WO2021258721A1 - Pearlescent pigment for powder coating, preparation method therefor, and reaction equipment therefor - Google Patents

Pearlescent pigment for powder coating, preparation method therefor, and reaction equipment therefor Download PDF

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Publication number
WO2021258721A1
WO2021258721A1 PCT/CN2021/070372 CN2021070372W WO2021258721A1 WO 2021258721 A1 WO2021258721 A1 WO 2021258721A1 CN 2021070372 W CN2021070372 W CN 2021070372W WO 2021258721 A1 WO2021258721 A1 WO 2021258721A1
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Prior art keywords
pearlescent pigment
film layer
polymer film
auxiliary agent
pearlescent
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PCT/CN2021/070372
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French (fr)
Chinese (zh)
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苏尔田
谢思维
林正交
林敏立
杨静
黎伍建
黄云燕
余慧忠
龙宪君
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广西七色珠光材料股份有限公司
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Publication of WO2021258721A1 publication Critical patent/WO2021258721A1/en

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • 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
    • B01J19/0053—Details of the reactor
    • 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
    • B01J19/0053—Details of the reactor
    • B01J19/006—Baffles
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10—Treatment with macromolecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/03—Powdery paints
    • C09D5/033—Powdery paints characterised by the additives

Definitions

  • the invention relates to a pearlescent pigment, more specifically, the invention relates to a pearlescent pigment for powder coating, a preparation method and a reaction device thereof.
  • Powder coating is a solid powdery synthetic resin coating formed by solid resin, pigments, fillers, additives, etc. Unlike ordinary solvent-based coatings and water-based coatings, the dispersion medium of powder coatings is not solvent and water, but air.
  • the powder coating is non-toxic and fully meets the requirements of the national environmental protection law; the utilization rate of raw materials is high, and the highest utilization rate is as high as 99%; it is easy to realize automatic operation, high production efficiency, and can reduce costs; the impact strength and toughness of the coating are both Good, it has excellent chemical resistance and electrical insulation; it is safe and convenient for storage and transportation.
  • Powder spraying uses the principle of high-voltage electrostatic corona electric field.
  • a high-voltage negative electrode is connected to the metal diversion mark of the spray gun head, and the sprayed workpiece is grounded to form a positive electrode, so that a strong electrostatic electric field is formed between the spray gun and the workpiece.
  • the compressed air used as the carrier gas sends the powder paint from the powder supply tank to the guide rod of the spray gun through the powder tube, the corona discharge generated by the guide rod connected to the high voltage negative electrode generates dense negative charges near it. , So that the powder is negatively charged and enters the electrostatic field with high electric field strength.
  • the powder evenly flies to the surface of the grounded workpiece to form a uniform thickness of powder layer, and then heat and solidify into Durable coating film.
  • the pearlescent pigment is coated on the surface of the substrate with one or several kinds of metal oxides to form a layered structure, which is a kind of pigment with pearlescent effect formed by the interference of light.
  • the thickness of the metal oxide coated on the surface of the substrate can be changed to produce different light interference effects to obtain pearlescent pigments with different colors and pearlescent effects.
  • problems such as low powder loading rate, easy to block the gun, and uneven dispersion on the surface of the spray plate, resulting in defects, shrinkage and other problems.
  • the powder coating bonding process is required. (The powder coating and resin are fully mixed and heated to make the pearlescent pigment and resin adhere together, which is called bonding). Bonding solves the problem of poor conductivity of pearlescent pigments, but increases the complexity of the process, and at the same time easily causes the particle size of the powder coating to increase, resulting in poor fluidity of the powder coating.
  • the purpose of the present invention is to overcome the shortcomings of the prior art and provide a pearlescent pigment for powder coatings, a preparation method and a reaction device thereof, so as to overcome the dispersibility, workability, shrinkage and defects of the pearlescent pigment in the powder system The problem of paint application.
  • the present invention provides a pearlescent pigment for powder coatings, which includes a pearlescent pigment substrate, a first polymer film layer coated on the surface of the pearlescent pigment substrate, and a first polymer film coated on the surface of the pearlescent pigment substrate.
  • the second polymer film layer on the surface of the material film layer.
  • the surface of the pearlescent pigment used in the powder coating of the present invention is covered with a polymer film layer, the organic polymer has reactivity to inorganic substances, and the organic functional group has reactivity or compatibility with organic substances. Therefore, when the organic polymer is between the inorganic and organic interface, it can form a bonding layer of organic matrix-polymer chain-inorganic matrix, which can couple and enhance the electrochemical performance and corrosion resistance of the pearlescent pigment surface. Pearlescent pigments have problems with electrification and at the same time enhance the weather resistance of the coating.
  • Surfactants have the characteristics of wetting, anti-sticking, solubilizing, dispersing, washing, anti-corrosion, anti-static, etc.; coating the surface of the pearlescent pigment with a surfactant layer can improve its dispersibility and wettability in the resin, Therefore, the modified pearlescent pigment is coated with the surface of the organic polymer layer and the surfactant layer. After adding the powder coating, the bonding process is not required, and it can be directly sprayed and sprayed on the board. At the same time, it has dispersibility and wettability.
  • the first polymer film layer contains a first auxiliary agent, and the first auxiliary agent is polyoxyethylene alkyl ether, polyoxyethylene alkyl phenol ether, One or more of polyoxyethylene fatty alcohol ethers.
  • the weight percentage of the first auxiliary agent relative to the pearlescent pigment substrate is 0.1-15.0%, or 0.2-10.0%, or 0.3-8.0%, Or 0.4-6.0%, preferably 0.5-3%.
  • the second polymer film layer contains a second auxiliary agent
  • the second auxiliary agent is polymethylsiloxane, polydimethylsiloxane, Polysiloxane-alcohol ether copolymer, alkyl alcohol amide, alkyl sulfonate acetamide, alkyl succinate sulfonate, alcohol amine alkyl benzene sulfonate, alkyl phenol sulfonate, polyoxygen One or more of ethylene monolaurate.
  • the weight percentage of the second auxiliary agent relative to the pearlescent pigment substrate is 0.1-18.0%, or 0.2-15.0%, or 0.3-10.0%, Or 0.4-8.0%, preferably 0.5-5%.
  • the pearlescent pigment substrate is made by coating oxide on the substrate, wherein the substrate is natural mica, synthetic mica, alumina, zinc oxide, oxide One or more of magnesium, calcium oxide, silicon oxide, iron oxide, monocrystalline silicon wafers, glass wafers, and the oxides are titanium oxide, iron oxide, magnesium oxide, zinc oxide, calcium oxide, silicon oxide, aluminum oxide, One or more of tin oxide.
  • the particle size range of the pearlescent pigment is 1 ⁇ m ⁇ D50 ⁇ 800 ⁇ m, and the preferred particle size range is 5 ⁇ m ⁇ D50 ⁇ 250 ⁇ m.
  • the present invention also provides a method for preparing pearlescent pigments for powder coatings, which includes the following steps:
  • the pearlescent pigment covering the first polymer film layer and the second polymer film layer is vacuum filtered from the suspension, washed and dried to obtain the pearlescent pigment for powder coating.
  • the reaction temperature is controlled to be 20-90°C, preferably 40-85°C, particularly preferably 60-80°C.
  • the drying temperature is 70-180°C, preferably 70-150°C, particularly preferably 100-140°C, and the drying time is 2-8 hours. Preferably 1.5-3.5 hours.
  • the pearlescent pigment for powder coating prepared by the preparation method of the present invention not only solves the coating application problems of the pearlescent pigment in the powder system, such as dispersibility, workability, shrinkage and defects, but also solves the lack of brightness and color of powder spraying
