CN1328339C - FBE pnenolic aldehyde modified epoxy powder coating and its preparation method - Google Patents
FBE pnenolic aldehyde modified epoxy powder coating and its preparation method Download PDFInfo
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Abstract
FBE酚醛改性环氧粉末涂料及其制备方法，按质量百分数计：酚醛改性环氧树脂25%～50%，E-12环氧树脂0%～25%，酚醛改性固化剂10%～15%，流平剂0.5%～2.0%，脱气剂0.2%～0.3%，固化促进剂0.02%～0.05%，中铬黄0.5%，酞菁蓝0.05%，钛白粉2.5%，沉淀硫酸钡25%～30%，其制备方法为：将酚醛改性环氧树脂、E-12环氧树脂、酚醛改性固化剂、流平剂高速混合1～2分钟，加入配方量的脱气剂、固化促进剂、中铬黄、酞菁蓝、钛白粉、沉淀硫酸钡混合3～5分钟；然后将混合物料加入挤出机熔融挤出，融物料经压片机压片，经冷却破碎送入磨粉机中粉碎分级，通过旋风分离器将过细粉末分离，经旋风分离的粉末筛分得到产品。FBE phenolic modified epoxy powder coating and its preparation method, by mass percentage: 25% to 50% of phenolic modified epoxy resin, 0% to 25% of E-12 epoxy resin, 10% to 10% of phenolic modified curing agent 15%, leveling agent 0.5%~2.0%, degassing agent 0.2%~0.3%, curing accelerator 0.02%~0.05%, medium chrome yellow 0.5%, phthalocyanine blue 0.05%, titanium dioxide 2.5%, precipitated barium sulfate 25% to 30%, the preparation method is: mix phenolic modified epoxy resin, E-12 epoxy resin, phenolic modified curing agent, and leveling agent at high speed for 1 to 2 minutes, add degassing agent, Curing accelerator, medium chrome yellow, phthalocyanine blue, titanium dioxide, and precipitated barium sulfate were mixed for 3 to 5 minutes; Pulverize and classify in the mill, separate the superfine powder through the cyclone separator, and sieve the powder separated by the cyclone to obtain the product.
Description
技术领域technical field
本发明涉及一种输油管道防腐用熔结环氧粉末涂料及其制备方法，特别是酚醛改性环氧粉末涂料的工艺方法。The invention relates to a fusion bonded epoxy powder coating for anticorrosion of oil pipelines and a preparation method thereof, in particular to a process method of phenolic modified epoxy powder coating.
背景技术Background technique
FBE环氧粉末涂料是一种不含溶剂、以粉末状态喷涂，并加热熔结成膜的新型防腐涂料，在对管道的喷涂、熔结过程中不存在污染。FBE epoxy powder coating is a new type of anti-corrosion coating that does not contain solvent, is sprayed in powder state, and is heated and fused to form a film. There is no pollution in the process of spraying and sintering of pipelines.
埋地钢管防腐的主要手段是防腐层加阴极保护，防腐层有沥青类防腐层、胶带、夹克、环氧粉末、FBE环氧粉末和三层聚乙烯(三层PE)等类型。国外长距离输油(气)管道的防腐层材料主要为FBE环氧粉末、三层聚乙烯，油田内部主要集输油(气)管道的防腐层材料也多为FBE环氧粉末和三层聚乙烯。与其他防腐层相比，FBE环氧粉末涂料具有附着力强，耐各种介质腐蚀，工艺、材料技术成熟，作业效率高，质量易于控制和检测补口简便、可靠的优点，因此在输油管线防腐中广泛采用。The main anti-corrosion method for buried steel pipes is anti-corrosion layer plus cathodic protection. The anti-corrosion layer includes asphalt anti-corrosion layer, tape, jacket, epoxy powder, FBE epoxy powder and three-layer polyethylene (three-layer PE). The anti-corrosion layer materials of foreign long-distance oil (gas) pipelines are mainly FBE epoxy powder and three-layer polyethylene. vinyl. Compared with other anti-corrosion coatings, FBE epoxy powder coating has the advantages of strong adhesion, corrosion resistance to various media, mature technology and material technology, high operating efficiency, easy quality control, easy and reliable inspection and repair, so it is used in oil pipelines. Widely used in anticorrosion.
