CN106929842A - 一种无铬钝化液及其制备方法 - Google Patents
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- C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
- C23C22/42—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also phosphates
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
- C23C22/08—Orthophosphates
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- C—CHEMISTRY; METALLURGY
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
- C23C22/36—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
- C23C22/361—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing titanium, zirconium or hafnium compounds
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
- C23C22/44—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also fluorides or complex fluorides
Abstract
本发明实施例公开了一种无铬钝化液及其制备方法，涉及金属表面材料处理技术领域。所述无铬钝化液由以下的原料制备而成：硅酸钠，有机硅烷，金属络合剂，磷酸，酸类络合剂，乙二醇，乙二胺四乙酸二钠，水。本发明的一种无铬钝化液不含铬等对环境和人体有重大危害的成分，减少了环境污染，并且组分简单、成本低廉、耐腐蚀效果好。
Description
技术领域
本发明涉及金属表面材料处理技术领域，尤其涉及一种无铬钝化液及其制备方法。
背景技术
钝化处理是指在一定的溶液中进行化学或电化学处理，在镀层上形成一层坚实致密的、稳定性高的薄膜的表面处理方法，钝化使镀层的耐腐蚀性能进一步的提高并增加表面光泽和抗污染的能力。如经过化学镀、电镀、酸洗、水洗等处理的工件表面非常活泼，所以要立即进行钝化处理，使处理后的金属表面形成一层保护膜，减缓腐蚀。对工件进行全面的钝化处理，可以提高其抗腐蚀性能，延长使用寿命。
金属表面进行钝化处理通常使用的是铬酸盐钝化。铬酸盐钝化膜致密，本身又耐蚀，与基体金属的结合力牢固，并且能够对裸漏处的金属表面再次钝化，对进一步腐蚀起到了抑制作用，即通常所说的“自愈能力”。然而，六价铬化合物有很高的毒性，是致癌物质。随着人们环境保护意识的增强，对于有毒有害物的控制日益强化。为此，许多替代六价铬的对策和工艺已经被广泛的提出来了。
发明内容
本发明的实施例提供一种无铬钝化液及其制备方法，能够减少环境污染，钝化液组分简单，成本低廉，耐腐蚀效果好。
为达到上述目的，本发明的实施例采用如下技术方案：
本发明的实施例提供一种无铬钝化液，包括以下的原料制备而成：硅酸钠，有机硅烷，金属络合剂，磷酸，酸类络合剂，乙二醇，乙二胺四乙酸二钠，水。
进一步的，所述一种无铬钝化液是由以下份数的原料制备而成：硅酸钠5-15g/L，有机硅烷0.5-15g/L，金属络合剂3-8g/L，磷酸10-30mL/L，酸类络合剂5-10g/L，乙二醇10-20g/L，乙二胺四乙酸二钠5-15g/L，其余为水。
进一步的，所述有机硅烷是羟基乙叉二磷酸、3-氨丙基三已氯基硅烷、硫酸羟胺、γ-缩水甘油醚氧丙基三甲氧基硅烷中的一种。
