-cutting modified powder and high-molecular organic matter-coated modified powder.
[0057] Preferably, the EB monomer comprises methyl methacrylate (MMA) ,n-Butyl methacrylate (NBMA), isobutyl methacrylate (IBMA), 2-phenoxyethyl acrylate (PHEA), methyl / lauryl acrylate (LMA / LA), ethoxyethoxyethyl acrylate (EOEOEA), methoxy polyethylene glycol 1000 acrylate (MPEG1000DA), methyl / tetrahydrofurfuryl acrylate (THFMA / THFA), caprolactone methacrylate (FM), 2-hydroxyethyl methacrylate phosphate (PM-2), N-(isobutyloxy) methacrylamide (IBMA), methyl / isobornyl acrylate (IBOMA / IBOA), hydroxyethyl modified acrylamide (HEAA), methacrylic acid Acid phosphate (PM-3), 4-hydroxybutyl acrylate (4HBA), methyl / hydroxyethyl acrylate (HEMA / HEA), methyl / hydroxypropyl acrylate (HPMA / HPA), ethylene glycol dimethacrylate (EGDMA), diethylaminoethyl methacrylate, unsaturated siloxane, vinyl silane, tripropylene glycol diacrylate TPGDA, dipentaerythritol hexaacrylate DPHA, hexanediol diacrylate PDDA, neopentyl glycol diacrylate NPGDA, pentaerythritol triacrylate PETA, trimethylolpropane triacrylate TMPTA, ethoxylated trimethylolpropane triacrylate EOTMPTA and other monofunctional, difunctional, or multifunctional monomers.
[0058] In a preferred embodiment of the present invention, the mass ratio of the ultrafine powder to be modified, the EB resin and the EB monomer is (50-97):(0-20):(3-50).
[0059] According to one aspect of the present invention, a modified ultrafine powder has a macromolecular organic matter cutting modification structure;
[0060] Alternatively, the modified ultrafine powder has a polymer organic matter-coated modified structure.
[0061] The modified ultrafine powder provided by the present invention is determined by the above-mentioned modification method, and the modified ultrafine powder has a macromolecular organic matter cutting modification structure or a macromolecular organic matter coating modification structure.
[0062] According to one aspect of the present invention, the above-mentioned modified ultrafine powder preparation device comprises: a raw material discharge bin 1, a flat square powder solidification pipeline 2 and a powder collecting device 3;
[0063] The feed inlet of the flat square powder solidification pipeline 2 is communicated with the discharge port of the raw material discharge bin 1 , and the discharge port of the flat square powder solidification pipeline 2 is communicated with the feed inlet of the powder collecting device 3 .
[0064] The flat square powder solidification pipeline 2 is provided with a high-pressure nitrogen scatterer 21 and an EB electron beam curtain generator 22;
[0065] The high-pressure nitrogen disperser 21 is used to disperse the powder into powder mist, and the powder mist is strip-shaped powder mist in the flat square powder curing pipeline 2; the electron beam curtain generated by the EB electron beam curtain generator 22 is arranged to be perpendicular to the flow direction of the strip-shaped powder mist.
[0066] The present invention provides a preparation device for modified ultrafine powder, which comprises a raw material discharge bin 1, a flat square powder curing pipeline 2 and a powder collecting device 3; the feed inlet of the flat square powder curing pipeline 2 is connected with the discharge outlet of the raw material discharge bin 1, and the discharge outlet of the flat square powder curing pipeline 2 is connected with the feed inlet of the powder collecting device 3; the flat square powder curing pipeline 2 is provided with a high-pressure nitrogen disperser 21 and an EB electron beam curtain generator 22, wherein: the high-pressure nitrogen disperser 21 is used to disperse the powder to form a strip-shaped powder mist, and the EB electron beam curtain generator 22 is below the high-pressure nitrogen disperser 21 and at the lower end of the flat square powder curing pipeline 2, and the EB electron beam curtain generated by it is used to solidify the ultrafine powder to be modified in the strip-shaped powder mist. The present invention realizes ultrafine powder with a macromolecular organic matter cutting / coating modified structure through the coordinated cooperation of various components in the modified ultrafine powder preparation device. The preparation method has the advantages of simple preparation process flow, high efficiency and suitability for factory production.
