CN104762616A - Carbon steel surface anticorrosive cerium salt passivator and use method thereof - Google Patents
Carbon steel surface anticorrosive cerium salt passivator and use method thereof Download PDFInfo
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Abstract
本发明公开了一种碳钢表面防腐铈盐钝化剂及其使用方法，所述碳钢表面防腐铈盐钝化剂采用在硝酸铈的溶度范围为500～5000ppm的水溶液中，加入体积百分比为3％质量百分数为30％的双氧水作为氧化剂，然后使用质量百分数为65％的硝酸调节pH值，pH值范围为1～4制得。选择化学浸泡法进行钝化，温度控制在30℃，时间为2h，水洗后热风吹干，干燥即可。本发明从根本上去除了传统钝化液中的六价铬和三价铬元素对环境和人体造成的危害，是一种新型环保铈盐钝化液。本发明的铈盐钝化液的钝化工艺、设备与传统的钝化工艺、设备相当，无需对现行设备进行改造。其钝化工艺简单、可靠，环境友好、操作简单、成本低、用量少、防腐性能佳、外表美观等优点。
The invention discloses a carbon steel surface anticorrosion cerium salt passivator and a use method thereof. The carbon steel surface anticorrosion cerium salt passivator is used in an aqueous solution with a solubility of cerium nitrate in the range of 500-5000ppm, and is added in a volume percentage It is prepared by using 3% hydrogen peroxide with a mass percentage of 30% as an oxidizing agent, and then using nitric acid with a mass percentage of 65% to adjust the pH value, and the pH value ranges from 1 to 4. Choose the chemical soaking method for passivation, the temperature is controlled at 30 ° C, the time is 2 hours, after washing with water, dry with hot air and dry. The invention fundamentally eliminates the harm caused by the hexavalent chromium and trivalent chromium elements in the traditional passivation solution to the environment and human body, and is a new environment-friendly cerium salt passivation solution. The passivation process and equipment of the cerium salt passivation solution of the present invention are equivalent to the traditional passivation process and equipment, and the current equipment does not need to be modified. Its passivation process is simple, reliable, environment-friendly, easy to operate, low cost, less dosage, good anti-corrosion performance, beautiful appearance and so on.
Description
技术领域technical field
本发明涉及防腐方法，尤其是一种碳钢表面防腐铈盐钝化剂及其使用方法。The invention relates to an anticorrosion method, in particular to a carbon steel surface anticorrosion cerium salt passivator and a use method thereof.
背景技术Background technique
针对Cr 6+和Cr 3+具有致癌作用，严重危害人体和环境，目前世界各国已开始采取措施严格限制Cr 6+和Cr 3+的使用，因此，研究新型无铬、环保的工艺已势在必行。铈盐钝化处理技术是目前金属防腐蚀的重要发展方向，因其具有环境友好、操作简单、成本低、用量少、防腐性能佳、外表美观等优点，成为取代目前传统的铬钝化的一大热门。C r 6+ and C r 3+ are carcinogenic and seriously harmful to the human body and the environment. At present, countries around the world have begun to take measures to strictly limit the use of C r 6+ and C r 3+ . Therefore, research on new chromium-free and environmentally friendly Craftsmanship is imperative. Cerium salt passivation treatment technology is an important development direction of metal anti-corrosion at present. Because of its advantages of environmental friendliness, simple operation, low cost, less dosage, good anti-corrosion performance, and beautiful appearance, it has become an alternative to the current traditional chromium passivation. A big hit.
发明内容Contents of the invention
本发明的目的在于提供一种碳钢表面防腐铈盐钝化剂及其使用方法，利用铈盐作为钝化剂，对金属基体进行浸泡处理，在其表面形成氧化铈转化膜，起到降低腐蚀电流、隔离基体等保护作用。The purpose of the present invention is to provide a carbon steel surface anti-corrosion cerium salt passivator and its use method. Using cerium salt as a passivator, the metal substrate is soaked to form a cerium oxide conversion film on the surface to reduce corrosion. Current, isolation matrix and other protection.
本发明的目的是这样实现的：一种碳钢表面防腐铈盐钝化剂，其特征在于：所述铈盐钝化剂的组分为：Ce(NO3)3·6H2O、硝酸、双氧水、水，所述碳钢表面防腐铈盐钝化剂采用在硝酸铈的溶度范围为500～5000ppm的水溶液中，加入体积百分比为3％质量百分数为30％的双氧水作为氧化剂，然后使用质量百分数为65％的硝酸调节pH值，pH值范围为1～4制得。The purpose of the present invention is achieved in that a carbon steel surface anticorrosion cerium salt passivator is characterized in that: the components of the cerium salt passivator are: Ce(NO 3 ) 3 6H 2 O, nitric acid, Hydrogen peroxide, water, the carbon steel surface anticorrosion cerium salt passivator adopts in the aqueous solution that the solubility range of cerium nitrate is 500～5000ppm, adds the hydrogen peroxide that the volume percentage is 3% and the mass percentage is 30% as oxidant, then uses the mass percentage The percentage is 65% nitric acid to adjust the pH value, and the pH value ranges from 1 to 4.