  • the problem also eliminates the bonding process of pearlescent pigments in powder coatings, greatly improves the utilization rate of pearlescent pigments, simplifies the powder coating process, reduces production costs, and improves production efficiency.
  • the present invention also provides a reaction device of a pearlescent pigment preparation method, which includes:
  • the feeding device is arranged on the outside of the reaction kettle, and the feeding device includes: a feeding pump system interface for automatically controlling the flow rate for introducing the suspended aqueous solution containing the pearlescent pigment substrate into the reaction kettle, and respectively used to form the first polymer film layer
  • the first auxiliary agent and the second auxiliary agent used to form the second polymer film layer are introduced into the reaction kettle through the manual control flow rate feeding pump system interface;
  • the steam coil is set around the reactor to increase the temperature of the solution in the reactor.
  • the stirring device is a stirring paddle driven by a motor.
  • a baffle for blocking the solution is provided in the reaction kettle to provide shearing force.
  • the bottom of the reaction kettle is provided with a discharge port. After the reaction is completed, the solution is put into the suction filter tank through the discharge port, and the surface package is obtained after washing, suction filtration, and drying. Pearlescent pigments for powder coatings coated with organic polymer layers.
  • reaction device of the present invention to prepare pearlescent pigments for powder coatings can not only continuously and automatically react, improve the efficiency of the pearlescent pigment reaction, reduce labor costs, but also can feed through different feeding ports, avoiding cross-contamination between materials , It can also accurately control the feeding speed of materials, so that the pearlescent pigments that are specially used for powder coatings have the best effect.
  • the pearlescent pigment prepared by the present invention can be directly used in the powder coating system, and the preferred addition amount is 0.5-8.0% by weight, particularly preferably 2.0-5.0% by weight. After stirring and mixing, it can be directly used in the powder coating. Spray construction.
  • the actual technical effect of the present invention not only guarantees the problem of charging with the resin in the powder coating, avoids the problem of nozzle blockage; but also solves the problem of dispersibility of powder spraying, achieving good brightness and brilliant color It also reduces the pearlescent pigment bonding steps in powder coatings, improves the utilization rate of pearlescent pigments, simplifies the process, reduces organic pollution in the bonding process, and reduces costs.
  • Fig. 1 is a schematic diagram of the structure of a pearlescent pigment reaction device used in powder coatings of the present invention.
  • the reaction device used in the preparation method of the pearlescent pigment of the present invention includes:
  • reaction kettle 10 a stirring device is provided in the reaction kettle 10;
  • the feeding device 20 is arranged on the outside of the reactor 10, and the feeding device 20 includes: a feeding pump system interface 200 that automatically controls the flow rate for introducing the suspended aqueous solution containing the pearlescent pigment substrate into the reactor 10, and each will be used to form the first
  • the first auxiliary agent for a polymer film layer and the second auxiliary agent for forming the second polymer film layer are introduced into the reaction kettle through the manual control flow rate feeding pump system interfaces 202 and 204; and
  • the steam coil 30 is arranged around the reactor 10 to increase the temperature of the solution in the reactor 10.
  • the reactor 10 is made of pure titanium metal, and the stirring device is a stirring paddle 102 driven by a motor 100.
  • a baffle 103 for blocking the solution is provided in the reaction kettle 10 to provide shearing force to make the solution agitated more fully.
  • the bottom of the reactor 10 is provided with a discharge port 107. After the reaction is completed, the solution is put into the suction filter tank through the discharge port 107, and the powder is washed, filtered, and dried to obtain a powder coated with an organic polymer layer on the surface. Pearlescent pigments for paints.
  • the steam valve opens, enters through the inlet 300 of the steam coil 30, and then exits from the outlet 302 of the steam coil 30, thereby increasing the temperature of the solution.
  • the motor 100 to drive the stirring paddle 102 to continuously rotate.
  • the speed of the stirring paddle is set to 450r/min.
  • the baffle 103 blocks the solution and provides longitudinal shearing force to make the solution agitate more fully; then open the steam valve and pass the steam plate
  • the inlet of the pipe 30 enters, and it is exported from the outlet of the steam coil 30, thereby raising the temperature of the solution to 70°C; after the temperature is constant, adjust the pH of the suspension in the reactor 10 to 6.5-9.0 with lye;
  • the feed pump system 202 with manual flow control is used to feed the polyoxyethylene alkyl ether into the solution at the feed port at a flow rate of 2L/h for reaction.
  • the feed volume is 0.5-2%.
  • the reaction After stirring for 2 hours, the reaction is complete, and then through the feeding pump system 202 that manually controls the flow rate at a flow rate of 3L/h, the polymethylsiloxane is put into the solution at the feeding port for reaction, the dosage is 0.5%-3%, and the coating Forming a second polymer film layer of the surfactant layer on the surface of the substrate;
  • the solution is put into the suction filter tank through the discharge port 107, and then washed, suction filtered, and dried at 120°C to obtain a pearlescent pigment for powder coating with an organic polymer layer on the surface. .
  • Examples 2 to 5 are basically the same as that of Example 1. The difference is that the substrate material and the coated oxide layer and the amount of coating are different, the resulting hue is different, the particle size is different, and the specific surface area is different, resulting in different dosages. And the feeding speed is different.
  • the specific process parameters and the test results of each layer are shown in Tables 1 to 5.
  • Table 1 shows the process parameters of Examples 1 to 5
  • the pearlescent additive amount is 5% and the spray plate size is 130mm x 70mm.
  • the main performance indicators of the pearlescent pigments for powder coatings prepared by the above examples are as follows. Among them, the finished pearlescent pigments are untreated before treatment, and after the modification is modified by this method. Of pearlescent pigments dedicated to powder coating systems.
  • Table 2 shows the main performance indicators of pearlescent pigments for powder coatings
  • the pearlescent pigments for powder coatings prepared by the reaction device of the present invention can not only react continuously and automatically, improve the efficiency of the pearlescent pigment reaction, reduce labor costs, but also can pass different
  • the feeding port is used for feeding, avoiding cross-contamination between the materials, and accurately controlling the feeding speed of the materials, so that the pearlescent pigments specially used for powder coatings have the best effect.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Paints Or Removers (AREA)

Abstract

Disclosed is a pearlescent pigment for a powder coating, comprising: a pearlescent pigment substrate, a first polymer film layer coated on the surface of the pearlescent pigment substrate, and a second polymer film layer coated on the surface of the first polymer film layer. In addition, also provided is a method for preparing a pearlescent pigment for a powder coating and reaction equipment therefor. Compared with the prior art, the pearlescent pigment for a powder coating obtained according to the preparation method of the present invention not only solves the coating application problems of the dispersivity, applicability, shrinkage cavity and defects of a pearlescent pigment in a powder system, but also solves the problems of insufficient brightness and color of powder spraying, and also eliminates the bonding process of a pearlescent pigment in a powder coating, remarkably improves the use rate of a pearlescent pigment, simplifies the process of implementing a powder coating, and reduces the production cost. The use of the reaction equipment of the present invention can not only efficiently carry out the reaction operation of the pearlescent pigment, but can also reduce the operation intensity, improve the labor efficiency, and save on the costs and the energy consumption.

