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CN108329793A - A kind of graphene is modified rust resisting pigment anti-corrosion primer and preparation method thereof - Google Patents

A kind of graphene is modified rust resisting pigment anti-corrosion primer and preparation method thereof Download PDF

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CN108329793A
CN108329793A CN201711300962.9A CN201711300962A CN108329793A CN 108329793 A CN108329793 A CN 108329793A CN 201711300962 A CN201711300962 A CN 201711300962A CN 108329793 A CN108329793 A CN 108329793A
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graphene
pigment
preparation
slurry
antirust pigment
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CN108329793B (en
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谭伟民
薛鹏
胡秀东
邹功文
郁飞
狄志刚
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CNOOC Energy Technology and Services Ltd
CNOOC Changzhou EP Coating Co Ltd
CNOOC Changzhou Paint and Coatings Industry Research Institute Co Ltd
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CNOOC Energy Technology and Services Ltd
CNOOC Changzhou EP Coating Co Ltd
CNOOC Changzhou Paint and Coatings Industry Research Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
    • C09D5/082Anti-corrosive paints characterised by the anti-corrosive pigment
    • C09D5/084Inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
    • C09D5/10Anti-corrosive paints containing metal dust
    • C09D5/103Anti-corrosive paints containing metal dust containing Al
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0812Aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2272Ferric oxide (Fe2O3)
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
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  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a kind of graphenes to be modified rust resisting pigment anti-corrosion primer, is prepared by following weight percent composition:Epoxy resin 18~30%, graphene slurry 5~15%, flake pigment 3~10%, rust resisting pigment 20~30%, filler 10~20%, dispersing aid 0.4~0.8%, diluent 20~30%.Its versatility with good mechanical performance and to a variety of base materials has good adhesive force for the carbon steel base material of zinc-plated, chromium plating and mild abrasion, and has excellent antiseptic property.

Description

一种石墨烯改性防锈颜料防腐底漆及其制备方法A kind of graphene modified antirust pigment anticorrosion primer and preparation method thereof

技术领域technical field

本发明涉及纳米聚合物复合材料技术领域,特别是,涉及一种石墨烯改性防锈颜料防腐底漆及其制备方法。The invention relates to the technical field of nano-polymer composite materials, in particular to a graphene-modified anti-rust pigment anti-corrosion primer and a preparation method thereof.

背景技术Background technique

环氧铁红底漆一种传统的腐蚀防护的涂料,对铁及其合金具有一定的防腐蚀效果。然而由于其构成材料的防腐效能限制,实际的防护效果并不突出,如何提高防腐性能是本领域亟需解决的技术问题。Epoxy iron red primer is a traditional corrosion protection coating, which has a certain anti-corrosion effect on iron and its alloys. However, due to the limited anti-corrosion performance of its constituent materials, the actual protection effect is not outstanding. How to improve the anti-corrosion performance is a technical problem that needs to be solved urgently in this field.

发明内容Contents of the invention

为了克服现有技术的不足,本发明的目的在于提供一种石墨烯改性防锈颜料防腐底漆,具有良好的机械性能以及对多种基材的通用性,对于镀锌、镀铬及轻度打磨的碳钢基材具有良好的附着力,且具有优异的防腐性能。In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a graphene modified antirust pigment anticorrosion primer, which has good mechanical properties and versatility to various substrates, and is suitable for galvanizing, chrome plating and mild Good adhesion to ground carbon steel substrates and excellent corrosion protection.

为解决上述问题,本发明所采用的技术方案如下:In order to solve the above problems, the technical scheme adopted in the present invention is as follows:

一种石墨烯改性防锈颜料防腐底漆,由以下重量百分比组分制备而成:A kind of graphene modified antirust pigment anticorrosion primer, is prepared from following components by weight percentage:

优选的,所述环氧树脂为E-44型环氧树脂、E-20型环氧树脂、E-02型环氧树脂中任一种或几种。Preferably, the epoxy resin is any one or more of E-44 epoxy resin, E-20 epoxy resin, and E-02 epoxy resin.