一种使用上述的一种碳钢表面防腐铈盐钝化剂处理碳钢表面的钝化方法，其特征在于包括以下步骤：对基材进行机械打磨、中温除油、流水冲洗、表面活化处理、去离子水冲洗、无水乙醇擦拭，选择化学浸泡法进行钝化，使用恒温水浴锅，温度控制在30℃，时间为2h，水洗后热风吹干，然后室温下干燥。A passivation method using the above-mentioned a kind of carbon steel surface anticorrosion cerium salt passivator to treat the surface of carbon steel is characterized in that it includes the following steps: mechanically grinding the base material, degreasing at medium temperature, running water washing, surface activation treatment, Rinse with deionized water, wipe with absolute ethanol, choose the chemical soaking method for passivation, use a constant temperature water bath, control the temperature at 30°C, and dry it with hot air for 2 hours. After washing with water, dry it with hot air, and then dry it at room temperature.
优选的，硝酸铈的溶度范围为500～1000ppm。Preferably, the solubility range of cerium nitrate is 500-1000 ppm.
优选的，pH值范围为2～3。Preferably, the pH range is 2-3.
优选的，所述水为RO水。Preferably, the water is RO water.
本发明配制的铈盐钝化液，从根本上去除了传统钝化液中的六价铬和三价铬元素对环境和人体造成的危害，是一种新型环保铈盐钝化液。本发明的铈盐钝化液的钝化工艺、设备与传统的钝化工艺、设备相当，无需对现行设备进行改造。其钝化工艺简单、可靠，环境友好、操作简单、成本低、用量少、防腐性能佳、外表美观等优点。The cerium salt passivation solution prepared by the invention fundamentally removes the harm caused by hexavalent chromium and trivalent chromium elements in the traditional passivation solution to the environment and human body, and is a new type of environment-friendly cerium salt passivation solution. The passivation process and equipment of the cerium salt passivation solution of the present invention are equivalent to the traditional passivation process and equipment, and the current equipment does not need to be modified. Its passivation process is simple, reliable, environment-friendly, easy to operate, low cost, less dosage, good anti-corrosion performance, beautiful appearance and so on.
附图说明Description of drawings
图1是本发明一种碳钢表面防腐铈盐钝化剂及其使用方法中所述pH＝3条件下，不同ppm硝酸铈浓度的Nyquist图；Fig. 1 is under the pH=3 condition described in a kind of carbon steel surface anticorrosion cerium salt passivator of the present invention and using method thereof, the Nyquist figure of different ppm cerium nitrate concentration;
图2是本发明一种碳钢表面防腐铈盐钝化剂及其使用方法中所述空白对照组的Nyquist图；Fig. 2 is the Nyquist diagram of the blank control group described in a kind of carbon steel surface anticorrosion cerium salt passivator of the present invention and using method thereof;
图3是本发明一种碳钢表面防腐铈盐钝化剂及其使用方法中所述3000ppm硝酸铈浓度条件下，不同pH的Nyquist图；Fig. 3 is under the 3000ppm cerium nitrate concentration condition described in a kind of carbon steel surface anticorrosion cerium salt passivator of the present invention and using method thereof, the Nyquist figure of different pH;
图4是本发明一种碳钢表面防腐铈盐钝化剂及其使用方法中所述pH＝2条件下，不同ppm硝酸铈浓度的Nyquist图。Fig. 4 is a Nyquist diagram of different ppm cerium nitrate concentrations under the condition of pH=2 described in a carbon steel surface anticorrosion cerium salt passivator and its use method of the present invention.
具体实施方式Detailed ways
下面结合实施例对本发明进行进一步的说明。The present invention will be further described below in conjunction with examples.