Description

用于粉末涂料的珠光颜料、制备方法及其反应装置Pearlescent pigment for powder coating, preparation method and reaction device thereof 技术领域Technical field
本发明涉及一种珠光颜料，更具体地说，本发明涉及一种用于粉末涂料的珠光颜料、制备方法及其反应装置。The invention relates to a pearlescent pigment, more specifically, the invention relates to a pearlescent pigment for powder coating, a preparation method and a reaction device thereof.
背景技术Background technique
粉末涂料是以固体树脂和颜料、填料、助剂等形成的固体粉末状合成树脂涂料。和普通溶剂型涂料及水性涂料不同，粉末涂料的分散介质不是溶剂和水，而是空气。粉末涂料具有不含毒性，完全符合国家环保法的要求；原材料利用率高，最高的利用率高达99％以上；易实现自动化操作，生产效率高，可降低成本；涂层抗冲击强度和韧性均好，具有优良的耐化学药品腐蚀性能和电气绝缘性能；存贮、运输安全和方便等特点。Powder coating is a solid powdery synthetic resin coating formed by solid resin, pigments, fillers, additives, etc. Unlike ordinary solvent-based coatings and water-based coatings, the dispersion medium of powder coatings is not solvent and water, but air. The powder coating is non-toxic and fully meets the requirements of the national environmental protection law; the utilization rate of raw materials is high, and the highest utilization rate is as high as 99%; it is easy to realize automatic operation, high production efficiency, and can reduce costs; the impact strength and toughness of the coating are both Good, it has excellent chemical resistance and electrical insulation; it is safe and convenient for storage and transportation.
目前，粉末涂料涂装市场的最大增长领域是：船舶工业、管道工业、汽车行业、木材和塑料用涂料涂装等领域，这些领域的需求大大促进了粉末涂料的需求量，未来粉末涂料的市场将会越来越大，应用会越来越广泛。At present, the largest growth areas of the powder coatings coating market are: shipbuilding, pipeline industry, automotive industry, wood and plastic coatings and other fields. The demand in these fields has greatly promoted the demand for powder coatings, and the future market for powder coatings It will be bigger and bigger, and the application will be more and more extensive.
粉末喷涂是利用高压静电电晕电场的原理，在喷枪头部金属导流标上接上高压负极，被喷涂工件接地形成正极，使喷枪和工件之间形成一个较强的静电电场。当作为运载气体的压缩空气，将粉末涂料从供粉桶经过粉管送到喷枪的导流杆时，由于导流杆接上高压负极产生的电晕放电，在其附近产生了密集的负电荷，使粉末带上负电荷，并进入了电场强度很高的静电场，在静电力和运载气体的双重作用下，粉末均匀地飞向接地工件表面形成厚薄均匀的粉层，再加热固化转化为耐久的涂膜。Powder spraying uses the principle of high-voltage electrostatic corona electric field. A high-voltage negative electrode is connected to the metal diversion mark of the spray gun head, and the sprayed workpiece is grounded to form a positive electrode, so that a strong electrostatic electric field is formed between the spray gun and the workpiece. When the compressed air used as the carrier gas sends the powder paint from the powder supply tank to the guide rod of the spray gun through the powder tube, the corona discharge generated by the guide rod connected to the high voltage negative electrode generates dense negative charges near it. , So that the powder is negatively charged and enters the electrostatic field with high electric field strength. Under the dual action of electrostatic force and carrier gas, the powder evenly flies to the surface of the grounded workpiece to form a uniform thickness of powder layer, and then heat and solidify into Durable coating film.
珠光颜料以一种或数种金属氧化物包覆在基材表面，形成层状的结构，通过光的干涉而形成的一种具有珠光效果的颜料。可以改变包覆在基材表面的金属氧化物厚度，使其产生不同的光的干涉作用，得到不同的颜色和珠光效果的 珠光颜料。但是，珠光颜料加入粉末涂料中直接用于静电喷涂时，存在上粉率不高、容易堵枪、喷板表面容易分散不均，造成缺陷、缩孔等问题，一般需要经过粉末涂料邦定工艺(将粉末涂料与树脂充分混合后加热，使珠光颜料与树脂粘附在一起，称为邦定)。邦定解决了珠光颜料导电性差的问题，但是，增加了工艺的复杂性，同时容易造成粉末涂料粒径增大，导致粉末涂料流动性变差。The pearlescent pigment is coated on the surface of the substrate with one or several kinds of metal oxides to form a layered structure, which is a kind of pigment with pearlescent effect formed by the interference of light. The thickness of the metal oxide coated on the surface of the substrate can be changed to produce different light interference effects to obtain pearlescent pigments with different colors and pearlescent effects. However, when pearlescent pigments are added to powder coatings for electrostatic spraying directly, there are problems such as low powder loading rate, easy to block the gun, and uneven dispersion on the surface of the spray plate, resulting in defects, shrinkage and other problems. Generally, the powder coating bonding process is required. (The powder coating and resin are fully mixed and heated to make the pearlescent pigment and resin adhere together, which is called bonding). Bonding solves the problem of poor conductivity of pearlescent pigments, but increases the complexity of the process, and at the same time easily causes the particle size of the powder coating to increase, resulting in poor fluidity of the powder coating.
有鉴于此，确有必要提供一种用于粉末涂料的珠光颜料、制备方法及其反应装置，以克服珠光颜料在粉末体系中的分散性、施工性、缩孔和缺陷的涂料应用问题。In view of this, it is indeed necessary to provide a pearlescent pigment for powder coatings, a preparation method and a reaction device thereof, to overcome the coating application problems of the pearlescent pigment in the powder system, such as dispersibility, workability, shrinkage and defects.
发明内容Summary of the invention
本发明的目的在于：克服现有技术的不足，提供一种用于粉末涂料的珠光颜料、制备方法及其反应装置，以克服珠光颜料在粉末体系中的分散性、施工性、缩孔和缺陷的涂料应用问题。The purpose of the present invention is to overcome the shortcomings of the prior art and provide a pearlescent pigment for powder coatings, a preparation method and a reaction device thereof, so as to overcome the dispersibility, workability, shrinkage and defects of the pearlescent pigment in the powder system The problem of paint application.
为了实现上述发明目的，本发明提供了一种用于粉末涂料的珠光颜料，其包括珠光颜料基材、包覆在珠光颜料基材表面的第一聚合物膜层，以及包覆在第一聚合物膜层表面的第二聚合物膜层。In order to achieve the above-mentioned purpose of the invention, the present invention provides a pearlescent pigment for powder coatings, which includes a pearlescent pigment substrate, a first polymer film layer coated on the surface of the pearlescent pigment substrate, and a first polymer film coated on the surface of the pearlescent pigment substrate. The second polymer film layer on the surface of the material film layer.