优选的,所述片状颜料为云母粉、玻璃鳞片、片状铝粉中的任一种或两种;所述防锈颜料为铁红、锌黄、锶黄中的任一种或几种。Preferably, the flake pigment is any one or both of mica powder, glass flakes, and flake aluminum powder; the antirust pigment is any one or more of iron red, zinc yellow, and strontium yellow .

优选的,所述填料为滑石粉、立德粉、沉淀硫酸钡中的任一种或几种。Preferably, the filler is any one or more of talcum powder, lithopone, and precipitated barium sulfate.

优选的,所述防沉助剂为有机膨润土、气相二氧化硅中的任一种或几种。Preferably, the anti-sedimentation aid is any one or more of organic bentonite and fumed silica.

优选的,所述稀释剂为二甲苯、丙二醇甲醚醋酸酯、丁醇中任一种或几种。Preferably, the diluent is any one or more of xylene, propylene glycol methyl ether acetate, and butanol.

优选的,所述石墨烯浆料由石墨烯粉末、分散剂、二甲苯和丁醇组成,石墨烯固体含量为10%。Preferably, the graphene slurry is composed of graphene powder, dispersant, xylene and butanol, and the graphene solid content is 10%.

优选的,所述石墨烯浆料中,石墨烯粉末为3~10层高纯石墨烯粉末,所述分散剂为7163A型分散剂,所述二甲苯和丁醇的体积比为4:1。Preferably, in the graphene slurry, the graphene powder is 3-10 layers of high-purity graphene powder, the dispersant is 7163A dispersant, and the volume ratio of xylene and butanol is 4:1.

本发明还涉及一种石墨烯改性防锈颜料防腐底漆的制备方法,包括:The present invention also relates to a preparation method of graphene modified antirust pigment anticorrosion primer, comprising:

S101.石墨烯浆料的准备:将分散剂加入二甲苯和丁醇组成的混合溶剂中并搅拌均匀,然后加入石墨烯粉末,搅拌后超声波分散,即得;S101. Preparation of graphene slurry: add the dispersant to a mixed solvent composed of xylene and butanol and stir evenly, then add graphene powder, and ultrasonically disperse after stirring to obtain the product;

S102.其它组分准备:按照配比准备环氧树脂、石墨烯浆料、片状颜料、防锈颜料、填料、防沉助剂和稀释剂;S102. Preparation of other components: prepare epoxy resin, graphene slurry, flake pigment, antirust pigment, filler, anti-sedimentation aid and diluent according to the proportion;

S103.混合制备:将环氧树脂与稀释剂混合均匀后,加入片状颜料、防锈颜料、填料、防沉助剂、石墨烯浆料并搅拌均匀,研磨至细度达到40μm以下,过滤即得。S103. Mixing preparation: After mixing epoxy resin and diluent evenly, add flake pigments, anti-rust pigments, fillers, anti-sedimentation aids, graphene slurry and stir evenly, grind until the fineness reaches below 40 μm, and filter have to.

进一步的,所述步骤S101中,石墨烯浆料的准备具体为:将分散剂加入二甲苯和丁醇组成的混合溶剂中并搅拌均匀,然后加入石墨烯粉末,搅拌0.5~1h,搅拌速度为250~350r/min,再以超声波分散仪进行分散,分散条件为超声8s、间歇20s、超声总时间为2h,分散时以循环水冷却,使浆料温度保持在25±3℃。Further, in the step S101, the preparation of the graphene slurry is as follows: adding the dispersant to the mixed solvent composed of xylene and butanol and stirring evenly, then adding the graphene powder, stirring for 0.5-1 h, and the stirring speed is 250~350r/min, and then disperse with an ultrasonic disperser. The dispersing conditions are ultrasonic 8s, intermittent 20s, and the total ultrasonic time is 2h. When dispersing, it is cooled by circulating water to keep the slurry temperature at 25±3°C.

