CN105086557B - Doped ferric oxide powder for anti-corrosive paint of epoxy resin and preparation method thereof - Google Patents
Doped ferric oxide powder for anti-corrosive paint of epoxy resin and preparation method thereof Download PDFInfo
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000000843 powder Substances 0.000 title claims abstract description 61
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 23
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 23
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003973 paint Substances 0.000 title abstract 4
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims abstract description 21
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 21
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 19
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004202 carbamide Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims description 22
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 17
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 14
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 14
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 10
- 238000005260 corrosion Methods 0.000 claims description 9
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 7
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 7
- 239000000347 magnesium hydroxide Substances 0.000 claims description 7
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000049 pigment Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 2
- RECVMTHOQWMYFX-UHFFFAOYSA-N oxygen(1+) dihydride Chemical compound [OH2+] RECVMTHOQWMYFX-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 21
- 230000007547 defect Effects 0.000 abstract description 2
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 abstract 2
- 230000002421 anti-septic effect Effects 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 abstract 1
- 238000010792 warming Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000001034 iron oxide pigment Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
Description
技术领域technical field
本发明属于防腐涂料技术领域，特别涉及一种用于环氧树脂防腐涂料的掺杂氧化铁粉体及其制备方法。The invention belongs to the technical field of anticorrosion coatings, in particular to a doped iron oxide powder used for epoxy resin anticorrosion coatings and a preparation method thereof.
背景技术Background technique
涂料的防腐涉及到涂料制备和涂料防腐性能两个方面的问题。一直以来，人们都在探索和研究各种方法以求增加涂料的防腐性能，环氧树脂涂料制备和生产企业主要采用环氧树脂为基料，并添加活性颜料、缓蚀剂和成膜助剂等。氧化铁作为重要的活性颜料在环氧树脂涂料中使用，在无机酸作用下将钢筋上的铁锈转化为有益的稳定保护层，阻止钢筋的进一步锈蚀。然而随着自然环境的日益恶化，需要防腐性能更加优异的涂料，因此对氧化铁颜料也提出更高的要求。The anticorrosion of coatings involves two aspects of coating preparation and coating anticorrosion performance. For a long time, people have been exploring and researching various methods in order to increase the anti-corrosion performance of coatings. Epoxy resin coating preparation and production enterprises mainly use epoxy resin as the base material, and add active pigments, corrosion inhibitors and film-forming aids. Wait. Iron oxide is used as an important active pigment in epoxy resin coatings. Under the action of inorganic acid, the rust on the steel bar is converted into a beneficial and stable protective layer to prevent further corrosion of the steel bar. However, with the deterioration of the natural environment, coatings with better anti-corrosion properties are required, so higher requirements are placed on iron oxide pigments.
发明内容Contents of the invention
本发明的目的是为了进一步提高环氧树脂防腐涂料的防腐性能，提供了一种用于环氧树脂防腐涂料的掺杂氧化铁粉体及其制备方法，该氧化铁粉体能够改善氧化铁粉体中的缺陷，提高氧化铁粉体的防腐性能；其制备方法具有工艺简单，价格低廉，性价比高的特点。The object of the present invention is to further improve the anticorrosion performance of epoxy resin anticorrosion coatings, and provide a kind of doped iron oxide powder for epoxy resin anticorrosion coatings and its preparation method, the iron oxide powder can improve the performance of iron oxide powder The defects in the iron oxide powder can be improved, and the anti-corrosion performance of the iron oxide powder is improved; the preparation method has the characteristics of simple process, low price and high cost performance.
本发明的目的是通过如下技术方案实现的：The purpose of the present invention is achieved through the following technical solutions:
一种用于环氧树脂防腐涂料的掺杂氧化铁粉体，由三氧化二铁和氧化镁组成，三氧化二铁和氧化镁的重量份数之比为(100～120)份：(1.67～2.5)份；A doped iron oxide powder for epoxy resin anticorrosion coatings, composed of ferric oxide and magnesium oxide, the ratio of parts by weight of ferric oxide and magnesium oxide is (100-120) parts: (1.67 ~2.5) parts;
较好的，三氧化二铁和氧化镁的重量份数之比为100：2.17；Preferably, the ratio of parts by weight of ferric oxide to magnesium oxide is 100:2.17;
上述掺杂氧化铁粉体的粒度范围为40～100nm。The particle size range of the doped iron oxide powder is 40-100 nm.