本发明用于粉末涂料的珠光颜料的表面包覆有聚合物膜层，有机聚合物对无机物具有反应性，有机官能基对有机物具有反应性或相容性。因此，当有机聚合物介于无机和有机界面之间，可形成有机基体-聚合物链-无机基体的结合层，起到偶联和增强珠光颜料表面的电化学性能和抗腐蚀性能，解决了珠光颜料带电性问题，同时增强了涂层的耐候性能。表面活性剂具有润湿、抗粘、增溶、分散、洗涤、防腐、抗静电等特点；在珠光颜料的表面包覆表面活性剂层，能提高其在树脂中的分散性、润湿性，因此经过有机聚合物层和表面活性剂层表面包覆，改性后的珠光颜料，再加入粉末涂料后，不需要邦定过程，可直接喷涂与喷板上，同时其分散性和润湿性好，很好地解决了粉末涂料的喷涂问题， 降低了粉末涂料的生产成本，提高了粉末涂料的利用率，同时提高了粉末涂料的喷涂效果，得到色彩艳丽的具有珠光效应的新型粉末涂料，扩展了粉末涂料的使用领域。The surface of the pearlescent pigment used in the powder coating of the present invention is covered with a polymer film layer, the organic polymer has reactivity to inorganic substances, and the organic functional group has reactivity or compatibility with organic substances. Therefore, when the organic polymer is between the inorganic and organic interface, it can form a bonding layer of organic matrix-polymer chain-inorganic matrix, which can couple and enhance the electrochemical performance and corrosion resistance of the pearlescent pigment surface. Pearlescent pigments have problems with electrification and at the same time enhance the weather resistance of the coating. Surfactants have the characteristics of wetting, anti-sticking, solubilizing, dispersing, washing, anti-corrosion, anti-static, etc.; coating the surface of the pearlescent pigment with a surfactant layer can improve its dispersibility and wettability in the resin, Therefore, the modified pearlescent pigment is coated with the surface of the organic polymer layer and the surfactant layer. After adding the powder coating, the bonding process is not required, and it can be directly sprayed and sprayed on the board. At the same time, it has dispersibility and wettability. Good, it solves the spraying problem of powder coatings, reduces the production cost of powder coatings, improves the utilization rate of powder coatings, and at the same time improves the spraying effect of powder coatings, and obtains colorful new powder coatings with pearl effect. Expanded the use of powder coatings.
作为本发明用于粉末涂料的珠光颜料的一种改进，所述第一聚合物膜层中含有第一助剂，第一助剂为聚氧化乙烯烷化醚、聚氧乙烯烷基酚醚、聚氧乙烯脂肪醇醚中的一种或多种。As an improvement of the pearlescent pigment used in powder coatings of the present invention, the first polymer film layer contains a first auxiliary agent, and the first auxiliary agent is polyoxyethylene alkyl ether, polyoxyethylene alkyl phenol ether, One or more of polyoxyethylene fatty alcohol ethers.
作为本发明用于粉末涂料的珠光颜料的一种改进，所述第一助剂相对于所述珠光颜料基材的重量百分比为0.1-15.0％，或0.2-10.0％，或0.3-8.0％，或0.4-6.0％，优选0.5-3％。As an improvement of the pearlescent pigment for powder coatings of the present invention, the weight percentage of the first auxiliary agent relative to the pearlescent pigment substrate is 0.1-15.0%, or 0.2-10.0%, or 0.3-8.0%, Or 0.4-6.0%, preferably 0.5-3%.
作为本发明用于粉末涂料的珠光颜料的一种改进，所述第二聚合物膜层中含有第二助剂，第二助剂为聚甲基硅氧烷、聚二甲基硅氧烷、聚硅氧烷-醇醚共聚物、烷基醇酰胺、烷基磺酸基乙酰胺、烷基琥珀酸酯磺酸盐、醇胺烷基苯磺酸盐、烷基酚磺酸酯、聚氧乙烯单月桂酸酯中的一种或多种。As an improvement of the pearlescent pigment used in powder coatings of the present invention, the second polymer film layer contains a second auxiliary agent, and the second auxiliary agent is polymethylsiloxane, polydimethylsiloxane, Polysiloxane-alcohol ether copolymer, alkyl alcohol amide, alkyl sulfonate acetamide, alkyl succinate sulfonate, alcohol amine alkyl benzene sulfonate, alkyl phenol sulfonate, polyoxygen One or more of ethylene monolaurate.
作为本发明用于粉末涂料的珠光颜料的一种改进，所述第二助剂相对于所述珠光颜料基材的重量百分比为0.1-18.0％，或0.2-15.0％，或0.3-10.0％，或0.4-8.0％，优选0.5-5％。As an improvement of the pearlescent pigment for powder coatings of the present invention, the weight percentage of the second auxiliary agent relative to the pearlescent pigment substrate is 0.1-18.0%, or 0.2-15.0%, or 0.3-10.0%, Or 0.4-8.0%, preferably 0.5-5%.
作为本发明用于粉末涂料的珠光颜料的一种改进，所述珠光颜料基材通过在基材包覆氧化物制成，其中，基材为天然云母、合成云母、氧化铝、氧化锌、氧化镁、氧化钙、氧化硅、氧化铁、单晶硅片、玻璃片中的一种或多种，氧化物为氧化钛、氧化铁、氧化镁、氧化锌、氧化钙、氧化硅、氧化铝、氧化锡中的一种或几种。As an improvement of the pearlescent pigment used in powder coatings of the present invention, the pearlescent pigment substrate is made by coating oxide on the substrate, wherein the substrate is natural mica, synthetic mica, alumina, zinc oxide, oxide One or more of magnesium, calcium oxide, silicon oxide, iron oxide, monocrystalline silicon wafers, glass wafers, and the oxides are titanium oxide, iron oxide, magnesium oxide, zinc oxide, calcium oxide, silicon oxide, aluminum oxide, One or more of tin oxide.
作为本发明用于粉末涂料的珠光颜料的一种改进，所述珠光颜料的粒径范围为1μm≤D50≤800μm，优选粒径范围为5μm≤D50≤250μm。As an improvement of the pearlescent pigment used in powder coatings of the present invention, the particle size range of the pearlescent pigment is 1μm≤D50≤800μm, and the preferred particle size range is 5μm≤D50≤250μm.
为了实现上述发明目的，本发明还提供了一种用于粉末涂料的珠光颜料的制备方法，其包括以下步骤：In order to achieve the above-mentioned purpose of the invention, the present invention also provides a method for preparing pearlescent pigments for powder coatings, which includes the following steps:
1)将第一助剂加入到含有珠光颜料基材的悬浮水溶液中进行表面聚合反 应，控制反应温度，控制搅拌速度在300-500r/min，控制溶液pH在6.5-9.0，使第一助剂聚合为第一聚合物膜层并吸附到珠光颜料基材的表面；1) Add the first auxiliary agent to the suspended aqueous solution containing the pearlescent pigment substrate for surface polymerization reaction, control the reaction temperature, control the stirring speed at 300-500r/min, control the pH of the solution at 6.5-9.0, and make the first auxiliary agent Polymerized into the first polymer film layer and adsorbed to the surface of the pearlescent pigment substrate;
2)搅拌1.5-2.5h充分反应后，再加入第二助剂，控制反应温度，控制搅拌速度在300-500r/min，控制溶液pH在6.5-9.0，搅拌1.5-2.5h，使第二助剂形成第二聚合物膜层并充分包覆在步骤1)形成的珠光颜料表面；2) After stirring for 1.5-2.5h to fully react, add the second auxiliary agent, control the reaction temperature, control the stirring speed at 300-500r/min, control the pH of the solution at 6.5-9.0, and stir for 1.5-2.5h to make the second auxiliary The agent forms the second polymer film layer and fully coats the surface of the pearlescent pigment formed in step 1);
3)将包覆第一聚合物膜层和第二聚合物膜层的珠光颜料从悬浮液中真空抽滤，经洗涤和干燥，获得用于粉末涂料的珠光颜料。3) The pearlescent pigment covering the first polymer film layer and the second polymer film layer is vacuum filtered from the suspension, washed and dried to obtain the pearlescent pigment for powder coating.
作为本发明珠光颜料的制备方法的一种改进，步骤1)和2)中，控制反应温度为20～90℃，优选40～85℃，特别优选60-80℃。As an improvement of the preparation method of the pearlescent pigment of the present invention, in steps 1) and 2), the reaction temperature is controlled to be 20-90°C, preferably 40-85°C, particularly preferably 60-80°C.
作为本发明珠光颜料的制备方法的一种改进，步骤3)中，烘干的温度是70-180℃，优选70-150℃，特别优选100-140℃，烘干时间为2～8小时，优选1.5-3.5小时。As an improvement of the preparation method of the pearlescent pigment of the present invention, in step 3), the drying temperature is 70-180°C, preferably 70-150°C, particularly preferably 100-140°C, and the drying time is 2-8 hours. Preferably 1.5-3.5 hours.