[0067] The working process of the modified ultrafine powder preparation device of this application is as follows:
[0068] After the ultrafine powder is adsorbed and coated with EB monomer and EB resin, it is placed in the raw material discharge bin 1, and quantitatively discharged through its own screw into the flat square pipe. The powder is dispersed into strip-shaped powder mist by a high-pressure nitrogen dispersing device. When the powder mist passes through the electron beam curtain generated by the EB electron beam curing device, the EB monomer and EB resin on the powder are quickly solidified into high-molecular organic matter. The high-molecular organic matter and the ultrafine powder are firmly combined to become high-molecular organic matter cutting modified powder and high-molecular organic matter coated modified powder.
[0069] It should be noted that the high-pressure nitrogen disperser 21 is located at the uppermost end of the flat square powder solidification pipe 2 below the outlet of the raw material discharge bin 1, and is used to disperse the powder to form strip-shaped powder mist. It can also reduce the oxygen in the space of the flat square powder solidification pipe 2. Under the protection of nitrogen, the EB monomer and EB resin on the strip-shaped powder mist are easily and completely solidified into saturated high-molecular organic matter. The high-molecular organic matter and the ultrafine powder are firmly combined to become high-molecular organic matter cutting modified powder and high-molecular organic matter coated modified powder.
[0070] It should be noted that the EB electron beam curtain generator 22 is located below the high-pressure nitrogen disperser 21 and at the lower end of the flat square powder curing pipe 2, and it generates an EB electron beam curtain to cure the EB monomer and EB resin on the powder; in this application, through the setting of the flat square powder curing pipe 2, after the powder is irradiated by the electron beam curtain, the EB monomer and EB resin inside and outside can be evenly cured.
[0071] In a preferred embodiment of the present invention, the raw material discharging bin 1 is a quantitative discharging bin, and the quantitative discharging is achieved by a quantitative screw.
[0072] As a preferred embodiment, the raw material discharge bin 1 is a bin with a screw that can quantitatively discharge materials. The raw material discharge bin 1 stores ultrafine powders that absorb and coat EB monomers and EB resins (ultrafine powders are fully mixed with EB monomers and EB resins. EB monomers and low-viscosity EB resins have low viscosity and small molecular weight and can be absorbed by the powders. The outside is also coated with EB monomers and EB resins). The screw of the bin itself can quantitatively discharge the powders to be cured and output them for curing.
[0073] In a preferred embodiment of the present invention, the powder collecting device 3 includes a powder collector 31 and a packaging machine 32; wherein: the powder collector 31 is connected to the discharge port pipe of the flat square powder curing pipe 2; the packaging machine 32 is arranged at the powder outlet of the powder collector 31, and is used to package the ultrafine powder collected by the collector and modified by EB electron beam curing.
[0074] In a preferred embodiment of the present invention, the powder collector 31 is further provided with an induced draft fan 33 , and the induced draft fan 33 connected to the powder collector 31 provides gravitational force to quickly collect the polymer organic matter cutting modified powder and the polymer organic matter coated modified powder into the powder collector 31 .
[0075] According to one aspect of the present invention, the modified ultrafine powder is used in the preparation of coatings and inks, engineering plastics, rubber, films, electronic products, cosmetics, advanced ceramics, microelectronics, aerospace, biopharmaceuticals and optical detection products.
[0076] The modified ultrafine powder provided by the present invention can be widely used in the preparation process of coating inks, engineering plastics, rubber, films, electronic products, cosmetics, advanced ceramics, microelectronics, aerospace, biopharmaceuticals and optical detection products.
[0077] The technical solution of the present invention will be further described below in conjunction with embodiments.
[0078] Example 1
[0079] Figure 1This is a schematic diagram of the structure of the ultrafine powder EB electron beam curing modification device provided in this embodiment.
[0080] Figure 2 A top view of the EB electron beam curing pipeline provided in this embodiment.
[0081] See also Figure 1 , an EB electron beam curing and modifying device for ultrafine powder, comprising: a raw material discharge bin 1, a flat square powder curing pipeline 2 and a powder collecting device 3;
[0082] The feed inlet of the flat square powder solidification pipeline 2 is communicated with the discharge port of the raw material discharge bin 1 , and the discharge port of the flat square powder solidification pipeline 2 is communicated with the feed inlet of the powder collecting device 3 .