进一步的，所述金属络合剂是钼酸钠、氟钛酸钾、氯化钯、硝酸钴、硝酸铈中的一种或多种混合物。
进一步的，所述酸类络合剂是单宁酸、柠檬酸或酒石酸中的一种。
本发明还提供了一种无铬钝化液的制备方法，包括：
S1、将硅酸钠溶解在适量水中，加入磷酸，搅拌均匀，并加热至30-60℃；
S2、将乙二胺四乙酸二钠，乙二醇，金属络合剂溶解在适量水中，加入有机硅烷，在30-60℃条件下搅拌20-40分钟；
S3、将步骤1获得的溶液与步骤2获得的溶液混合，搅拌90-120分钟，用稀硫酸或氢氧化钠溶液调节pH1.5-3.0，得到所述无铬钝化液。
进一步的，所述稀硫酸是0.5-1.0mol/L的稀硫酸。
进一步的，所述氢氧化钠溶液是0.5-1.0mol/L的氢氧化钠溶液。
本发明实施例提供的一种无铬钝化液及其制备方法，具有以下优点：
（1）制备工艺简单可行，生产成本低廉；（2）不含铬，对环境友好；（3）本发明制备的钝化液，钝化效果好，耐腐蚀能力强。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案，下面结合具体实施方式对本发明作进一步详细描述。
实施例1
一种无铬钝化液，由下列份数的原料制备而成：硅酸钠5-8g/L，3-氨丙基三已氯基硅烷0.5-5g/L，氯化钯3-4g/L，磷酸10-15mL/L，柠檬酸5-8g/L，乙二醇10-15g/L，乙二胺四乙酸二钠5-8g/L，其余为水。
一种无铬钝化液制备方法，包括：
S1、将硅酸钠溶解在适量水中，加入磷酸，搅拌均匀，并加热至30℃；
S2、将乙二胺四乙酸二钠，乙二醇，氯化钯溶解在适量水中，加入3-氨丙基三已氯基硅烷，在30℃条件下搅拌40分钟；
S3、将步骤1获得的溶液与步骤2获得的溶液混合，搅拌120分钟，用0.5mol/L稀硫酸或0.5mol/L氢氧化钠溶液调节pH至1.8，得到所述无铬钝化液。
实施例2
一种无铬钝化液，由下列份数的原料制备而成：硅酸钠5-8g/L，3-氨丙基三已氯基硅烷0.5-5g/L，氯化钯3-4g/L，磷酸10-15mL/L，柠檬酸5-8g/L，乙二醇10-15g/L，乙二胺四乙酸二钠5-8g/L，其余为水。
一种无铬钝化液制备方法，包括：
S1、将硅酸钠溶解在适量水中，加入磷酸，搅拌均匀，并加热至60℃；
S2、将乙二胺四乙酸二钠，乙二醇，氯化钯溶解在适量水中，加入3-氨丙基三已氯基硅烷，在60℃条件下搅拌20分钟；
S3、将步骤1获得的溶液与步骤2获得的溶液混合，搅拌100分钟，用0.8mol/L稀硫酸或0.8mol/L氢氧化钠溶液调节pH至2.8，得到所述无铬钝化液。
实施例3
一种无铬钝化液，由下列份数的原料制备而成：硅酸钠8-10g/L，3-氨丙基三已氯基硅烷5-10g/L，氯化钯4-6g/L，磷酸15-20mL/L，柠檬酸5-8g/L，乙二醇10-15g/L，乙二胺四乙酸二钠8-10g/L，其余为水。
一种无铬钝化液制备方法，包括：
S1、将硅酸钠溶解在适量水中，加入磷酸，搅拌均匀，并加热至30℃；
S2、将乙二胺四乙酸二钠，乙二醇，氯化钯溶解在适量水中，加入3-氨丙基三已氯基硅烷，在30℃条件下搅拌40分钟；
S3、将步骤1获得的溶液与步骤2获得的溶液混合，搅拌120分钟，用0.5mol/L稀硫酸或0.5mol/L氢氧化钠溶液调节pH至1.8，得到所述无铬钝化液。
实施例4
一种无铬钝化液，由下列份数的原料制备而成：硅酸钠8-10g/L，3-氨丙基三已氯基硅烷5-10g/L，氯化钯4-6g/L，磷酸15-20mL/L，柠檬酸5-8g/L，乙二醇10-15g/L，乙二胺四乙酸二钠8-10g/L，其余为水。
一种无铬钝化液制备方法，包括：
S1、将硅酸钠溶解在适量水中，加入磷酸，搅拌均匀，并加热至60℃；
S2、将乙二胺四乙酸二钠，乙二醇，氯化钯溶解在适量水中，加入3-氨丙基三已氯基硅烷，在60℃条件下搅拌20分钟；