采用本发明制备方法制备的用于粉末涂料的珠光颜料，既解决了珠光颜料在粉末体系中的分散性、施工性、缩孔和缺陷的涂料应用问题，又解决了粉末喷涂的亮度和颜色不足问题，还消除了粉末涂料中珠光颜料的邦定过程，大大提高了珠光颜料使用率，简化了粉末涂料的工艺，降低了生产成本，提升了生产效率。The pearlescent pigment for powder coating prepared by the preparation method of the present invention not only solves the coating application problems of the pearlescent pigment in the powder system, such as dispersibility, workability, shrinkage and defects, but also solves the lack of brightness and color of powder spraying The problem also eliminates the bonding process of pearlescent pigments in powder coatings, greatly improves the utilization rate of pearlescent pigments, simplifies the powder coating process, reduces production costs, and improves production efficiency.
为了实现上述发明目的，本发明还提供了一种珠光颜料的制备方法的反应装置，其包括：In order to achieve the above-mentioned object of the invention, the present invention also provides a reaction device of a pearlescent pigment preparation method, which includes:
反应釜，反应釜内设有搅拌装置；Reaction kettle, a stirring device is installed in the reaction kettle;
加料装置，设置在反应釜外侧，加料装置包括：用于将含有珠光颜料基材的悬浮水溶液导入反应釜内的自动控制流速的加料泵系统接口，以及分别将用于形成第一聚合物膜层的第一助剂和用于形成第二聚合物膜层的第二助剂导入反应釜内的手动控制流速的加料泵系统接口；以及The feeding device is arranged on the outside of the reaction kettle, and the feeding device includes: a feeding pump system interface for automatically controlling the flow rate for introducing the suspended aqueous solution containing the pearlescent pigment substrate into the reaction kettle, and respectively used to form the first polymer film layer The first auxiliary agent and the second auxiliary agent used to form the second polymer film layer are introduced into the reaction kettle through the manual control flow rate feeding pump system interface; and
蒸汽盘管，围绕反应釜设置，用于提升反应釜内溶液的温度。The steam coil is set around the reactor to increase the temperature of the solution in the reactor.
作为本发明反应装置的一种改进，所述搅拌装置为通过电机带动的搅拌 桨。As an improvement of the reaction device of the present invention, the stirring device is a stirring paddle driven by a motor.
作为本发明反应装置的一种改进，所述反应釜内设有阻挡溶液的挡流板，用于提供剪切力。As an improvement of the reaction device of the present invention, a baffle for blocking the solution is provided in the reaction kettle to provide shearing force.
作为本发明反应装置的一种改进，所述反应釜的底部设有放料口，反应完全后，通过放料口将溶液放入抽滤池中，经洗涤、抽滤、烘干得到表面包覆有机聚合物层的用于粉末涂料的珠光颜料。As an improvement of the reaction device of the present invention, the bottom of the reaction kettle is provided with a discharge port. After the reaction is completed, the solution is put into the suction filter tank through the discharge port, and the surface package is obtained after washing, suction filtration, and drying. Pearlescent pigments for powder coatings coated with organic polymer layers.
采用本发明反应装置制备用于粉末涂料的珠光颜料，既能连续自动的进行反应，提高珠光颜料反应的效率，降低劳动成本，又能通过不同的加料口进行加料，避免了物料间的交叉污染，还可对物料的加料速度进行精准控制，使得到的专用于粉末涂料的珠光颜料效果最佳。Using the reaction device of the present invention to prepare pearlescent pigments for powder coatings can not only continuously and automatically react, improve the efficiency of the pearlescent pigment reaction, reduce labor costs, but also can feed through different feeding ports, avoiding cross-contamination between materials , It can also accurately control the feeding speed of materials, so that the pearlescent pigments that are specially used for powder coatings have the best effect.
此外，本发明制备的珠光颜料，可直接用于粉末涂料体系，优选添加量为0.5-8.0％(重量)，特别优选2.0-5.0％(重量)，经过搅拌混匀后，直接用于粉末涂料喷涂施工。In addition, the pearlescent pigment prepared by the present invention can be directly used in the powder coating system, and the preferred addition amount is 0.5-8.0% by weight, particularly preferably 2.0-5.0% by weight. After stirring and mixing, it can be directly used in the powder coating. Spray construction.
相对于现有技术，本发明的实际技术效果：既保证了与粉末涂料中树脂带电性的问题，避免了喷头堵料的问题；又解决了粉末喷涂的分散性问题，达到亮度好和颜色绚丽的喷涂效果；还减少了粉末涂料中珠光颜料邦定步骤，提升了珠光颜料利用率，简化了工艺，减少了邦定过程中的有机污染，降低了成本。Compared with the prior art, the actual technical effect of the present invention: not only guarantees the problem of charging with the resin in the powder coating, avoids the problem of nozzle blockage; but also solves the problem of dispersibility of powder spraying, achieving good brightness and brilliant color It also reduces the pearlescent pigment bonding steps in powder coatings, improves the utilization rate of pearlescent pigments, simplifies the process, reduces organic pollution in the bonding process, and reduces costs.
附图说明Description of the drawings
以下结合附图和具体实施例，对本发明用于粉末涂料的珠光颜料、制备方法及其反应装置进行详细说明，其中：The pearlescent pigment for powder coating, preparation method and reaction device of the present invention will be described in detail below with reference to the accompanying drawings and specific embodiments, in which:
图1为本发明用于粉末涂料的珠光颜料的反应装置的结构示意图。Fig. 1 is a schematic diagram of the structure of a pearlescent pigment reaction device used in powder coatings of the present invention.
具体实施方式detailed description
为了进一步了解本发明，以下结合实施例对本发明作进一步的详细阐述，但并非对本发明的限制，应当理解，这些描述只是为了进一步说明本发明的特 征和优点，而不是对本发明权利要求的限制。凡依照本发明公开内容所作的任何本领域的等同替换，均属于本发明的保护范围。In order to further understand the present invention, the following examples will further describe the present invention in detail, but it is not a limitation of the present invention. It should be understood that these descriptions are only to further illustrate the features and advantages of the present invention, not to limit the claims of the present invention. Any equivalent replacement in this field made in accordance with the disclosure of the present invention falls within the protection scope of the present invention.
反应装置Reaction device
请参照图1所示，用于本发明珠光颜料的制备方法的反应装置，包括：Please refer to FIG. 1, the reaction device used in the preparation method of the pearlescent pigment of the present invention includes:
反应釜10，反应釜10内设有搅拌装置； Reaction kettle 10, a stirring device is provided in the reaction kettle 10;
加料装置20，设置在反应釜10外侧，加料装置20包括：用于将含有珠光颜料基材的悬浮水溶液导入反应釜10内的自动控制流速的加料泵系统接口200，以及分别将用于形成第一聚合物膜层的第一助剂和用于形成第二聚合物膜层的第二助剂导入反应釜内的手动控制流速的加料泵系统接口202、204；以及The feeding device 20 is arranged on the outside of the reactor 10, and the feeding device 20 includes: a feeding pump system interface 200 that automatically controls the flow rate for introducing the suspended aqueous solution containing the pearlescent pigment substrate into the reactor 10, and each will be used to form the first The first auxiliary agent for a polymer film layer and the second auxiliary agent for forming the second polymer film layer are introduced into the reaction kettle through the manual control flow rate feeding pump system interfaces 202 and 204; and