相比现有技术,本发明的有益效果在于:Compared with the prior art, the beneficial effects of the present invention are:

1、本发明利用对石墨烯预分散制备石墨烯浆料,解决了石墨烯较易团聚、分散困难、分散稳定性不佳等问题,保证了石墨烯改性防锈颜料防腐底漆良好的稳定性;1. The present invention utilizes the pre-dispersion of graphene to prepare graphene slurry, which solves the problems of easy agglomeration of graphene, difficulty in dispersion, poor dispersion stability, etc., and ensures the good stability of graphene modified antirust pigment anticorrosion primer sex;

2、本发明利用石墨烯优异的机械性能实现对涂层的增强增韧,提高了涂层的机械性能;2. The present invention utilizes the excellent mechanical properties of graphene to enhance and toughen the coating, improving the mechanical properties of the coating;

3、本发明利用大片状颜料和小片状纳米材料石墨烯之间的空隙互补、相互填充,形成“迷宫效应”,增加涂层对腐蚀介质的阻隔屏障能力,从而提高涂料的防腐性能;3. The present invention utilizes the gaps between the large flake pigment and the small flake nano-material graphene to complement each other and fill each other to form a "labyrinth effect" to increase the barrier ability of the coating to the corrosive medium, thereby improving the anti-corrosion performance of the coating;

4、本发明石墨烯改性防锈颜料防腐底漆对镀锌、镀铬及轻度打磨的碳钢基材均具有良好的附着力,且具有优异的防腐性能。4. The graphene-modified anti-rust pigment anti-corrosion primer of the present invention has good adhesion to galvanized, chrome-plated and lightly polished carbon steel substrates, and has excellent anti-corrosion performance.

具体实施方式Detailed ways

下面结合具体实施方式对本发明作进一步详细说明。The present invention will be further described in detail below in combination with specific embodiments.

本发明下述实施例中所用的原材料除另有说明外均为市售工业用品,均可通过商业渠道购得。Unless otherwise specified, the raw materials used in the following examples of the present invention are commercially available industrial supplies, which can be purchased through commercial channels.

本发明涉及一种石墨烯改性防锈颜料防腐底漆,由以下重量百分比组分制备而成:环氧树脂18~30%,石墨烯浆料5~15%,片状颜料3~10%,防锈颜料20~30%,填料10~20%,分散助剂0.4~0.8%,稀释剂20~30%。The invention relates to a graphene-modified anti-rust pigment anti-corrosion primer, which is prepared from the following components in weight percent: 18-30% of epoxy resin, 5-15% of graphene slurry, and 3-10% of flake pigment , anti-rust pigment 20-30%, filler 10-20%, dispersing aid 0.4-0.8%, diluent 20-30%.

优选的,所述环氧树脂为E-44型环氧树脂、E-20型环氧树脂、E-02型环氧树脂中任一种或几种。所述片状颜料为云母粉、玻璃鳞片、片状铝粉中的任一种或两种;所述防锈颜料为铁红、锌黄、锶黄中的任一种或几种。所述填料为滑石粉、立德粉、沉淀硫酸钡中的任一种或几种。所述防沉助剂为有机膨润土、气相二氧化硅中的任一种或几种。所述稀释剂为二甲苯、丙二醇甲醚醋酸酯、丁醇中任一种或几种。所述石墨烯浆料由石墨烯粉末、分散剂、二甲苯和丁醇组成,石墨烯固体含量为10%。所述石墨烯浆料中,石墨烯粉末为3~10层高纯石墨烯粉末,所述分散剂为7163A型分散剂,3~10层高纯石墨烯粉末为由中海油常州涂料化工研究院自主合成,7163A型分散剂由中海油常州涂料化工研究院有限公司合成,所述二甲苯和丁醇的体积比为4:1。Preferably, the epoxy resin is any one or more of E-44 epoxy resin, E-20 epoxy resin, and E-02 epoxy resin. The flake pigment is any one or two of mica powder, glass flakes, and flake aluminum powder; the antirust pigment is any one or more of iron red, zinc yellow, and strontium yellow. The filler is any one or more of talcum powder, lithopone, and precipitated barium sulfate. The anti-sedimentation aid is any one or more of organic bentonite and fumed silica. The diluent is any one or more of xylene, propylene glycol methyl ether acetate, and butanol. The graphene slurry is composed of graphene powder, dispersant, xylene and butanol, and the graphene solid content is 10%. In the graphene slurry, the graphene powder is 3-10 layers of high-purity graphene powder, the dispersant is a 7163A type dispersant, and the 3-10 layers of high-purity graphene powder is independently produced by CNOOC Changzhou Paint Chemical Research Institute. Synthesis, 7163A type dispersant was synthesized by CNOOC Changzhou Paint Chemical Research Institute Co., Ltd., the volume ratio of xylene and butanol was 4:1.