[0083] The flat square powder solidification pipeline 2 is provided with a high-pressure nitrogen scatterer 21 and an EB electron beam curtain generator 22;
[0084] The high-pressure nitrogen disperser 21 is used to disperse the powder into powder mist, and the powder mist is strip-shaped powder mist in the flat square powder curing pipeline 2; the electron beam curtain generated by the EB electron beam curtain generator 22 is arranged to be perpendicular to the flow direction of the strip-shaped powder mist.
[0085] The modified ultrafine powder preparation device provided by the present invention comprises a raw material discharge bin 1, a flat square powder solidification pipeline 2 and a powder collecting device 3. The present invention realizes ultrafine powder with a macromolecular organic matter cutting / coating modified structure through the coordinated cooperation of various components in the modified ultrafine powder preparation device. The preparation method has the advantages of simple preparation process flow, high efficiency and suitability for factory production.
[0086] See also Figure 1 In a preferred embodiment of the present invention, the high-pressure nitrogen disperser 21 is located at the uppermost end of the flat square powder solidification pipe 2 below the outlet of the raw material discharge bin 1, and is used to disperse the powder to form strip-shaped powder mist, and can also reduce the oxygen in the space of the flat square powder solidification pipe 2. Under the protection of nitrogen, the EB monomer and EB resin on the strip-shaped powder mist are easily and completely solidified into saturated high-molecular organic matter, and the high-molecular organic matter and the ultrafine powder are firmly combined to become high-molecular organic matter cutting modified powder and high-molecular organic matter coated modified powder.
[0087] See also Figure 1 , Figure 2In a preferred embodiment of the present invention, the EB electron beam curtain generator 22 is located below the high-pressure nitrogen scatterer 21 and at the lower end of the flat square powder curing pipe 2, and generates an EB electron beam curtain to cure the EB monomer and EB resin on the powder. In the present application, through the setting of the flat square powder curing pipe 2, after the powder is irradiated by the electron beam curtain, the EB monomer and EB resin inside and outside the powder can be evenly cured.
[0088] Continue to see Figure 1 In a preferred embodiment of the present invention, the raw material discharging bin 1 is a quantitative discharging bin, and the quantitative discharging is achieved by a quantitative screw.
[0089] Preferably, the raw material discharge bin 1 is a bin with a screw that can quantitatively discharge materials. The raw material discharge bin 1 stores ultrafine powders that absorb and coat EB monomers and EB resins (ultrafine powders are fully mixed with EB monomers and EB resins. EB monomers and low-viscosity EB resins have low viscosity and small molecular weight and can be absorbed by the powders. The outside is also coated with EB monomers and EB resins). The screw of the bin itself can quantitatively discharge the powders to be cured and output them for curing.
[0090] See also Figure 1 In a preferred embodiment of the present invention, the powder collecting device 3 includes a powder collector 31 and a packaging machine 32; wherein: the powder collector 31 is connected to the discharge port of the flat square powder curing pipe 2; the packaging machine 32 is arranged at the powder outlet of the powder collector 31, and is used to package the ultrafine powder collected by the collector and modified by EB electron beam curing.
[0091] In a preferred mode of this embodiment, the powder collector 31 is further provided with an induced draft fan 33 , and the induced draft fan 33 connected to the powder collector 31 provides gravitational force to quickly collect the polymer organic matter cutting modified powder and the polymer organic matter coated modified powder into the powder collector 31 .
[0092] Preferably, the ultrafine powder modification method according to this embodiment comprises the following steps:
[0093] After the EB monomer and EB resin are fully and evenly mixed with the ultrafine powder, the ultrafine powder will adsorb (or coat) the EB monomer and EB resin, and the above ultrafine powder is stored in a silo with a screw that can quantitatively discharge the material, the induced draft fan 33 and the EB electron beam device are turned on, the high-pressure nitrogen dispersing device is turned on, and then the screw of the raw material silo is turned on; the powder in the silo is pushed into the flat square pipe, and the powder is quickly dispersed into a strip-shaped powder mist when passing through the high-pressure nitrogen dispersing device. When the powder mist passes through the EB electron beam curtain emitted by the EB electron beam device, the EB monomer and EB resin on the powder are quickly solidified into saturated macromolecular organic matter and firmly combined with the powder to become organic matter cutting modified powder and high-molecular organic matter coated modified powder, thereby achieving the modification purpose. The ultrafine powder is then collected by the collection box under the gravitational force of the induced draft fan 33, and packaged by the packaging machine 32 to obtain an EB electron beam cured and modified ultrafine powder finished product.