上述掺杂氧化铁粉体的制备方法，包括如下步骤：The preparation method of the above-mentioned doped iron oxide powder comprises the following steps:
(1)取氯化铁、尿素、含镁离子化合物和水作为原料，将其混合后，搅拌均匀，在反应温度为80～95℃条件下，反应3～5小时，获得黄色的浑浊前驱体溶液；(1) Take ferric chloride, urea, magnesium ion-containing compound and water as raw materials, mix them, stir evenly, and react at a reaction temperature of 80-95°C for 3-5 hours to obtain a yellow turbid precursor solution;
其中，四种原料加入量的重量份数比为：氯化铁203～244份，尿素240～300份，蒸馏水400～500份，含镁离子化合物中镁离子1～1.5份；Among them, the weight-to-number ratios of the additions of the four raw materials are: 203-244 parts of ferric chloride, 240-300 parts of urea, 400-500 parts of distilled water, and 1-1.5 parts of magnesium ions in the compound containing magnesium ions;
所述的含镁离子化合物为氯化镁和氢氧化镁中的一种或两种；The magnesium ion-containing compound is one or both of magnesium chloride and magnesium hydroxide;
(2)将前驱体溶液过滤，取沉淀干燥，然后在加热炉中按照80～100℃/h的速度升温到450～550℃，并保温1.5～3小时，然后自然空气冷却至室温，得到掺杂氧化铁粉体。(2) Filter the precursor solution, take the precipitate and dry it, then raise the temperature to 450-550°C in a heating furnace at a rate of 80-100°C/h, keep it warm for 1.5-3 hours, and then cool it to room temperature in natural air to obtain the doped Mixed iron oxide powder.
上述掺杂氧化铁粉体在应用时，以重量含量为0.45wt％的掺量加入环氧树脂中，作为防腐涂料的活性颜料。When the above-mentioned doped iron oxide powder is applied, it is added into the epoxy resin in an amount of 0.45 wt % by weight, as an active pigment of the anti-corrosion coating.
与现有技术相比，本发明的优势在于：Compared with the prior art, the present invention has the advantages of:
1、本发明的氧化铁粉体中掺杂了氧化镁，加入到环氧树脂涂料中后，与加入纯氧化铁粉体的环氧树脂涂料相比，大幅提高了涂料的防腐性能。1. The iron oxide powder of the present invention is doped with magnesium oxide, and after being added to the epoxy resin coating, compared with the epoxy resin coating adding pure iron oxide powder, the anti-corrosion performance of the coating is greatly improved.
2、本发明掺杂氧化铁粉体是由氯化铁、尿素以及镁离子等原料反应而成，原料易得，货源充足，无污染，加工简单，成本低廉。2. The doped iron oxide powder of the present invention is formed by the reaction of raw materials such as ferric chloride, urea, and magnesium ions. The raw materials are easy to obtain, sufficient supply, no pollution, simple processing, and low cost.
3、由于氧化铁粉体中掺杂的氧化镁量很小，用常规的混粉方法很难将二者混合均匀；本发明的通过湿法的溶液沉淀法将二者共同沉淀，不仅混合均匀而且粉体粒度细小。3. Since the amount of magnesium oxide doped in the iron oxide powder is very small, it is difficult to mix the two evenly with the conventional powder mixing method; the solution precipitation method of the present invention co-precipitates the two, not only mixing evenly And the powder particle size is fine.
具体实施方式detailed description
下面结合具体实施例子对本发明进行进一步详细说明，但本发明的保护范围不受具体的实施例子所限制。另外，以不违背本发明技术方案的前提下，对本发明所做的本领域普通技术人员容易实现的任何改动或改变都将落入本发明的权利要求范围之内。The present invention will be described in further detail below in conjunction with specific implementation examples, but the protection scope of the present invention is not limited by the specific implementation examples. In addition, on the premise of not violating the technical solution of the present invention, any modifications or changes made to the present invention that are easily realized by those skilled in the art will fall within the scope of the claims of the present invention.
以下实施例中的原料均为市购。The raw materials in the following examples are all commercially available.
实施例1Example 1
将各原料按照重量份数：氯化铁为203份，尿素为240份，蒸馏水为400份，氯化镁中镁离子为1份的比例混合均匀，利用溶液沉淀法，反应温度为95℃，反应时间为4小时，获得黄色的浑浊前驱体溶液；According to the parts by weight of each raw material: 203 parts of ferric chloride, 240 parts of urea, 400 parts of distilled water, and 1 part of magnesium ions in magnesium chloride, mix them evenly, use the solution precipitation method, the reaction temperature is 95 ℃, the reaction time For 4 hours, a yellow turbid precursor solution was obtained;
将前驱体溶液过滤，取沉淀在50℃烘箱中干燥，然后在马弗炉中按照100℃/h的速度升温到550℃，保温2小时后，自然空气冷却到室温，得到镁掺杂氧化铁。Filter the precursor solution, take the precipitate and dry it in an oven at 50°C, then heat it up to 550°C in a muffle furnace at a rate of 100°C/h, keep it warm for 2 hours, and cool it to room temperature with natural air to obtain magnesium-doped iron oxide .