实施例1Example 1

制备石墨烯改性防锈颜料防腐底漆Q-1Preparation of graphene modified antirust pigment anticorrosion primer Q-1

1.1、制备石墨烯浆料1.1. Preparation of graphene slurry

将1g 7163A型分散剂加入44g二甲苯和丁醇组成的混合溶剂(二甲苯与丁醇的体积比为4:1)中并搅拌均匀,然后加入5g 3~10层高纯石墨烯粉末,搅拌0.5h,搅拌速度为300r/min,再以超声波分散仪进行分散,分散条件为超声8s、间歇20s、超声总时间为2h,分散时以循环水冷却,使浆料温度保持在25±3℃,制得石墨烯浆料,备用。Add 1g of 7163A type dispersant to a mixed solvent composed of 44g of xylene and butanol (the volume ratio of xylene to butanol is 4:1) and stir evenly, then add 5g of 3-10 layers of high-purity graphene powder, and stir 0.5h, the stirring speed is 300r/min, and then disperse with an ultrasonic disperser. The dispersing conditions are ultrasonic 8s, intermittent 20s, and the total ultrasonic time is 2h. When dispersing, cool with circulating water to keep the slurry temperature at 25±3℃ , to prepare graphene slurry for subsequent use.

表1、石墨烯改性防锈颜料防腐底漆Q-1各组分配比表Table 1. Graphene-modified anti-rust pigment anti-corrosion primer Q-1 distribution ratio of each component

1.2、石墨烯改性防锈颜料防腐底漆Q-1的混合制备1.2. Mixing preparation of graphene-modified anti-rust pigment anti-corrosion primer Q-1

按照表1中配比,将环氧树脂与稀释剂混合均匀后,加入片状颜料、防锈颜料、填料、石墨烯浆料和防沉助剂,开启搅拌,搅拌速度为400r/min,搅拌30min,混合均匀后,用卧式砂磨机进行研磨,研磨至细度达到40μm以下,过120目滤网,即得石墨烯改性防锈颜料防腐底漆Q-1。According to the ratio in Table 1, after mixing the epoxy resin and diluent evenly, add flake pigments, anti-rust pigments, fillers, graphene slurry and anti-sedimentation aids, start stirring, the stirring speed is 400r/min, stir After 30 minutes, after mixing evenly, use a horizontal sand mill to grind until the fineness reaches below 40 μm, and pass through a 120-mesh filter to obtain the graphene-modified anti-rust pigment anti-corrosion primer Q-1.

实施例2Example 2

制备石墨烯改性防锈颜料防腐底漆Q-2Preparation of graphene modified antirust pigment anticorrosion primer Q-2

2.1、制备石墨烯浆料2.1. Preparation of graphene slurry

将1.5g 7163A型分散剂加入43.5g二甲苯和丁醇组成的混合溶剂(二甲苯与丁醇的体积比为4:1)中并搅拌均匀,然后加入5g 3~10层高纯石墨烯粉末,搅拌1h,搅拌速度为250r/min,再以超声波分散仪进行分散,分散条件为超声8s、间歇20s、超声总时间为2h,分散时以循环水冷却,使浆料温度保持在25±3℃,制得石墨烯浆料,备用。Add 1.5g of 7163A type dispersant to a mixed solvent composed of 43.5g of xylene and butanol (the volume ratio of xylene to butanol is 4:1) and stir evenly, then add 5g of 3-10 layers of high-purity graphene powder , stirred for 1h, the stirring speed was 250r/min, and then dispersed with an ultrasonic disperser. The dispersion conditions were ultrasonic 8s, intermittent 20s, and the total ultrasonic time was 2h. When dispersing, it was cooled by circulating water to keep the slurry temperature at 25±3 ℃, the graphene slurry was prepared and set aside.