CN1511903A中公开了一种耐酸型熔融结合环氧改性粉末涂料，由E-12环氧树脂、固化剂双氰胺+醚唑、改性剂热固性酚醛树脂和填料SiO2组成，可耐36.5％的盐酸腐蚀。Disclosed in CN1511903A is an acid-resistant type fusion-bonded epoxy-modified powder coating, which is composed of E-12 epoxy resin, curing agent dicyandiamide+etherazole, modifier thermosetting phenolic resin and filler SiO2 , which can withstand 36.5% hydrochloric acid corrosion.
CN1511904A中公开了一种耐海水型熔融结合环氧改性粉末涂料，由E-12环氧树脂、固化剂双氰胺、改性剂超细TiO2和填料CaCO3、BaSO4组成，可耐饱和NaCl或KCl水溶液。Disclosed in CN1511904A is a seawater-resistant type fusion-bonding epoxy-modified powder coating, which is composed of E-12 epoxy resin, curing agent dicyandiamide, modifier superfine TiO 2 and filler CaCO 3 , BaSO 4 , which can withstand Saturated NaCl or KCl aqueous solution.
然而现有FBE环氧粉末涂料往往采用E-12环氧树脂-双氰胺体系，存在交联程度低、流平性差的缺点，形成的防腐涂层难以满足埋地输油管道日益提高的重防腐要求。However, the existing FBE epoxy powder coatings often use E-12 epoxy resin-dicyandiamide system, which has the disadvantages of low cross-linking degree and poor leveling, and the formed anti-corrosion coating cannot meet the increasing heavy-duty anti-corrosion requirements of buried oil pipelines. Require.
发明内容Contents of the invention
本发明可通过如下措施来实现：The present invention can be realized by following measures:
FBE酚醛改性环氧粉末涂料的配方为：按质量百分数计The formula of FBE phenolic modified epoxy powder coating is: by mass percentage
酚醛改性环氧树脂 25％～50％Phenolic modified epoxy resin 25%～50%
环氧树脂E-12 0％～25％Epoxy resin E-12 0%～25%
酚醛改性固化剂 10％～15％Phenolic modified curing agent 10%～15%
流平剂 0.5％～2.0％Leveling agent 0.5%～2.0%
脱气剂 0.2％～0.3％Degassing agent 0.2%～0.3%
固化促进剂 0.02％～0.05％Curing Accelerator 0.02%～0.05%
中铬黄 0.5％Medium chrome yellow 0.5%
酞菁蓝 0.05％Phthalocyanine Blue 0.05%
钛白粉 2.5％Titanium dioxide 2.5%
沉淀硫酸钡 25％～30％。Precipitated barium sulfate 25% to 30%.
按上述配方，本发明的FBE酚醛改性环氧粉末涂料的制备方法为：Press above-mentioned prescription, the preparation method of FBE phenolic modified epoxy powder coating of the present invention is:
(1)将酚醛改性环氧树脂、环氧树脂E-12、酚醛改性固化剂、流平剂高速混合1～2分钟，加入配方量的脱气剂、固化促进剂、中铬黄、酞菁蓝、钛白粉、沉淀硫酸钡混合3～5分钟；(1) Mix phenolic modified epoxy resin, epoxy resin E-12, phenolic modified curing agent, and leveling agent at high speed for 1 to 2 minutes, and add the degassing agent, curing accelerator, medium chrome yellow, Mix phthalocyanine blue, titanium dioxide, and precipitated barium sulfate for 3 to 5 minutes;
(2)混合物料加入挤出机熔融挤出，料段温度80～92℃，熔融段温度95～105℃，混炼段110～120℃，出料段100～110℃；物料平均滞留时间不超过60秒；(2) The mixed material is put into the extruder to melt and extrude, the temperature of the material section is 80-92°C, the temperature of the melting section is 95-105°C, the mixing section is 110-120°C, and the discharge section is 100-110°C; the average residence time of the material is not more than 60 seconds;
(3)融物料经压片机压片，控制厚度在1～3mm，经冷却破碎送入磨粉机中粉碎分级，通过旋风分离器将过细粉末分离，经旋风分离的粉末筛分得到产品，粒度控制：150μm筛上粉末≤3％，250μm筛上粉末≤0.2％。(3) The melted material is pressed into tablets by a tablet press, and the thickness is controlled at 1-3 mm. After cooling and crushing, it is sent to a mill for pulverization and classification. The superfine powder is separated by a cyclone separator, and the product is obtained by sieving the powder separated by the cyclone. Particle size control: 150μm sieve powder≤3%, 250μm sieve powder≤0.2%.