本发明的目的是这样实现的：一种碳钢表面防腐铈盐钝化剂，其特征在于：所述铈盐钝化剂的组分为：Ce(NO3)3·6H2O、硝酸、双氧水、水，所述碳钢表面防腐铈盐钝化剂采用在硝酸铈的溶度范围为500～5000ppm的水溶液中，加入体积百分比为3％质量百分数为30％的双氧水作为氧化剂，然后使用质量百分数为65％的硝酸调节pH值，pH值范围为1～4制得。The purpose of the present invention is achieved in that a carbon steel surface anticorrosion cerium salt passivator is characterized in that: the components of the cerium salt passivator are: Ce(NO 3 ) 3 6H 2 O, nitric acid, Hydrogen peroxide, water, the carbon steel surface anticorrosion cerium salt passivator adopts in the aqueous solution that the solubility range of cerium nitrate is 500～5000ppm, adds the hydrogen peroxide that the volume percentage is 3% and the mass percentage is 30% as oxidant, then uses the mass percentage The percentage is 65% nitric acid to adjust the pH value, and the pH value ranges from 1 to 4.
一种使用上述的一种碳钢表面防腐铈盐钝化剂处理碳钢表面的钝化方法，其特征在于包括以下步骤：对基材进行机械打磨、中温除油、流水冲洗、表面活化处理、去离子水冲洗、无水乙醇擦拭，选择化学浸泡法进行钝化，使用恒温水浴锅，温度控制在30℃，时间为2h，水洗后热风吹干，然后室温下干燥。A passivation method using the above-mentioned a kind of carbon steel surface anticorrosion cerium salt passivator to treat the surface of carbon steel is characterized in that it includes the following steps: mechanically grinding the base material, degreasing at medium temperature, running water washing, surface activation treatment, Rinse with deionized water, wipe with absolute ethanol, choose the chemical soaking method for passivation, use a constant temperature water bath, control the temperature at 30°C, and dry it with hot air for 2 hours. After washing with water, dry it with hot air, and then dry it at room temperature.
优选的，硝酸铈的溶度范围为500～1000ppm。Preferably, the solubility range of cerium nitrate is 500-1000 ppm.
优选的，pH值范围为2～3。Preferably, the pH range is 2-3.
优选的，所述水为RO水。Preferably, the water is RO water.
本发明一种碳钢表面防腐铈盐钝化剂及其使用方法具有如下优点：A kind of carbon steel surface anticorrosion cerium salt passivator of the present invention and using method thereof have following advantages:
1.该钝化方法具有环境友好、操作简单、成本低、用量少、防腐性能佳、外表美观等优点。1. The passivation method has the advantages of environmental friendliness, simple operation, low cost, less dosage, good anti-corrosion performance and beautiful appearance.
2.该钝化方法参数优化检测方法简单，且参数变化都比较容易控制。2. The parameter optimization detection method of the passivation method is simple, and the parameter changes are relatively easy to control.
3.优化后的钝化方法能对碳钢钢板的表面起到很好的防腐作用。3. The optimized passivation method can play a very good anti-corrosion effect on the surface of the carbon steel plate.
下面结合实施例对本发明做进一步的说明，但本发明不仅限于下述实施例。The present invention will be further described below in conjunction with the examples, but the present invention is not limited to the following examples.
实施例1：Example 1:
在硝酸铈的溶度分别为500ppm、1000ppm、3000ppm、5000ppm的水溶液中，加入体积百分比为3％质量百分数为30％的双氧水作为氧化剂，然后使用质量百分数为65％的硝酸调节pH值，控制pH值为3。基材为150mm*75mm*1.2mm规格的碳钢钢板。对基材进行机械打磨、中温除油、表面活化处理，选择化学浸泡法进行钝化，使用恒温水浴锅，温度控制在30℃，时间为2h。对上述四组试样进行硫酸铜点滴试验，记录钝化膜表面硫酸铜液滴变色的状况，试验结果如表1。通过试验结果，可以看到，在pH＝3条件下，1000ppm，3000ppm，5000ppm硝酸铈浓度的钝化效果比500ppm的有着很大改善。但三者之间的差异不大，我们认为在达到一定的浓度后，硝酸铈浓度对的钝化效果的影响有限。In the aqueous solution whose solubility of cerium nitrate is 500ppm, 1000ppm, 3000ppm, 5000ppm respectively, adding volume percentage is 3% hydrogen peroxide which is 30% by mass percentage as oxidant, then use nitric acid which is 65% by mass percentage to adjust the pH value and control the pH The value is 3. The base material is a carbon steel plate with a size of 150mm*75mm*1.2mm. The substrate is mechanically polished, degreased at medium temperature, surface activated, and passivated by chemical immersion, using a constant temperature water bath, the temperature is controlled at 30°C, and the time is 2h. The copper sulfate spot test was carried out on the above four groups of samples, and the discoloration of copper sulfate droplets on the surface of the passivation film was recorded. The test results are shown in Table 1. Through the test results, it can be seen that under the condition of pH=3, the passivation effect of 1000ppm, 3000ppm, 5000ppm cerium nitrate concentration is much better than that of 500ppm. But the difference among the three is not big. We think that after reaching a certain concentration, the influence of the concentration of cerium nitrate on the passivation effect of cerium nitrate is limited.