表2、石墨烯改性防锈颜料防腐底漆Q-2各组分配比表Table 2. Graphene modified anti-rust pigment anti-corrosion primer Q-2 distribution ratio of each component

2.2、石墨烯改性防锈颜料防腐底漆Q-2的混合制备2.2. Mixing preparation of graphene-modified anti-rust pigment anti-corrosion primer Q-2

按照表2中配比,将环氧树脂与稀释剂混合均匀后,加入片状颜料、防锈颜料、填料、石墨烯浆料和防沉助剂,开启搅拌,搅拌速度为400r/min,搅拌30min,混合均匀后,用卧式砂磨机进行研磨,研磨至细度达到40μm以下,过120目滤网,即得石墨烯改性防锈颜料防腐底漆Q-2。According to the ratio in Table 2, after mixing the epoxy resin and diluent evenly, add flake pigments, anti-rust pigments, fillers, graphene slurry and anti-sedimentation aids, start stirring, the stirring speed is 400r/min, stir After 30 minutes, after mixing evenly, grind with a horizontal sand mill until the fineness reaches below 40 μm, and pass through a 120-mesh filter to obtain the graphene-modified anti-rust pigment anti-corrosion primer Q-2.

实施例3Example 3

制备石墨烯改性防锈颜料防腐底漆Q-3Preparation of graphene modified antirust pigment anticorrosion primer Q-3

3.1、制备石墨烯浆料3.1. Preparation of graphene slurry

将0.5g 7163A型分散剂加入44.5g二甲苯和丁醇组成的混合溶剂(二甲苯与丁醇的体积比为4:1)中并搅拌均匀,然后加入5g 3~10层高纯石墨烯粉末,搅拌1h,搅拌速度为350r/min,再以超声波分散仪进行分散,分散条件为超声8s、间歇20s、超声总时间为2h,分散时以循环水冷却,使浆料温度保持在25±3℃,制得石墨烯浆料,备用。Add 0.5g of 7163A type dispersant to 44.5g of mixed solvent composed of xylene and butanol (the volume ratio of xylene to butanol is 4:1) and stir evenly, then add 5g of 3-10 layers of high-purity graphene powder , stirred for 1h, the stirring speed was 350r/min, and then dispersed with an ultrasonic disperser. The dispersion conditions were ultrasonic 8s, intermittent 20s, and the total ultrasonic time was 2h. When dispersing, it was cooled by circulating water to keep the slurry temperature at 25±3 ℃, the graphene slurry was prepared and set aside.

表3、石墨烯改性防锈颜料防腐底漆Q-3各组分配比表Table 3. Graphene modified anti-rust pigment anti-corrosion primer Q-3 distribution ratio of each component

3.2、石墨烯改性防锈颜料防腐底漆Q-3的混合制备3.2. Mixing preparation of graphene-modified anti-rust pigment anti-corrosion primer Q-3

按照表3中配比,将环氧树脂与稀释剂混合均匀后,加入片状颜料、防锈颜料、填料、石墨烯浆料和防沉助剂,开启搅拌,搅拌速度为400r/min,搅拌30min,混合均匀后,用卧式砂磨机进行研磨,研磨至细度达到40μm以下,过120目滤网,即得石墨烯改性防锈颜料防腐底漆Q-3。According to the ratio in Table 3, after mixing the epoxy resin and diluent evenly, add flake pigments, anti-rust pigments, fillers, graphene slurry and anti-sedimentation aids, start stirring, the stirring speed is 400r/min, stir After 30 minutes, after mixing evenly, grind with a horizontal sand mill until the fineness reaches below 40 μm, and pass through a 120-mesh filter to obtain the graphene-modified anti-rust pigment anti-corrosion primer Q-3.