本发明的优点在于该FBE酚醛改性环氧粉末涂料具有施工工艺良好、交联密度高、耐化学介质性能优异、附着力强、耐磨、耐冷热冲击和光泽高的特点，能满足埋地管道的保护要求，而且具有工艺简单、原料易得等特点，适合大规模工业生产。The advantage of the present invention is that the FBE phenolic modified epoxy powder coating has the characteristics of good construction technology, high crosslinking density, excellent chemical medium resistance, strong adhesion, wear resistance, cold and heat shock resistance and high gloss, and can meet the requirements of buried It is suitable for large-scale industrial production because of its simple process and easy access to raw materials.
本发明FBE酚醛改性环氧粉末涂料采用酚醛改性环氧树脂为基料，其结构示意如图：The FBE phenolic modified epoxy powder coating of the present invention adopts phenolic modified epoxy resin as the base material, and its structure is schematically shown in the figure:
与传统的环氧树脂相比，具有交联活性位多、反应活性高、可高温快速固化的特点，配合酚醛改性固化剂形成的涂膜致密、防腐性能好，而且流平性好、光泽高。Compared with the traditional epoxy resin, it has the characteristics of more cross-linking active sites, high reactivity, and rapid curing at high temperature. The coating film formed with the phenolic modified curing agent is dense, has good anti-corrosion performance, and has good leveling and gloss. high.
本发明涉及具有施工工艺良好、耐化学介质性能优异、附着力强、耐磨、耐冷热冲击的FBE酚醛改性环氧粉末涂料及其制备方法。FBE环氧粉末涂料选用酚醛改性环氧树脂为基料，与酚醛改性固化剂、流平剂、固化促进剂、消泡剂、钛白粉、沉淀硫酸钡、酞菁蓝和中铬黄等通过高速混合、熔融挤出、冷却压片、粉碎分级和筛分等工序得到。The invention relates to a FBE phenolic modified epoxy powder coating with good construction technology, excellent chemical medium resistance, strong adhesion, wear resistance, and cold and heat shock resistance and a preparation method thereof. FBE epoxy powder coatings use phenolic modified epoxy resin as the base material, together with phenolic modified curing agent, leveling agent, curing accelerator, defoamer, titanium dioxide, precipitated barium sulfate, phthalocyanine blue and medium chrome yellow, etc. It is obtained through high-speed mixing, melt extrusion, cooling and pressing, pulverizing, grading and sieving.
具体实施方式Detailed ways
实施例1：Example 1:
本实施例示范了本发明的FBE酚醛改性环氧粉末涂料的制备方法。This embodiment demonstrates the preparation method of the FBE phenolic modified epoxy powder coating of the present invention.