[0094] Example 2
[0095] The difference between this embodiment and embodiment 1 is that the pipeline in the EB electron beam curtain area of the EB electron beam curing pipeline line in this embodiment is disconnected at the top and bottom, thin at the top and thick at the bottom, and the powder is modified through the EB electron beam curtain by inertia. Under the suction force of the induced draft fan 33, the modified powder is quickly sucked into the powder collection box by the thick pipeline, and the remaining components and their connections are the same as in embodiment 1, so as to obtain an EB electron beam curing and modification device for ultrafine powders.
[0096] Compared with Example 1, the device of this embodiment is to be used for the effect and protection of the electron beam on the outside world; it should be noted that in the EB electron beam curtain area, the pipeline is disconnected and also within the protection scope of the present invention. Example 3 (Application of the modified composite matting powder of the present invention)
[0097] A modification method using the EB electron beam curing modification device of Example 1 comprises the following steps:
[0098] (1) After uniformly mixing "UV polyester acrylic resin: trimethylolpropane triacrylate TMPTA: n-butyl methacrylate NBMA = 2:4:4", fully mix with 5 micron white carbon black ultrafine powder, put it into the raw material bin, turn on the induced draft fan 33 and the EB electron beam equipment, turn on the high-pressure nitrogen scattering device, and then turn on the screw on the raw material bin to evenly feed the flat square pipe;
[0099] The mass ratio of the ultrafine white carbon black powder to the UV polyester acrylic resin and the EB monomer (trimethylolpropane triacrylate and n-butyl methacrylate) is 50:2:8.
[0100] The UV polyester acrylic resin is 6361-100 of Changxing Resin, and has a viscosity of 150-250CP.
[0101] (2) The powder enters the flat square tube and is quickly dispersed into strip-shaped powder mist by the nitrogen dispersion device in the pipeline. The strip-shaped powder mist enters the EB electron beam curtain area. The EB monomer and EB resin on the powder are quickly solidified into large macromolecular organic matter and firmly combined with the powder in 0.005-0.1 seconds, completing the modification into macromolecular organic matter-implanted modified silica and macromolecular organic matter-coated modified silica, which is a new composite matting powder;
[0102] (3) The powder cured by EB electron beam is collected by a collector, and then packaged by a packaging machine 32 to obtain ultrafine powder modified by EB electron beam curing.
[0103] In this embodiment, the EB resin and EB monomer have low viscosity and small molecular weight, and can be fully mixed with white carbon black powder to achieve adsorption and coating. The white carbon black adsorbed and coated with EB resin and EB monomer is put into the silo, and pushed into the flat square pipeline through the screw of the silo. The nitrogen dispersing device in the pipeline quickly disperses it into strip-shaped white carbon black powder mist. When the strip-shaped white carbon black powder mist passes through the EB electron beam curtain area of the pipeline, the EB resin and EB monomer on the white carbon black are quickly solidified into large macromolecular organic matter under the action of the EB electron beam curtain, and the large macromolecular organic matter and the powder are hardened into one; the powder After the edges and corners of the surface are coated with high-hardness polymer organic matter, the feel is significantly improved and the scratch resistance is improved; EB resin and EB monomer have a small molecular weight and can be adsorbed into the pores of silica powder to achieve a filling effect. After being cured by EB electron beam curtain, the toughness of the powder can be enhanced and the permeability of the powder can be increased, and the powder has high permeability; after adsorption and coating, the water and oil absorption of the powder is reduced, the probability of powder agglomeration is reduced, and it is not easy to sink to the bottom. The dispersion of the powder is also significantly improved, making it more widely used in coatings, inks, plastics, rubber and other fields.