实施例4Example 4

制备石墨烯改性防锈颜料防腐底漆Q-4Preparation of graphene modified antirust pigment anticorrosion primer Q-4

4.1、制备石墨烯浆料4.1. Preparation of graphene slurry

将1g 7163A型分散剂加入44g二甲苯和丁醇组成的混合溶剂(二甲苯与丁醇的体积比为4:1)中并搅拌均匀,然后加入5g 3~10层高纯石墨烯粉末,搅拌1h,搅拌速度为250r/min,再以超声波分散仪进行分散,分散条件为超声8s、间歇20s、超声总时间为2h,分散时以循环水冷却,使浆料温度保持在25±3℃,制得石墨烯浆料,备用。Add 1g of 7163A type dispersant to a mixed solvent composed of 44g of xylene and butanol (the volume ratio of xylene to butanol is 4:1) and stir evenly, then add 5g of 3-10 layers of high-purity graphene powder, and stir 1h, the stirring speed is 250r/min, and then disperse with an ultrasonic disperser. The dispersing conditions are ultrasonic 8s, intermittent 20s, and the total ultrasonic time is 2h. When dispersing, it is cooled by circulating water to keep the slurry temperature at 25±3°C. Make graphene slurry, standby.

表4、石墨烯改性防锈颜料防腐底漆Q-4各组分配比表Table 4. Graphene-modified anti-rust pigment anti-corrosion primer Q-4 distribution ratio of each component

4.2、石墨烯改性防锈颜料防腐底漆Q-4的混合制备4.2. Mixing preparation of graphene-modified anti-rust pigment anti-corrosion primer Q-4

按照表4中配比,将环氧树脂与稀释剂混合均匀后,加入片状颜料、防锈颜料、填料、石墨烯浆料和防沉助剂,开启搅拌,搅拌速度为400r/min,搅拌30min,混合均匀后,用卧式砂磨机进行研磨,研磨至细度达到40μm以下,过120目滤网,即得石墨烯改性防锈颜料防腐底漆Q-4。According to the ratio in Table 4, after mixing the epoxy resin and the diluent evenly, add flake pigments, anti-rust pigments, fillers, graphene slurry and anti-sedimentation aids, start stirring, the stirring speed is 400r/min, and stir After 30 minutes, after mixing evenly, grind with a horizontal sand mill until the fineness reaches below 40 μm, and pass through a 120-mesh filter to obtain the graphene-modified anti-rust pigment anti-corrosion primer Q-4.

实施例5Example 5

制备石墨烯改性防锈颜料防腐底漆Q-5Preparation of graphene modified antirust pigment anticorrosion primer Q-5

5.1、制备石墨烯浆料5.1. Preparation of graphene slurry

将1g 7163A型分散剂加入44g二甲苯和丁醇组成的混合溶剂(二甲苯与丁醇的体积比为4:1)中并搅拌均匀,然后加入5g 3~10层高纯石墨烯粉末,搅拌1h,搅拌速度为350r/min,再以超声波分散仪进行分散,分散条件为超声8s、间歇20s、超声总时间为2h,分散时以循环水冷却,使浆料温度保持在25±3℃,制得石墨烯浆料,备用。Add 1g of 7163A type dispersant to a mixed solvent composed of 44g of xylene and butanol (the volume ratio of xylene to butanol is 4:1) and stir evenly, then add 5g of 3-10 layers of high-purity graphene powder, and stir 1h, the stirring speed is 350r/min, and then disperse with an ultrasonic disperser. The dispersing conditions are ultrasonic 8s, intermittent 20s, and the total ultrasonic time is 2h. When dispersing, it is cooled by circulating water to keep the temperature of the slurry at 25±3°C. Make graphene slurry, standby.