将酚醛改性环氧树脂50.00kg、酚醛改性固化剂10.00kg、流平剂2.00kg加入高速混合机中混合2分钟，加入脱气剂0.28kg、固化促进剂0.02kg、中铬黄0.50kg、酞菁蓝0.05kg、钛白粉2.50kg、沉淀硫酸钡34.65kg，高速混合3分钟，预混合物料加入挤出机熔融挤出，加料段温度88℃，熔融段温度100℃，混炼段110℃，出料段100℃，挤出机转速控制在70rpm，在风冷履带式压片破碎机上压片、冷却、破碎，压片厚度2mm，破碎成5～10mm的薄片，在粉碎磨中经粉碎、分级、旋风分离器分离和筛分得到产品，通过旋风分离除去过细粉末，产品粒度控制：150μm筛上粉末≤3％，250μm筛上粉末≤0.2％。Add 50.00kg of phenolic modified epoxy resin, 10.00kg of phenolic modified curing agent, and 2.00kg of leveling agent into a high-speed mixer and mix for 2 minutes, add 0.28kg of degasser, 0.02kg of curing accelerator, and 0.50kg of medium chrome yellow , Phthalocyanine blue 0.05kg, titanium dioxide 2.50kg, precipitated barium sulfate 34.65kg, mixed at high speed for 3 minutes, the premixed material was added to the extruder to melt and extrude, the temperature of the feeding section was 88°C, the temperature of the melting section was 100°C, and the mixing section was 110°C ℃, the discharge section is 100 ℃, the extruder speed is controlled at 70rpm, the tablet is pressed, cooled and crushed on the air-cooled crawler-type tablet crusher. Grinding, grading, cyclone separator separation and sieving to obtain the product, and cyclone separation to remove superfine powder, product particle size control: 150μm sieve powder ≤ 3%, 250μm sieve powder ≤ 0.2%.
实施例2：Example 2:
FBE酚醛改性环氧粉末涂料的配方如下：The formula of FBE phenolic modified epoxy powder coating is as follows:
酚醛改性环氧树脂 37.50kgPhenolic modified epoxy resin 37.50kg
E-12环氧树脂 12.50kgE-12 Epoxy Resin 12.50kg
酚醛改性固化剂 12.50kgPhenolic modified curing agent 12.50kg
流平剂 1.00kgLeveling agent 1.00kg
脱气剂 0.30kgDegasser 0.30kg
固化促进剂 0.03kgCuring Accelerator 0.03kg
中铬黄 0.50kgMedium Chrome Yellow 0.50kg
酞菁蓝 0.05kgPhthalocyanine blue 0.05kg
钛白粉 2.50kgTitanium dioxide 2.50kg
沉淀硫酸钡 33.12kgPrecipitated barium sulfate 33.12kg
产品粒度控制：150μm筛上粉末≤3％，250μm筛上粉末≤0.2％。Product particle size control: 150 μm sieve powder ≤ 3%, 250 μm sieve powder ≤ 0.2%.
实施例3：Example 3:
FBE酚醛改性环氧粉末涂料的配方如下：The formula of FBE phenolic modified epoxy powder coating is as follows:
酚醛改性环氧树脂 25.00kgPhenolic modified epoxy resin 25.00kg
E-12环氧树脂 25.00kgE-12 epoxy resin 25.00kg
酚醛改性固化剂 15.00kgPhenolic modified curing agent 15.00kg
流平剂 1.70kgLeveling agent 1.70kg
脱气剂 0.20kgDegasser 0.20kg
固化促进剂 0.05kgCuring Accelerator 0.05kg
中铬黄 0.50kgMedium Chrome Yellow 0.50kg
酞菁蓝 0.05kgPhthalocyanine blue 0.05kg
钛白粉 2.50kgTitanium dioxide 2.50kg
沉淀硫酸钡 30.00kgPrecipitated barium sulfate 30.00kg
产品粒度控制：150μm筛上粉末≤3％，250μm筛上粉末≤0.2％。Product particle size control: 150 μm sieve powder ≤ 3%, 250 μm sieve powder ≤ 0.2%.