该方法制备的掺杂氧化铁粉体中，三氧化二铁和氧化镁的重量份数之比为100:1.67，粉体的粒径为40～100nm。In the doped iron oxide powder prepared by the method, the ratio by weight of ferric oxide to magnesium oxide is 100:1.67, and the particle size of the powder is 40-100nm.
本发明的掺杂氧化铁粉体使用时，将掺杂氧化铁粉体以0.45wt％的掺量加入双酚A型环氧树脂中，以起到提高防腐性能的作用，并按照HG/T 2884-1997的方法进行防腐性能测试。When the doped iron oxide powder of the present invention is used, the doped iron oxide powder is added to the bisphenol A type epoxy resin in an amount of 0.45wt%, so as to improve the anticorrosion performance, and according to HG/T 2884-1997 method for anti-corrosion performance test.
实施例2Example 2
将各原料按照重量份数：氯化铁为203份，尿素为245份，蒸馏水为405份，氢氧化镁中镁离子为1.1份的比例混合均匀，利用溶液沉淀法反应，反应温度为80℃，反应时间为5小时，获得黄色的浑浊前驱体溶液；Mix the raw materials in parts by weight: 203 parts of ferric chloride, 245 parts of urea, 405 parts of distilled water, and 1.1 parts of magnesium ions in magnesium hydroxide, and use the solution precipitation method to react. The reaction temperature is 80°C , the reaction time is 5 hours, and a yellow turbid precursor solution is obtained;
将前驱体溶液过滤，取沉淀在50℃烘箱中干燥，然后在马弗炉中按照80℃/h的速度升温到450℃，保温3小时后，自然空气冷却到室温，得到镁掺杂氧化铁。Filter the precursor solution, take the precipitate and dry it in an oven at 50°C, then heat it up to 450°C in a muffle furnace at a rate of 80°C/h, keep it warm for 3 hours, and cool it to room temperature with natural air to obtain magnesium-doped iron oxide .
该方法制备的掺杂氧化铁粉体中，三氧化二铁和氧化镁的重量份数之比为100:1.83，粉体的粒径为40～100nm。In the doped iron oxide powder prepared by the method, the weight ratio of ferric oxide and magnesium oxide is 100:1.83, and the particle size of the powder is 40-100nm.
本发明掺杂氧化铁粉体的使用方法和检测方法同实施例1。The use method and detection method of the doped iron oxide powder of the present invention are the same as in Example 1.
实施例3Example 3
将各原料按照重量份数：氯化铁203份，尿素250份，蒸馏水为410份，氢氧化镁中镁离子为1.2份的比例混合均匀，利用溶液沉淀法反应，反应温度为90℃，反应时间为3小时，获得黄色的浑浊前驱体溶液；The raw materials are mixed in parts by weight: 203 parts of ferric chloride, 250 parts of urea, 410 parts of distilled water, and 1.2 parts of magnesium ions in magnesium hydroxide. The time is 3 hours, and a yellow turbid precursor solution is obtained;
将前驱体溶液过滤，取沉淀在60℃烘箱中干燥，然后在马弗炉中按照90℃/h的速度升温到500℃，保温1.5小时后，自然空气冷却到室温，得到镁掺杂氧化铁。Filter the precursor solution, take the precipitate and dry it in an oven at 60°C, then heat it up to 500°C in a muffle furnace at a rate of 90°C/h, keep it warm for 1.5 hours, and cool it to room temperature with natural air to obtain magnesium-doped iron oxide .
该方法制备的掺杂氧化铁粉体中，三氧化二铁和氧化镁的重量份数之比为100:2，粉体的粒径为40～100nm。In the doped iron oxide powder prepared by the method, the weight ratio of ferric oxide and magnesium oxide is 100:2, and the particle size of the powder is 40-100nm.
本发明掺杂氧化铁粉体的使用方法和检测方法同实施例1。The use method and detection method of the doped iron oxide powder of the present invention are the same as in Example 1.
实施例4Example 4
将各原料按照重量份数：氯化铁为203份，尿素为255份，蒸馏水为415份，氯化镁中镁离子为1.3份，的比例混合均匀，制备方法同实施例1。Each raw material is mixed according to the weight parts: 203 parts of ferric chloride, 255 parts of urea, 415 parts of distilled water, 1.3 parts of magnesium ions in the magnesium chloride, and the ratio of the preparation method is the same as that of Example 1.
该方法制备的掺杂氧化铁粉体中，三氧化二铁和氧化镁的重量份数之比为100:2.17，粉体的粒径为40～100nm。In the doped iron oxide powder prepared by the method, the weight ratio of ferric oxide and magnesium oxide is 100:2.17, and the particle size of the powder is 40-100nm.