表5、石墨烯改性防锈颜料防腐底漆Q-5各组分配比表Table 5. Graphene-modified anti-rust pigment anti-corrosion primer Q-5 distribution ratio of each component

5.2、石墨烯改性防锈颜料防腐底漆Q-5的混合制备5.2. Mixing preparation of graphene-modified anti-rust pigment anti-corrosion primer Q-5

按照表5中配比,将环氧树脂与稀释剂混合均匀后,加入片状颜料、防锈颜料、填料、石墨烯浆料和防沉助剂,开启搅拌,搅拌速度为400r/min,搅拌30min,混合均匀后,用卧式砂磨机进行研磨,研磨至细度达到40μm以下,过120目滤网,即得石墨烯改性防锈颜料防腐底漆Q-5。According to the ratio in Table 5, after mixing the epoxy resin and diluent evenly, add flake pigments, anti-rust pigments, fillers, graphene slurry and anti-sedimentation aids, start stirring, the stirring speed is 400r/min, stir After 30 minutes, after mixing evenly, grind with a horizontal sand mill until the fineness reaches below 40 μm, and pass through a 120-mesh filter to obtain the graphene-modified anti-rust pigment anti-corrosion primer Q-5.

实施例6Example 6

性能对比试验Performance comparison test

采用本发明实施例1~5制备的石墨烯改性防锈颜料防腐底漆Q-1~Q-5和一种市售普通环氧铁红底漆分别制备膜厚为30±5μm的漆膜并进行检测,获得检测数据对比表6如下:The graphene-modified antirust pigment anticorrosion primer Q-1~Q-5 prepared by the embodiments of the present invention 1~5 and a kind of commercially available common epoxy iron red primer respectively prepare a paint film with a film thickness of 30 ± 5 μm And carry out detection, obtain the detection data comparison table 6 as follows:

表6、检测数据对比表Table 6. Test data comparison table

结合上表6可以看出,在相同漆膜厚度的条件下,本发明中制备方法获得的通用型石墨烯改性环氧防腐底漆抗冲击强度优于市售环氧铁红底漆,耐盐雾性远远优于市售环氧铁红底漆,具有良好的推广前景。Can find out in conjunction with above table 6, under the condition of same paint film thickness, the general-purpose graphene-modified epoxy anticorrosion primer that preparation method obtains in the present invention has impact strength better than commercially available epoxy iron red primer, resistant to The salt spray property is far superior to the commercial epoxy iron red primer, and has a good promotion prospect.

对本领域的技术人员来说,可根据以上描述的技术方案以及构思,做出其它各种相应的改变以及形变,而所有的这些改变以及形变都应该属于本发明权利要求的保护范围之内。Those skilled in the art can make various other corresponding changes and deformations according to the above-described technical solutions and concepts, and all these changes and deformations should fall within the protection scope of the claims of the present invention.

Claims (10)