按实施例制得的FBE酚醛改性环氧粉末涂料可达到的技术指标：The technical index that the FBE phenolic modified epoxy powder coating that makes by embodiment can reach:
a.FBE酚醛改性环氧粉末的性能a. Properties of FBE phenolic modified epoxy powder
项目 质量指标Project Quality Index
外观 色泽均匀，无结块Appearance Uniform color, no agglomeration
固化时间(180℃)/min ≤5Curing time (180℃)/min ≤5
固化时间(180℃)/s ≤90Curing time (180℃)/s ≤90
附着力/级 ≤2Adhesion/grade ≤2
不挥发物含量(％) ≥99.4Non-volatile content (%) ≥99.4
粒度分布(％)Particle size distribution(%)
150μm筛上粉末 ≤3.0150μm sieve powder ≤3.0
250μm筛上粉末 ≤0.2250μm sieve powder ≤0.2
密度(kg/m3) 1300～1500Density (kg/m 3 ) 1300～1500
磁性物含量(％) ≤0.002Magnetic substance content (%) ≤0.002
b.FBE酚醛改性环氧粉末涂层的性能指标b. Performance index of FBE phenolic modified epoxy powder coating
项目 质量指标Project Quality Index
外观 平整，色泽均匀，允许有轻微桔皮Appearance is smooth and even in color, slight orange peel is allowed
24h阴极剥离(mm) ≤424h cathodic disbonding (mm) ≤4
28d阴极剥离(mm) ≤1028d cathodic disbondment (mm) ≤10
断面孔隙率(级) 1～4Cross section porosity (grade) 1～4
粘结面孔隙率(级) 1～4Bonding surface porosity (grade) 1～4
抗3°弯曲 无裂纹3°bending resistance no cracks
抗1.5J冲击 无针孔1.5J impact resistance No pinholes
电气强度(MV/M) ≥30Electric strength (MV/M) ≥30
体积电阻率(Ω·m) 1×1013 Volume resistivity (Ω·m) 1×10 13
附着力(级) 1～3Adhesion (grade) 1～3
耐磨性(L/μm) ≥3Abrasion resistance (L/μm) ≥3
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| CN101531857B (en) * | 2009-04-24 | 2011-02-16 | 江苏欧赛德钢涂有限公司 | Epoxy resin powder paint and application thereof |
| CN102161859A (en) * | 2011-05-27 | 2011-08-24 | 常州市飞扬粉末涂料有限公司 | Modified epoxy heavy-duty anticorrosion powder paint and preparation method thereof |
| CN103131297B (en) * | 2013-02-03 | 2016-03-30 | 安徽伟迈信息技术有限公司 | A kind of powder coating containing trioctyl trimellitate |
| CN103160184A (en) * | 2013-02-20 | 2013-06-19 | 江苏吉福新材料有限公司 | Rapidly-solidified phenolic aldehyde epoxy coating |
| CN103351784A (en) * | 2013-07-19 | 2013-10-16 | 天津瑞远粉末涂料有限公司 | Rolling painting fusion bonded epoxy powder coating and preparation method thereof |
| CN106439263A (en) * | 2016-11-21 | 2017-02-22 | 无锡金顶石油管材配件制造有限公司 | Anti-corrosion petroleum pipeline |
| CN106634431B (en) * | 2016-12-20 | 2019-06-25 | 山东东宏管业股份有限公司 | A kind of clinkery epoxy powder coating and preparation method thereof with super-drainage structure |
| CN108003745A (en) * | 2017-12-01 | 2018-05-08 | 成都信达高分子材料有限公司 | A kind of pure epoxy powdery paints and preparation method thereof |
| CN108084840A (en) * | 2017-12-01 | 2018-05-29 | 成都信达高分子材料有限公司 | A kind of pure epoxy powdery paints and preparation method thereof |
| CN110105842B (en) * | 2019-04-23 | 2021-08-31 | 天津翔盛新材料有限公司 | Special drag-reducing and wax-preventing powder coating for crude oil conveying pipeline and application |
| CN110819157A (en) * | 2019-11-28 | 2020-02-21 | 衡阳科盈钢管有限公司 | Production process of double-layer epoxy powder |
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| 浅谈粉末涂料配方设计问题 南仁植等，现代涂料与涂装 低污染化发展 2004 * |
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