蒸汽盘管30，围绕反应釜10设置，用于提升反应釜10内溶液的温度。The steam coil 30 is arranged around the reactor 10 to increase the temperature of the solution in the reactor 10.
在图1所示实施方式中，反应釜10为纯钛金属制成，搅拌装置为通过电机100带动的搅拌桨102。反应釜内10设有阻挡溶液的挡流板103，用于提供剪切力，使溶液搅拌更加充分。反应釜10的底部设有放料口107，反应完全后，通过放料口107将溶液放入抽滤池中，经洗涤、抽滤、烘干得到表面包覆有机聚合物层的用于粉末涂料的珠光颜料。蒸汽阀门打开，通过蒸汽盘管30的入口300进入，再从蒸汽盘管30的出口302导出，从而提升溶液的温度。In the embodiment shown in FIG. 1, the reactor 10 is made of pure titanium metal, and the stirring device is a stirring paddle 102 driven by a motor 100. A baffle 103 for blocking the solution is provided in the reaction kettle 10 to provide shearing force to make the solution agitated more fully. The bottom of the reactor 10 is provided with a discharge port 107. After the reaction is completed, the solution is put into the suction filter tank through the discharge port 107, and the powder is washed, filtered, and dried to obtain a powder coated with an organic polymer layer on the surface. Pearlescent pigments for paints. The steam valve opens, enters through the inlet 300 of the steam coil 30, and then exits from the outlet 302 of the steam coil 30, thereby increasing the temperature of the solution.
实施例1Example 1
将300kg粒径为5-25μm的由二氧化钛包覆的天然云母薄片制成的珠光颜料成品和去离子水制成1:12(重量比)的悬浮溶液后，通过自动控制流速的加料泵系统200在反应釜口将含有珠光颜料的悬浮水溶液导入反应釜10内；After 300 kg of pearlescent pigment products made of natural mica flakes coated with titanium dioxide with a particle size of 5-25 μm and deionized water are made into a 1:12 (weight ratio) suspension solution, it is passed through a feeding pump system 200 that automatically controls the flow rate. Introduce the suspended aqueous solution containing pearlescent pigments into the reactor 10 at the mouth of the reactor;
将电机100开启带动搅拌桨102不停转动，搅拌桨转速设置为450r/min，同时挡流板103阻挡溶液，提供纵向剪切力，使溶液搅拌更加充分；再将蒸汽阀门打开，通过蒸汽盘管30入口进入，再从蒸汽盘管30出口导出，从而提升溶液的温度到70℃；温度恒定后，用碱液将反应釜10内的悬浮液pH调节至6.5-9.0；Turn on the motor 100 to drive the stirring paddle 102 to continuously rotate. The speed of the stirring paddle is set to 450r/min. At the same time, the baffle 103 blocks the solution and provides longitudinal shearing force to make the solution agitate more fully; then open the steam valve and pass the steam plate The inlet of the pipe 30 enters, and it is exported from the outlet of the steam coil 30, thereby raising the temperature of the solution to 70°C; after the temperature is constant, adjust the pH of the suspension in the reactor 10 to 6.5-9.0 with lye;
通过手动控制流速的加料泵系统202以2L/h的流速，在加料口将聚氧化乙烯烷化醚入溶液中进行反应，加料量为0.5-2％，包覆在基材表面形成第一有机聚合物膜层；The feed pump system 202 with manual flow control is used to feed the polyoxyethylene alkyl ether into the solution at the feed port at a flow rate of 2L/h for reaction. The feed volume is 0.5-2%. Polymer film
搅拌2小时后，反应完全，再通过手动控制流速的加料泵系统202以3L/h的流速，在加料口将聚甲基硅氧烷入溶液中进行反应，用量0.5％-3％，包覆在基材表面形成表面活性剂层第二聚合物膜层；After stirring for 2 hours, the reaction is complete, and then through the feeding pump system 202 that manually controls the flow rate at a flow rate of 3L/h, the polymethylsiloxane is put into the solution at the feeding port for reaction, the dosage is 0.5%-3%, and the coating Forming a second polymer film layer of the surfactant layer on the surface of the substrate;
搅拌3小时后，反应完全后，通过放料口107将溶液放入抽滤池中，之后经过洗涤、抽滤、120℃烘干得到表面包覆有机聚合物层的用于粉末涂料的珠光颜料。After stirring for 3 hours, after the reaction is complete, the solution is put into the suction filter tank through the discharge port 107, and then washed, suction filtered, and dried at 120°C to obtain a pearlescent pigment for powder coating with an organic polymer layer on the surface. .
实施例2～5与实施例1方法基本相同，不同之处在于基片材料和包覆的氧化物层及包覆量不同，生成的色相不同，粒径不同，比表面积不同，导致用量不同，且需要加料速度不同。具体工艺参数和各层测试结果如表1～5所示。The methods of Examples 2 to 5 are basically the same as that of Example 1. The difference is that the substrate material and the coated oxide layer and the amount of coating are different, the resulting hue is different, the particle size is different, and the specific surface area is different, resulting in different dosages. And the feeding speed is different. The specific process parameters and the test results of each layer are shown in Tables 1 to 5.
表1为实施例1～5工艺参数Table 1 shows the process parameters of Examples 1 to 5
Figure PCTCN2021070372-appb-000001
Figure PCTCN2021070372-appb-000001
珠光添加量5％及喷板尺寸130mm x70mm固定，通过上述实施例制得的粉末涂料用珠光颜料主要性能指标如下，其中，处理前为未处理珠光颜料成品，处理后为用该方法改性后的专用于粉末涂料体系的珠光颜料。The pearlescent additive amount is 5% and the spray plate size is 130mm x 70mm. The main performance indicators of the pearlescent pigments for powder coatings prepared by the above examples are as follows. Among them, the finished pearlescent pigments are untreated before treatment, and after the modification is modified by this method. Of pearlescent pigments dedicated to powder coating systems.
表2为粉末涂料专用珠光颜料主要性能指标Table 2 shows the main performance indicators of pearlescent pigments for powder coatings
Figure PCTCN2021070372-appb-000002
Figure PCTCN2021070372-appb-000002
结合以上对本发明实施例的描述可以看出，采用本发明反应装置制备的用于粉末涂料的珠光颜料，既能连续自动的进行反应，提高珠光颜料反应的效率，降低劳动成本，又能通过不同的加料口进行加料，避免了物料间的交叉污染， 又可对物料的加料速度进行精准控制，使得到的专用于粉末涂料的珠光颜料效果最佳。In combination with the above description of the embodiments of the present invention, it can be seen that the pearlescent pigments for powder coatings prepared by the reaction device of the present invention can not only react continuously and automatically, improve the efficiency of the pearlescent pigment reaction, reduce labor costs, but also can pass different The feeding port is used for feeding, avoiding cross-contamination between the materials, and accurately controlling the feeding speed of the materials, so that the pearlescent pigments specially used for powder coatings have the best effect.
上述实施例并非是对于本发明的限制，本发明并非仅限于上述实施例，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改，等同替换、改进等，均应包含在本发明的保护范围之内。The above-mentioned embodiments are not a limitation to the present invention, and the present invention is not limited to the above-mentioned embodiments. For those skilled in the art, the present invention can have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (13)