1.一种石墨烯改性防锈颜料防腐底漆,其特征在于,由以下重量百分比组分制备而成:1. a graphene modified antirust pigment anticorrosion primer, is characterized in that, is prepared from by following weight percent component: 2.如权利要求1所述的石墨烯改性防锈颜料防腐底漆,其特征在于,所述环氧树脂为E-44型环氧树脂、E-20型环氧树脂、E-02型环氧树脂中任一种或几种。2. graphene modified antirust pigment anticorrosion primer as claimed in claim 1, is characterized in that, described epoxy resin is E-44 type epoxy resin, E-20 type epoxy resin, E-02 type Any one or several of epoxy resins. 3.如权利要求1所述的石墨烯改性防锈颜料防腐底漆,其特征在于,所述片状颜料为云母粉、玻璃鳞片、片状铝粉中的任一种或两种;所述防锈颜料为铁红、锌黄、锶黄中的任一种或几种。3. Graphene modified antirust pigment anticorrosion primer as claimed in claim 1, is characterized in that, described flaky pigment is any one or both in mica powder, glass flake, flaky aluminum powder; The anti-rust pigment is any one or more of iron red, zinc yellow and strontium yellow. 4.如权利要求1所述的石墨烯改性防锈颜料防腐底漆,其特征在于,所述填料为滑石粉、立德粉、沉淀硫酸钡中的任一种或几种。4. Graphene modified antirust pigment anticorrosion primer as claimed in claim 1, is characterized in that, described filler is any one or more in talcum powder, lithopone, precipitated barium sulfate. 5.如权利要求1所述的石墨烯改性防锈颜料防腐底漆,其特征在于,所述防沉助剂为有机膨润土、气相二氧化硅中的任一种或几种。5. graphene modified antirust pigment anticorrosion primer as claimed in claim 1, is characterized in that, described anti-sedimentation aid is any one or more in organic bentonite, fumed silica. 6.如权利要求1所述的石墨烯改性防锈颜料防腐底漆,其特征在于,所述稀释剂为二甲苯、丙二醇甲醚醋酸酯、丁醇中任一种或几种。6. Graphene modified antirust pigment anticorrosion primer as claimed in claim 1, is characterized in that, described diluent is any one or more in xylene, propylene glycol methyl ether acetate, butanol. 7.如权利要求1~6任一项所述的石墨烯改性防锈颜料防腐底漆,其特征在于,所述石墨烯浆料由石墨烯粉末、分散剂、二甲苯和丁醇组成,石墨烯固体含量为10%。7. the graphene modified antirust pigment anticorrosion primer as claimed in any one of claims 1 to 6, is characterized in that, described graphene slurry is made up of graphene powder, dispersant, xylene and butanol, The graphene solids content was 10%. 8.如权利要求7所述的石墨烯改性防锈颜料防腐底漆,其特征在于,所述石墨烯浆料中,石墨烯粉末为3~10层高纯石墨烯粉末,所述分散剂为7163A型分散剂,所述二甲苯和丁醇的体积比为4:1。8. graphene modified antirust pigment anticorrosion primer as claimed in claim 7, is characterized in that, in described graphene slurry, graphene powder is 3~10 layers of high-purity graphene powders, and described dispersant It is 7163A type dispersant, the volume ratio of xylene and butanol is 4:1. 9.权利要求8所述石墨烯改性防锈颜料防腐底漆的制备方法,包括:9. the preparation method of graphene modified antirust pigment anticorrosion primer described in claim 8, comprising: S101.石墨烯浆料的准备:将分散剂加入二甲苯和丁醇组成的混合溶剂中并搅拌均匀,然后加入石墨烯粉末,搅拌后超声波分散,即得;S101. Preparation of graphene slurry: add the dispersant to a mixed solvent composed of xylene and butanol and stir evenly, then add graphene powder, and ultrasonically disperse after stirring to obtain the product; S102.其它组分准备:按照配比准备环氧树脂、石墨烯浆料、片状颜料、防锈颜料、填料、防沉助剂和稀释剂;S102. Preparation of other components: prepare epoxy resin, graphene slurry, flake pigment, antirust pigment, filler, anti-sedimentation aid and diluent according to the proportion; S103.混合制备:将环氧树脂与稀释剂混合均匀后,加入片状颜料、防锈颜料、填料、防沉助剂、石墨烯浆料并搅拌均匀,研磨至细度达到40μm以下,过滤即得。S103. Mixing preparation: After mixing epoxy resin and diluent evenly, add flake pigments, anti-rust pigments, fillers, anti-sedimentation aids, graphene slurry and stir evenly, grind until the fineness reaches below 40 μm, and filter have to. 10.如权利要求9所述的石墨烯改性防锈颜料防腐底漆的制备方法,其特征在于,所述步骤S101中,石墨烯浆料的准备具体为:将分散剂加入二甲苯和丁醇组成的混合溶剂中并搅拌均匀,然后加入石墨烯粉末,搅拌0.5~1h,搅拌速度为250~350r/min,再以超声波分散仪进行分散,分散条件为超声8s、间歇20s、超声总时间为2h,分散时以循环水冷却,使浆料温度保持在25±3℃。10. the preparation method of graphene modified antirust pigment anticorrosion primer as claimed in claim 9, it is characterized in that, in described step S101, the preparation of graphene slurry is specifically: adding dispersant to xylene and butyl Mixed solvent composed of alcohol and stir evenly, then add graphene powder, stir for 0.5-1h, stirring speed is 250-350r/min, and then disperse with ultrasonic disperser, the dispersion conditions are ultrasonic 8s, intermittent 20s, total ultrasonic time 2h, cooling with circulating water during dispersion to keep the slurry temperature at 25±3°C.
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