S3、将步骤1获得的溶液与步骤2获得的溶液混合，搅拌100分钟，用0.8mol/L稀硫酸或0.8mol/L氢氧化钠溶液调节pH至2.8，得到所述无铬钝化液。
实施例5
一种无铬钝化液，由下列份数的原料制备而成：硅酸钠10-15g/L，3-氨丙基三已氯基硅烷10-15g/L，氯化钯6-8g/L，磷酸20-30mL/L，柠檬酸8-10g/L，乙二醇15-20g/L，乙二胺四乙酸二钠10-15g/L，其余为水。
一种无铬钝化液制备方法，包括：
S1、将硅酸钠溶解在适量水中，加入磷酸，搅拌均匀，并加热至30℃；
S2、将乙二胺四乙酸二钠，乙二醇，氯化钯溶解在适量水中，加入3-氨丙基三已氯基硅烷，在30℃条件下搅拌40分钟；
S3、将步骤1获得的溶液与步骤2获得的溶液混合，搅拌120分钟，用0.5mol/L稀硫酸或0.5mol/L氢氧化钠溶液调节pH至1.8，得到所述无铬钝化液。
实施例6
一种无铬钝化液，由下列份数的原料制备而成：硅酸钠10-15g/L，3-氨丙基三已氯基硅烷10-15g/L，氯化钯6-8g/L，磷酸20-30mL/L，柠檬酸8-10g/L，乙二醇15-20g/L，乙二胺四乙酸二钠10-15g/L，其余为水。
一种无铬钝化液制备方法，包括：
S1、将硅酸钠溶解在适量水中，加入磷酸，搅拌均匀，并加热至60℃；
S2、将乙二胺四乙酸二钠，乙二醇，氯化钯溶解在适量水中，加入3-氨丙基三已氯基硅烷，在60℃条件下搅拌20分钟；
S3、将步骤1获得的溶液与步骤2获得的溶液混合，搅拌100分钟，用0.8mol/L稀硫酸或0.8mol/L氢氧化钠溶液调节pH至2.8，得到所述无铬钝化液。
本说明书中的各个实施例均采用递进的方式描述，各个实施例之间相同相似的部分互相参见即可，每个实施例重点说明的都是与其他实施例的不同之处。尤其，对于设备实施例而言，由于其基本相似于方法实施例，所以描述得比较简单，相关之处参见方法实施例的部分说明即可。以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求的保护范围为准。
Claims (8)
1.一种无铬钝化液，其特征在于，包括以下的原料制备而成：硅酸钠，有机硅烷，金属络合剂，磷酸，酸类络合剂，乙二醇，乙二胺四乙酸二钠，水。
2.根据权利要求1所述的一种无铬钝化液，其特征在于，包括以下份数的原料制备而成：硅酸钠5-15g/L，有机硅烷0.5-15g/L，金属络合剂3-8g/L，磷酸10-30mL/L，酸类络合剂5-10g/L，乙二醇10-20g/L，乙二胺四乙酸二钠5-15g/L，其余为水。
3.根据权利要求1所述的一种无铬钝化液，其特征在于，所述有机硅烷是羟基乙叉二磷酸、3-氨丙基三已氯基硅烷、硫酸羟胺、γ-缩水甘油醚氧丙基三甲氧基硅烷中的一种。
4.根据权利要求1所述的一种无铬钝化液，其特征在于，所述金属络合剂是钼酸钠、氟钛酸钾、氯化钯、硝酸钴、硝酸铈中的一种或多种混合物。
5.根据权利要求1所述的一种无铬钝化液，其特征在于， 所述酸类络合剂是单宁酸、柠檬酸或酒石酸中的一种。
6.一种无铬钝化液制备方法，其特征在于，包括以下步骤：
S1、将硅酸钠溶解在适量水中，加入磷酸，搅拌均匀，并加热至30-60℃；
S2、将乙二胺四乙酸二钠，乙二醇，金属络合剂溶解在适量水中，加入有机硅烷，在30-60℃条件下搅拌20-40分钟；
S3、将S1获得的溶液与S2获得的溶液混合，搅拌90-120分钟，用稀硫酸或氢氧化钠溶液调节pH1.5-3.0，得到所述无铬钝化液。
7.根据权利要求6所述的一种无铬钝化液制备方法，其特征在于，所述稀硫酸是0.5-1.0mol/L的稀硫酸。
8.根据权利要求6所述的一种无铬钝化液制备方法，其特征在于，所述氢氧化钠溶液是0.5-1.0mol/L的氢氧化钠溶液。
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