[0104] Performance comparison:
[0105] 1. The matting powder produced by this process is prepared into a paint film for comparative application:
[0106]
[0107]
[0108] Note: "Parts" in the above table are parts by mass; the resin is acrylic resin GNU2450 (Guangzhou Jujia New Materials); the mixed solvent is butyl acetate / xylene / PMA=5 / 3 / 2; the ratio of the auxiliary agent including defoamer and leveling agent is 3:1, wherein: the leveling agent is 10% BYK333 (BYK Chemical) and the defoamer is BYK141 (BYK Chemical)
[0109] 2. Performance comparison results:
[0110] Gloss: The gloss of the above test group 1 and control groups 1 and 2 was less than 10;
[0111] Scrape film transparency: The transparency of the scraped film of the matting powder (Jujia) prepared in the test group 1 in this embodiment is visually superior to that of the competitive control group 2 and the unmodified powder control group 1;
[0112] Anti-scratch: The modified powder of Jujia in test group 1 was scratch-resistant without leaving any marks, while the nails of control group left white marks, and the nails of control group 2, the competitor's product left white marks;
[0113] RCA test: In this embodiment, the matting powder (Jujia) prepared in test group 1 has an RCA resistance of 45 cycles, the control group 1 has 7 cycles, and the control group 2 competitive product has an RCA resistance of 8 cycles;
[0114] Feel: The matting powder (Jujia) prepared in the test group 1 in this embodiment has a feel like baby skin, the control group 1 has a rough and poor feel, and the control group 2 has a rough and poor feel;
[0115] Resistance to solvent wiping (alcohol): In this embodiment, the paint film prepared by test group 1 was scratch-free after 80 times; the paint film of the control group was damaged after 13 times, and the paint film of the competitor of control group 2 was damaged after 20 times;
[0116] Storage for 60 days: The matting powder (Jujia) prepared in Example 1 had no hard sedimentation phenomenon and recovered to the original state after stirring; the control groups 1 and 2 agglomerated and had hard sedimentation.
[0117] Example 4 (Application of modified carbon black of the present invention)
[0118] A modification method using the EB electron beam curing modification device of Example 1 comprises the following steps:
[0119] (1) Methyl methacrylate (MMA): n-butyl methacrylate (NBMA): hydroxypropyl acrylate (HPA): diethylaminoethyl methacrylate in a ratio of 7:1:1:1 are mixed evenly, and then mixed evenly with carbon black powder with a D50 of 10 microns and placed in a raw material bin, and the induced draft fan 33 and the EB electron beam device are turned on, the nitrogen scattering device is turned on, and the screw on the raw material bin is turned on to evenly feed the material into the flat square pipe;
[0120] The mass ratio of the carbon black ultrafine powder to the EB monomer (methyl methacrylate, n-butyl methacrylate, hydroxypropyl acrylate and diethylaminoethyl methacrylate) is 60:10.
[0121] (2) The carbon black powder enters the flat square tube and is quickly dispersed into strip-shaped powder mist by the nitrogen dispersion device in the pipeline. When the strip-shaped powder mist enters the EB electron beam curtain area, the monomer on the powder is quickly solidified into a large macromolecular organic substance and firmly combined with the carbon black in 0.005-0.1 seconds, completing the modification into macromolecular organic intercalation modified carbon black and macromolecular organic coating modified carbon black;
[0122] (3) The modified carbon black powder after EB electron beam curing is collected by a collector, and then packaged by a packaging machine 32 to obtain modified carbon black modified by EB electron beam curing.
[0123] Performance comparison:
[0124] 1. Application comparison of carbon black powder produced by this process:
[0125]
[0126]
[0127] Note: "Parts" in the above table refer to parts by mass; the resin is acrylic resin GNU2450 (Guangzhou Jujia New Materials); the mixed solvent is butyl acetate / xylene / PMA=5 / 3 / 2; the auxiliary agent is a dispersant, and the dispersant is BYK163 (BYK Chemical).
[0128] 2. Performance comparison results:
[0129] Grinding efficiency: In this embodiment, the modified carbon black of test group 2 needs to be ground twice to reach a fineness of 5 microns, while control group 3 needs 4 times; the competitive product of control group 4 needs 3 times. To achieve the same fineness, the grinding efficiency of the modified powder of Jujia is much higher.
[0130] Color paste viscosity: In this embodiment, the viscosity of the modified carbon black in test group 2 (Polyjia modified carbon black) is 4000CP, which is extremely low; while the viscosity of the control group 3 is a paste; the competitor of the control group 4 (Mitsubishi MA100) is 15000CP, and the Polyjia modified powder wins completely.