  1. 一种用于粉末涂料的珠光颜料，其特征在于，所述珠光颜料包括珠光颜料基材、包覆在珠光颜料基材表面的第一聚合物膜层，以及包覆在第一聚合物膜层表面的第二聚合物膜层。A pearlescent pigment for powder coatings, characterized in that the pearlescent pigment comprises a pearlescent pigment substrate, a first polymer film layer coated on the surface of the pearlescent pigment substrate, and a first polymer film layer coated on the surface of the pearlescent pigment substrate The second polymer film layer on the surface.
  2. 根据权利要求1所述的用于粉末涂料的珠光颜料，其特征在于，所述第一聚合物膜层中含有第一助剂，第一助剂为聚氧化乙烯烷化醚、聚氧乙烯烷基酚醚、聚氧乙烯脂肪醇醚中的一种或多种。The pearlescent pigment for powder coatings according to claim 1, wherein the first polymer film layer contains a first auxiliary agent, and the first auxiliary agent is polyoxyethylene alkyl ether, polyoxyethylene alkyl One or more of base phenol ether and polyoxyethylene fatty alcohol ether.
  3. 根据权利要求2所述的用于粉末涂料的珠光颜料，其特征在于，所述第一助剂相对于所述珠光颜料基材的重量百分比为0.1-15.0％，或0.2-10.0％，或0.3-8.0％，或0.4-6.0％，优选0.5-3％。The pearlescent pigment for powder coatings according to claim 2, wherein the weight percentage of the first auxiliary agent relative to the pearlescent pigment substrate is 0.1-15.0%, or 0.2-10.0%, or 0.3 -8.0%, or 0.4-6.0%, preferably 0.5-3%.
  4. 根据权利要求1所述的用于粉末涂料的珠光颜料，其特征在于，所述第二聚合物膜层中含有第二助剂，第二助剂为聚甲基硅氧烷、聚二甲基硅氧烷、聚硅氧烷-醇醚共聚物、烷基醇酰胺、烷基磺酸基乙酰胺、烷基琥珀酸酯磺酸盐、醇胺烷基苯磺酸盐、烷基酚磺酸酯、聚氧乙烯单月桂酸酯中的一种或多种。The pearlescent pigment for powder coatings according to claim 1, wherein the second polymer film layer contains a second auxiliary agent, and the second auxiliary agent is polymethylsiloxane, polydimethylsiloxane, and polydimethylsiloxane. Silicone, polysiloxane-alcohol ether copolymer, alkyl alcohol amide, alkyl sulfonate acetamide, alkyl succinate sulfonate, alcohol amine alkyl benzene sulfonate, alkyl phenol sulfonic acid One or more of ester and polyoxyethylene monolaurate.
  5. 根据权利要求4所述的用于粉末涂料的珠光颜料，其特征在于，所述第二助剂相对于所述珠光颜料基材的重量百分比为0.1-18.0％，或0.2-15.0％，或0.3-10.0％，或0.4-8.0％，优选0.5-5％。The pearlescent pigment for powder coatings according to claim 4, wherein the weight percentage of the second auxiliary agent relative to the pearlescent pigment substrate is 0.1-18.0%, or 0.2-15.0%, or 0.3 -10.0%, or 0.4-8.0%, preferably 0.5-5%.
  6. 根据权利要求1所述的用于粉末涂料的珠光颜料，其特征在于，所述珠光颜料基材通过在基材包覆氧化物制成，其中，基材为天然云母、合成云母、氧化铝、氧化锌、氧化镁、氧化钙、氧化硅、氧化铁、单晶硅片、玻璃片中的一种或多种，氧化物为氧化钛、氧化铁、氧化镁、氧化锌、氧化钙、氧化硅、氧化铝、氧化锡中的一种或几种。The pearlescent pigment for powder coatings according to claim 1, wherein the pearlescent pigment substrate is made by coating oxide on the substrate, wherein the substrate is natural mica, synthetic mica, alumina, One or more of zinc oxide, magnesium oxide, calcium oxide, silicon oxide, iron oxide, monocrystalline silicon wafers, glass flakes, and the oxides are titanium oxide, iron oxide, magnesium oxide, zinc oxide, calcium oxide, silicon oxide One or more of, aluminum oxide and tin oxide.
  7. 根据权利要求1所述的用于粉末涂料的珠光颜料，其特征在于，所述珠光颜料的粒径范围为1μm≤D50≤800μm，优选粒径范围为5μm≤D50≤250μm。The pearlescent pigment for powder coatings according to claim 1, characterized in that the particle size range of the pearlescent pigment is 1μm≤D50≤800μm, preferably the particle size range is 5μm≤D50≤250μm.
  8. 一种权利要求1至7中任一项所述的用于粉末涂料的珠光颜料的制备方法，其特征在于，包括以下步骤：A method for preparing pearlescent pigments for powder coatings according to any one of claims 1 to 7, characterized in that it comprises the following steps:
    1)将第一助剂加入到含有珠光颜料基材的悬浮水溶液中进行表面聚合反应，控制反应温度，控制搅拌速度在300-500r/min，控制溶液pH在6.5-9.0，使第一助剂聚合为第一聚合物膜层并吸附到珠光颜料基材的表面；1) Add the first auxiliary agent to the suspended aqueous solution containing the pearlescent pigment substrate for surface polymerization reaction, control the reaction temperature, control the stirring speed at 300-500r/min, control the pH of the solution at 6.5-9.0, and make the first auxiliary agent Polymerized into the first polymer film layer and adsorbed to the surface of the pearlescent pigment substrate;
    2)搅拌1.5-2.5h充分反应后，再加入第二助剂，控制反应温度，控制搅拌速度在300-500r/min，控制溶液pH在6.5-9.0，使第二助剂形成第二聚合物膜层并充分包覆在步骤1)形成的珠光颜料表面；以及2) After stirring for 1.5-2.5h to fully react, add the second auxiliary agent, control the reaction temperature, control the stirring speed at 300-500r/min, control the pH of the solution at 6.5-9.0, and make the second auxiliary agent form the second polymer The film layer fully covers the surface of the pearlescent pigment formed in step 1); and
    3)将包覆第一聚合物膜层和第二聚合物膜层的珠光颜料从悬浮液中真空抽滤，经洗涤和干燥，获得用于粉末涂料的珠光颜料。3) The pearlescent pigment covering the first polymer film layer and the second polymer film layer is vacuum filtered from the suspension, washed and dried to obtain the pearlescent pigment for powder coating.
  9. 根据权利要求8所述的珠光颜料的制备方法，其特征在于，步骤1)和2)中，控制反应温度为20～90℃，优选40～85℃，特别优选60-80℃。The method for preparing pearlescent pigments according to claim 8, characterized in that in steps 1) and 2), the reaction temperature is controlled to be 20-90°C, preferably 40-85°C, particularly preferably 60-80°C.
  10. 一种用于权利要求8或9所述的珠光颜料的制备方法的反应装置，其特征在于，包括：A reaction device used in the method for preparing pearlescent pigments according to claim 8 or 9, characterized in that it comprises:
    反应釜，反应釜内设有搅拌装置；Reaction kettle, a stirring device is installed in the reaction kettle;
    加料装置，设置在反应釜外侧，加料装置包括：用于将含有珠光颜料基材的悬浮水溶液导入反应釜内的自动控制流速的加料泵系统接口，以及分别将用于形成第一聚合物膜层的第一助剂和用于形成第二聚合物膜层的第二助剂导入反应釜内的手动控制流速的加料泵系统接口；以及The feeding device is arranged on the outside of the reaction kettle, and the feeding device includes: a feeding pump system interface for automatically controlling the flow rate for introducing the suspended aqueous solution containing the pearlescent pigment substrate into the reaction kettle, and respectively used to form the first polymer film layer The first auxiliary agent and the second auxiliary agent used to form the second polymer film layer are introduced into the reaction kettle through the manual control flow rate feeding pump system interface; and
    蒸汽盘管，围绕反应釜设置，用于提升反应釜内溶液的温度。The steam coil is set around the reactor to increase the temperature of the solution in the reactor.
  11. 根据权利要求10所述的反应装置，其特征在于，所述搅拌装置为通过电机带动的搅拌桨。The reaction device according to claim 10, wherein the stirring device is a stirring paddle driven by a motor.
  12. 根据权利要求10所述的反应装置，其特征在于，所述反应釜内设有阻挡溶液的挡流板，用于提供剪切力。The reaction device according to claim 10, wherein a baffle for blocking the solution is provided in the reaction kettle for providing shearing force.
  13. 根据权利要求10所述的反应装置，其特征在于，所述反应釜的底部设有放料口，反应完全后，通过放料口将溶液放入抽滤池中，经洗涤、抽滤、烘干得到表面包覆有机聚合物层的用于粉末涂料的珠光颜料。The reaction device according to claim 10, wherein the bottom of the reaction kettle is provided with a discharge port, after the reaction is completed, the solution is put into the suction filter tank through the discharge port, and is washed, filtered, and dried. The pearlescent pigment for powder coating with the surface coated with an organic polymer layer is obtained by drying.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117247689A (en) * 2023-08-25 2023-12-19 广东华江粉末科技有限公司 Preparation method of sand grain metal powder coating
CN117624942A (en) * 2023-12-05 2024-03-01 广西七色珠光材料股份有限公司 Titanium-free silver pearlescent pigment, and preparation method and application thereof