本发明掺杂氧化铁粉体的使用方法和检测方法同实施例1。The use method and detection method of the doped iron oxide powder of the present invention are the same as in Example 1.
实施例5Example 5
将各原料按照重量份数：氯化铁为203份，尿素为260份，蒸馏水为430份，氢氧化镁中镁离子为1.5份的比例混合均匀，制备方法同实施例1。The raw materials were mixed evenly in parts by weight: 203 parts of ferric chloride, 260 parts of urea, 430 parts of distilled water, and 1.5 parts of magnesium ions in magnesium hydroxide. The preparation method was the same as in Example 1.
该方法制备的掺杂氧化铁粉体中，三氧化二铁和氧化镁的重量份数之比为100：2.5，粉体的粒径为40～100nm。In the doped iron oxide powder prepared by the method, the weight ratio of ferric oxide and magnesium oxide is 100:2.5, and the particle size of the powder is 40-100nm.
本发明掺杂氧化铁粉体的使用方法和检测方法同实施例1。The use method and detection method of the doped iron oxide powder of the present invention are the same as in Example 1.
实施例6Example 6
将各原料按照重量份数：氯化铁为244份，尿素为300份，蒸馏水为500份，氯化镁中镁离子为0.5份，氢氧化镁中镁离子为0.5份的比例混合均匀，制备方法同实施例2。The raw materials are mixed in parts by weight: 244 parts of ferric chloride, 300 parts of urea, 500 parts of distilled water, 0.5 parts of magnesium ions in magnesium chloride, and 0.5 parts of magnesium ions in magnesium hydroxide. The preparation method is the same as Example 2.
该方法制备的掺杂氧化铁粉体中，三氧化二铁和氧化镁的重量份数之比为120：1.67，粉体的粒径为40～100nm。In the doped iron oxide powder prepared by the method, the weight ratio of ferric oxide and magnesium oxide is 120:1.67, and the particle size of the powder is 40-100nm.
实施例7Example 7
将各原料按照重量份数：氯化铁为223.5份，尿素为270份，蒸馏水为450份，氯化镁中镁离子为0.5份，氢氧化镁中镁离子为0.5份的比例混合均匀，制备方法同实施例3。The raw materials are mixed according to parts by weight: 223.5 parts of ferric chloride, 270 parts of urea, 450 parts of distilled water, 0.5 parts of magnesium ions in magnesium chloride, and 0.5 parts of magnesium ions in magnesium hydroxide. The preparation method is the same as Example 3.
该方法制备的掺杂氧化铁粉体中，三氧化二铁和氧化镁的重量份数之比为110：1.67，粉体的粒径为40～100nm。In the doped iron oxide powder prepared by the method, the weight ratio of ferric oxide and magnesium oxide is 110:1.67, and the particle size of the powder is 40-100nm.
实施例8Example 8
将各原料按照重量份数：氯化铁为244份，尿素为300份，蒸馏水为500份，氯化镁中镁离子为1.5份的比例混合均匀，制备方法同实施例2。The raw materials were mixed evenly in parts by weight: 244 parts of ferric chloride, 300 parts of urea, 500 parts of distilled water, and 1.5 parts of magnesium ions in magnesium chloride. The preparation method was the same as in Example 2.
该方法制备的掺杂氧化铁粉体中，三氧化二铁和氧化镁的重量份数之比为120：2.5，粉体的粒径为40～100nm。In the doped iron oxide powder prepared by the method, the weight ratio of ferric oxide and magnesium oxide is 120:2.5, and the particle size of the powder is 40-100nm.
下表1是以上实施例1～5制得的掺杂氧化铁粉体以及纯氧化铁粉体以0.45wt％的掺量加入双酚A型环氧树脂中，并对环氧树脂的防腐性能指标进行比较。由表1可以看出，将掺杂氧化铁粉体掺入环氧树脂后，其防腐性能较掺入纯氧化铁粉体的防腐性能更好，尤其是三氧化二铁和氧化镁的重量份之比为100:2.17时效果最好。The following table 1 shows that the doped iron oxide powder and pure iron oxide powder obtained in the above examples 1-5 are added to the bisphenol A epoxy resin at a dosage of 0.45wt%, and the anticorrosion properties of the epoxy resin indicators for comparison. It can be seen from Table 1 that after the doped iron oxide powder is mixed with epoxy resin, its anticorrosion performance is better than that of pure iron oxide powder, especially the weight parts of ferric oxide and magnesium oxide It works best when the ratio is 100:2.17.
表1、掺入氧化铁粉体的环氧树脂防腐性能指标Table 1. Anticorrosion performance index of epoxy resin mixed with iron oxide powder
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