表1不同硝酸铈浓度处理后钢板的硫酸铜点滴试验变色时间Table 1 Discoloration time of copper sulfate drop test of steel plate after treatment with different cerium nitrate concentrations
0号实验为经过打磨抛光后但未经钝化处理的碳钢钢板试样的硫酸铜点滴试验空白试验测试结果。对比空白实验，可以看到，经过钝化处理的试样的耐蚀性能得到很大改善。Experiment No. 0 is the test result of the blank test of the copper sulfate spot test on the carbon steel plate sample that has been polished but not passivated. Compared with the blank experiment, it can be seen that the corrosion resistance of the passivated sample has been greatly improved.
实施例2：Example 2:
在硝酸铈的溶度范围为3000ppm的水溶液中，加入体积百分比为3％质量百分数为30％的双氧水作为氧化剂，然后使用质量百分数为65％的硝酸调节pH值，pH值分别为1、2、3、4。基材为150mm*75mm*1.2mm规格的碳钢钢板。对基材进行机械打磨、中温除油、表面活化处理，选择化学浸泡法进行钝化，使用恒温水浴锅，温度控制在30℃，时间为2h。对上述四组试样进行硫酸铜点滴试验，记录钝化膜表面硫酸铜液滴变色的状况，试验结果如表2。通过试验结果，我们可以看到，在3000ppm硝酸铈浓度条件下，pH＝2的钝化效果比pH＝1、pH＝3、pH＝4着比较大的改善，优势明显。In the aqueous solution whose solubility range of cerium nitrate is 3000ppm, adding volume percentage is 3% by volume and is 30% hydrogen peroxide as oxidant, then use the nitric acid of 65% by mass to adjust pH value, pH value is respectively 1,2, 3, 4. The base material is a carbon steel plate with a size of 150mm*75mm*1.2mm. The substrate is mechanically polished, degreased at medium temperature, surface activated, and passivated by chemical immersion, using a constant temperature water bath, the temperature is controlled at 30°C, and the time is 2h. The copper sulfate spot test was carried out on the above four groups of samples, and the discoloration of copper sulfate droplets on the surface of the passivation film was recorded. The test results are shown in Table 2. Through the test results, we can see that under the condition of 3000ppm cerium nitrate concentration, the passivation effect of pH=2 is much better than that of pH=1, pH=3, pH=4, and the advantage is obvious.
0号实验为经过打磨抛光后但未经钝化处理的碳钢钢板试样的硫酸铜点滴试验空白试验测试结果。对比空白实验，可以看到，经过钝化处理的试样的耐蚀性能得到很大改善。Experiment No. 0 is the test result of the blank test of the copper sulfate spot test on the carbon steel plate sample that has been polished but not passivated. Compared with the blank experiment, it can be seen that the corrosion resistance of the passivated sample has been greatly improved.
表4不同pH下处理后钢板的硫酸铜点滴试验变色时间Copper sulfate drop test discoloration time of steel plate after treatment under different pHs in table 4
实施例3：Example 3:
在硝酸铈的溶度分别为：500ppm、1000ppm、3000ppm、5000ppm的水溶液中，加入体积百分比为3％质量百分数为30％的双氧水作为氧化剂，然后使用质量百分数为65％的硝酸调节pH值，pH值为3。对基材进行机械打磨、中温除油、表面活化处理，选择化学浸泡法进行钝化，使用恒温水浴锅，温度控制在30℃，时间为2h。对上述四组实验对象测试表面钝化膜的交流阻抗值，结果如附图1。经过打磨抛光后但未经钝化处理的碳钢钢板试样交流阻抗试验的空白试验测试结果如附图2。The solubility of cerium nitrate is respectively: in the aqueous solution of 500ppm, 1000ppm, 3000ppm, 5000ppm, adding volume percent is that 3% by volume is the hydrogen peroxide of 30% by mass percent as oxidant, then uses the nitric acid of 65% by mass percent to adjust the pH value, pH The value is 3. The substrate is mechanically polished, degreased at medium temperature, surface activated, and passivated by chemical immersion, using a constant temperature water bath, the temperature is controlled at 30°C, and the time is 2h. The AC impedance value of the surface passivation film was tested for the above four groups of experimental objects, and the results are shown in Figure 1. The blank test results of the AC impedance test of the carbon steel plate sample after grinding and polishing but without passivation treatment are shown in Figure 2.