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114539808A (en) * 2022-03-03 2022-05-27 河南凌宝新材料科技有限公司 High-dispersity pearlescent pigment and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006092443A1 (en) * 2005-03-03 2006-09-08 Grillo-Werke Ag Surface-modified zinc oxide particles
CN1923908A (en) * 2005-09-03 2007-03-07 林一中 Dustless pearlescent pigment
CN101591502A (en) * 2008-05-30 2009-12-02 比亚迪股份有限公司 A kind of polyurethane coating and preparation method thereof
CN103919693A (en) * 2014-03-26 2014-07-16 上海得高实业有限公司 Water dispersible powder syrup for oleophylic treatment and product applying powder syrup
CN107021516A (en) * 2017-05-24 2017-08-08 福建鸿丰纳米科技有限公司 The method of nano-calcium carbonate high pressure saponification wet-process activation
CN206642714U (en) * 2017-03-07 2017-11-17 江西华明纳米碳酸钙有限公司 A kind of super fine calcium carbonate preparation coats kettle with modified calcium
CN206751718U (en) * 2017-05-24 2017-12-15 福建鸿丰纳米科技有限公司 The device of nano-calcium carbonate high pressure saponification wet-process activation

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7338995B2 (en) * 2004-03-06 2008-03-04 E.I. Du Pont De Nemours And Company Titanium dioxide—containing polymers and films with reduced melt fracture
CN101601632B (en) * 2009-06-16 2012-02-22 苏州和茂生物技术有限公司 Application of composition containing 20(S)-protopanaxadiol in preparing cosmetic for caring skin
CN201482482U (en) * 2009-08-27 2010-05-26 浙江华友钴业股份有限公司 Device of composite powder material
WO2013159098A1 (en) * 2012-04-20 2013-10-24 Valspar Sourcing, Inc. Method for making titanium dioxide pigment grind dispersion and paint
AU2014290450B2 (en) * 2013-07-19 2018-03-29 Swimc Llc Polymer-encapsulated pigment particle
CN107400383B (en) * 2016-05-19 2019-08-02 福建坤彩材料科技股份有限公司 One kind being directly used in electrostatic powder coating pearlescent pigment and preparation method thereof
CN108410015B (en) * 2018-02-09 2020-01-21 林一中 Special flow-mark-free pearlescent pigment for plastics and preparation method thereof
CN108948850A (en) * 2018-07-16 2018-12-07 清远市绚淳环保新材料有限公司 A kind of aqueous copper gold pigment and preparation method thereof
CN110256875B (en) * 2019-06-27 2021-01-15 广西福宝信科技有限公司 Composite modifier capable of improving oxygen index and application method of composite modifier in preparation of modified red mud for coating
CN110183896A (en) * 2019-06-27 2019-08-30 广西福宝信科技有限公司 Technique red mud modified composite modifier and its be surface-treated in coating filling with red mud

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006092443A1 (en) * 2005-03-03 2006-09-08 Grillo-Werke Ag Surface-modified zinc oxide particles
CN1923908A (en) * 2005-09-03 2007-03-07 林一中 Dustless pearlescent pigment
CN101591502A (en) * 2008-05-30 2009-12-02 比亚迪股份有限公司 A kind of polyurethane coating and preparation method thereof
CN103919693A (en) * 2014-03-26 2014-07-16 上海得高实业有限公司 Water dispersible powder syrup for oleophylic treatment and product applying powder syrup
CN206642714U (en) * 2017-03-07 2017-11-17 江西华明纳米碳酸钙有限公司 A kind of super fine calcium carbonate preparation coats kettle with modified calcium
CN107021516A (en) * 2017-05-24 2017-08-08 福建鸿丰纳米科技有限公司 The method of nano-calcium carbonate high pressure saponification wet-process activation
CN206751718U (en) * 2017-05-24 2017-12-15 福建鸿丰纳米科技有限公司 The device of nano-calcium carbonate high pressure saponification wet-process activation

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117247689A (en) * 2023-08-25 2023-12-19 广东华江粉末科技有限公司 Preparation method of sand grain metal powder coating
CN117247689B (en) * 2023-08-25 2024-04-16 广东华江粉末科技有限公司 Preparation method of sand grain metal powder coating
CN117624942A (en) * 2023-12-05 2024-03-01 广西七色珠光材料股份有限公司 Titanium-free silver pearlescent pigment, and preparation method and application thereof

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