[0131] Hue: In this embodiment, the modified carbon black in test group 2 (Polyjia modified carbon black) is bluish black, while the unmodified powder in control group 3 is yellowish gray black, has no fluidity, and has no luster; the competitive product in control group 4 is grayish black and slightly dull. The quality is greatly improved after the Polyjia process modification.
[0132] Storage (10 days of hot and cold cycles): In this embodiment, the modified carbon black of test group 2 (Polyjia modified carbon black) did not become coarse, while the unmodified carbon black of control group 3 became coarse after 3 days; the competitive product of control group 4 began to become coarse after 10 days.
[0133] In summary, the modified carbon black of this application exhibits excellent performance after a series of rigorous tests.
[0134] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.
Claims
1. A method for preparing modified ultrafine powder, characterized in that: The preparation method comprises: The ultrafine powder to be modified is mixed with EB resin and EB monomer and then atomized to form atomized particles of 1 to 200 μm. The atomized particles are then cured using an EB electron beam curtain to obtain modified ultrafine powder.
2. The method for preparing modified ultrafine powder according to claim 1, characterized in that: The ultrafine powder to be modified includes organic ultrafine powder and / or inorganic ultrafine powder; Preferably, the ultrafine powder to be modified includes at least one of quartz sand, silicon powder, calcium carbonate, kaolin, talc, bentonite, barite, wollastonite, mica, diatomaceous earth, brucite, barium sulfate, dolomite, titanium dioxide, aluminum hydroxide, magnesium hydroxide, and aluminum oxide; Preferably, the particle size of the ultrafine powder to be modified is 1 to 200 μm.
3. The method for preparing modified ultrafine powder according to claim 1, characterized in that: The EB resin is a resin that can achieve EB curing; Preferably, the EB resin is an EB resin with a viscosity between 200-2500CP; More preferably, the EB resin includes at least one of a low viscosity UV acrylic resin, a low viscosity UV epoxy acrylic resin, a low viscosity polyester type UV resin, a low viscosity UV prepolymer resin, and a low viscosity epoxy compound; And / or, the EB monomer is an unsaturated monomer capable of EB curing, preferably a monofunctional, difunctional or polyfunctional unsaturated monomer.
4. The method for preparing modified ultrafine powder according to claim 1, characterized in that: The mass ratio of the ultrafine powder to be modified, the EB resin and the EB monomer is (50-97):(0-20):(3-50).
5. A modified ultrafine powder, characterized in that: The modified ultrafine powder has a macromolecular organic matter interplantation modification structure; or, the modified ultrafine powder has a macromolecular organic matter coating modification structure.
6. The modified ultrafine powder preparation device according to claim 5, characterized in that: The preparation device comprises: a raw material discharge bin (1), a flat square powder solidification pipeline (2) and a powder collecting device (3); The feed inlet of the flat square powder solidification pipeline (2) is connected to the discharge port of the raw material discharge bin (1), and the discharge port of the flat square powder solidification pipeline (2) is connected to the feed inlet of the powder collecting device (3); The flat square powder solidification pipeline (2) is provided with a high-pressure nitrogen scatterer (21) and an EB electron beam curtain generator (22); The high-pressure nitrogen disperser (21) is used to disperse the powder into powder mist, and the powder mist is strip-shaped powder mist in the flat square powder solidification pipeline (2); The electron beam curtain generated by the EB electron beam curtain generator (22) is arranged to be perpendicular and cross-arranged with the flow direction of the strip-shaped powder mist.
7. The device for preparing modified ultrafine powder according to claim 6, characterized in that: The raw material discharge bin (1) is a quantitative discharge bin, and the quantitative discharge is achieved by a quantitative screw.
8. The device for preparing modified ultrafine powder according to claim 6, characterized in that: The powder collecting device comprises a powder collector (31) and a packaging machine (32); wherein: the powder collector (31) is connected to the discharge pipe of the flat square powder solidification pipe (2); and the packaging machine (32) is arranged at the powder outlet of the powder collector (31); Preferably, the powder collector (31) is also provided with an induced draft fan (33).
9. Use of the modified ultrafine powder according to claim 5 in the preparation of coatings and inks, engineering plastics, rubber, films, electronic products, cosmetics, advanced ceramics, microelectronics, aerospace, biopharmaceuticals and optical detection products.
Citation Information
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