对比图1和图2，我们可以看到与经过打磨抛光后未经表面预处理、处理的碳钢钢板试样相比，所有钝化后的碳钢钢板的交流阻抗皆有大幅度提升，说明试样的腐蚀电流急剧减小，耐蚀性有很大提升。这也说明了氧化铈转化膜确实起到了相当大的缓蚀作用，具有一定应用前景。Comparing Figure 1 and Figure 2, we can see that compared with the carbon steel plate samples without surface pretreatment and treatment after grinding and polishing, the AC impedance of all passivated carbon steel plates has been greatly improved, indicating that The corrosion current of the sample decreased sharply, and the corrosion resistance was greatly improved. This also shows that the cerium oxide conversion coating does play a considerable role in corrosion inhibition and has certain application prospects.
图1显示，在pH＝3条件下，钝化效果并不是随着硝酸铈浓度的增大而越来越好，在3000ppm硝酸铈浓度条件下，钝化效果最好。Figure 1 shows that under the condition of pH=3, the passivation effect is not getting better with the increase of the concentration of cerium nitrate, and the passivation effect is the best under the condition of 3000ppm cerium nitrate concentration.
实施例4：Example 4:
在硝酸铈的溶度为3000ppm的水溶液中，加入体积百分比为3％质量百分数为30％的双氧水作为氧化剂，然后使用质量百分数为65％的硝酸调节pH值，pH值分别为1、2、3、4。对基材进行机械打磨、中温除油、表面活化处理，选择化学浸泡法进行钝化，使用恒温水浴锅，温度控制在30℃，时间为2h。测试四组待测组表面钝化膜的交流阻抗值，结果如附图3。试验结果显示，在pH＝2条件下，钝化效果最好。与硫酸铜点滴试验结果相同。In the aqueous solution with a solubility of cerium nitrate of 3000ppm, add 3% by volume and 30% by mass of hydrogen peroxide as an oxidant, then use 65% by mass of nitric acid to adjust the pH value, the pH values are 1, 2, and 3 respectively , 4. The substrate is mechanically polished, degreased at medium temperature, surface activated, and passivated by chemical immersion, using a constant temperature water bath, the temperature is controlled at 30°C, and the time is 2h. The AC impedance values of the passivation films on the surfaces of the four groups to be tested were tested, and the results are shown in Figure 3. The test results show that the passivation effect is the best under the condition of pH=2. The same result as the copper sulfate spot test.
实施例5：Example 5:
在硝酸铈的溶度分别为：500ppm、1000ppm、3000ppm、5000ppm的水溶液中，加入体积百分比为3％质量百分数为30％的双氧水作为氧化剂，然后使用质量百分数为65％的硝酸调节pH值，pH值为2。对基材进行机械打磨、中温除油、表面活化处理，选择化学浸泡法进行钝化，使用恒温水浴锅，温度控制在30℃，时间为2h。测试四组待测对象表面钝化膜的交流阻抗值，结果如附图4。试验结果表明，在pH＝2条件下，1000ppm硝酸铈浓度的钝化效果最好。The solubility of cerium nitrate is respectively: in the aqueous solution of 500ppm, 1000ppm, 3000ppm, 5000ppm, adding volume percent is that 3% by volume is the hydrogen peroxide of 30% by mass percent as oxidant, then uses the nitric acid of 65% by mass percent to adjust the pH value, pH The value is 2. The substrate is mechanically polished, degreased at medium temperature, surface activated, and passivated by chemical immersion, using a constant temperature water bath, the temperature is controlled at 30°C, and the time is 2h. The AC impedance values of the passivation films on the surfaces of the four groups of objects to be tested were tested, and the results are shown in Figure 4. The test results show that under the condition of pH=2, the passivation effect of 1000ppm cerium nitrate concentration is the best.
对比图1，在pH＝2条件下，1000ppm硝酸铈浓度的钝化效果优于在pH＝3条件下，3000ppm硝酸铈浓度的钝化效果。Comparing Fig. 1, under the condition of pH=2, the passivation effect of 1000ppm cerium nitrate concentration is better than that of 3000ppm cerium nitrate concentration under the condition of pH=3.
以上所述仅为本发明的具体实施方案的详细描述，并不以此限制本发明，凡在本发明的设计思路上所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。The above is only a detailed description of specific embodiments of the present invention, and does not limit the present invention. Any modifications, equivalent replacements and improvements made on the design ideas of the present invention should be included in the protection of the present invention. within range.
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