CN110760827A - 高温黑色锰系磷化液、制备方法及其应用 - Google Patents
高温黑色锰系磷化液、制备方法及其应用 Download PDFInfo
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 29
- 239000011572 manganese Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title description 6
- 229910000599 Cr alloy Inorganic materials 0.000 claims abstract description 17
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 17
- 239000000788 chromium alloy Substances 0.000 claims abstract description 17
- 239000010959 steel Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract description 4
- NDEMNVPZDAFUKN-UHFFFAOYSA-N guanidine;nitric acid Chemical compound NC(N)=N.O[N+]([O-])=O.O[N+]([O-])=O NDEMNVPZDAFUKN-UHFFFAOYSA-N 0.000 abstract description 3
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 abstract 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 abstract 1
- 229960004889 salicylic acid Drugs 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 30
- 239000003208 petroleum Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910001437 manganese ion Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- MFXMOUUKFMDYLM-UHFFFAOYSA-L zinc;dihydrogen phosphate Chemical compound [Zn+2].OP(O)([O-])=O.OP(O)([O-])=O MFXMOUUKFMDYLM-UHFFFAOYSA-L 0.000 description 3
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- -1 iron ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 235000019832 sodium triphosphate Nutrition 0.000 description 2
- LJRGBERXYNQPJI-UHFFFAOYSA-M sodium;3-nitrobenzenesulfonate Chemical compound [Na+].[O-][N+](=O)C1=CC=CC(S([O-])(=O)=O)=C1 LJRGBERXYNQPJI-UHFFFAOYSA-M 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910000616 Ferromanganese Inorganic materials 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- 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
- C23C22/07—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
- C23C22/18—Orthophosphates containing manganese cations
-
- C—CHEMISTRY; METALLURGY
- 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
- C23C22/73—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 characterised by the process
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
本发明提供一种高温黑色锰系磷化液，以重量百分比计，包括以下成分：水杨酸2.3‑7.3％，二氧化锰10.1‑13.1％，硝酸12.3‑14.3％，硝酸胍1.8‑2.8％，马日夫盐5.1‑7.1％，余量为水。该高温黑色锰系磷化液耐腐蚀性好，能够在高铬合金钢表面形成连续均匀致密磷化膜。
Description
技术领域
本发明涉及磷化处理液，尤其是涉及一种高温黑色锰系磷化液及其制备方法。
背景技术
在石油行业中，现有的石油管箍大多由T95、N80等低铬合金钢制成，对这些低铬合金钢的磷化处理均采用高温锰系磷化液，其得到的磷化膜连续致密，耐磨耐蚀性都很好。
随着时代的发展，石油管箍材质采用低铬合金钢已经不能满足实际应用的需求，因此出现了P110、V150、V175为材质的高铬合金钢石油管箍，对于这些石油管箍，如果仍然使用现有的高温锰系磷化液进行表面化学处理，就会存在很多问题：第一，磷化反应速度较慢，磷化膜形成的时间很长：P110需要60-70分钟完成反应；V150、V175需要90分钟以上完成反应；第二，高铬合金钢经过磷化处理，得到的磷化膜厚度比低铬合金钢的磷化膜薄很多，试验发现，高铬合金钢经过普通高温锰系磷化液进行磷化处理后，得到的磷化膜一般为7-14μm(一般磷化膜的厚度要求为15-30μm)；第三，磷化处理过程中，铁被酸溶解，溶解下来的铁离子一部分参与成膜反应形成磷化膜成分，而另一部分铁离子则被氧化成沉淀，从溶液中析出形成磷化渣，现有的高温锰系磷化液容易产生大量的磷化渣，磷化渣将沾附到磷化工件上面，使磷化膜粗糙不平。
由此看来，普通锰系磷化液虽可以勉强适用低铬合金钢的表面磷化处理，但是一旦钢工件中铬合金的含量变高后，铬合金中的铬、锰、镍等合金元素使钢铁表面的极化电位升高，同时铬镍容易在管箍表面产生一层保护性的氧化膜，这样一来，普通锰系磷化液侵蚀钢铁表面会很难，磷化处理得到的膜层较薄，且容易产生大量的磷化渣。
中国专利CN 200810048834.4公开了一种无污染的刹车片五金件的微晶磷化处理液,主要由下列重量份的原料制成:硝酸锌40-50份,磷酸二氢锌22-30份,马日夫盐(酸式磷酸锰)30-40份,硝酸胍1.5-2份,间硝基苯磺酸钠1.5-2份,三聚磷酸钠1-2份,酒石酸2-4份,磺基水杨酸2-3份,柠檬酸1.5-2.5份,水1000-1200份。本发明用于铁制小五金件的表面的发黑磷化处理,具有磷化速度快,性能好,环境污染轻,成本低等特点。其磷化膜磷化结晶细,色泽均匀,呈一致的黑色,并且耐蚀性能好。尤其是本发明选择对环境污染小、高效的原料,通过优化组合,合理配比,使得本发明在磷化和环保方面均取得了优异的效果。该专利配方含锌锰元素，不是严格意思上的纯锰系磷化液,且锌元素参与成膜后磷化膜在摩擦过程中出现粉化，容易造成石油管箍“卡死”“咬死”等现象；该配方仅含酸式盐(磷酸二氢锌，马日夫盐)，酸性弱，不易在金属上形成膜层，特别是在低铬高铬钢上。
发明内容
为了克服现有技术存在的缺点，本发明的目的之一在于提供一种高温黑色锰系磷化液，该高温黑色锰系磷化液能够在高铬合金钢表面形成连续均匀致密磷化膜。
本发明的目的之二在于提供该高温黑色锰系磷化液的制备方法。
本发明的目的之三在于提供该高温黑色锰系磷化液在高铬合金钢表面处理中的应用。
本发明高温黑色锰系磷化液以重量百分比计，包括以下成分：
优选地，本发明高温黑色锰系磷化液中还可以加入2.3-5.1％的高锰酸钾，高锰酸钾是强氧化剂，加速磷化处理反应。
优选地，本发明高温黑色锰系磷化液以重量百分比计，由以下成分制成：
本发明高温黑色锰系磷化液的制备方法：将各成分称量，共混、搅拌溶解均匀即可。
本发明高温黑色锰系磷化液中二氧化锰直接提供锰离子，马日夫盐通过水解提供锰离子，提供锰离子有缓冲的余地，保持槽液长期稳定；通过高温使金属盐沉积反应向右移动，形成磷酸锰铁沉积在工件表面上，形成连续均匀致密磷化膜。
本发明高温黑色锰系磷化液的使用方法如下：将上述制备好的磷化液按10-12％配制成槽液，加温至65-95℃，把除油除锈好的高铬合金钢石油管箍浸泡其中15-30分钟后取出，用清水洗净，热风吹干。
本发明高温黑色锰系磷化液的有益效果如下：耐腐蚀性好，能够在高铬合金钢表面形成连续均匀致密磷化膜。
具体实施方式
下面通过实施例对本发明作进一步说明，但不作为对本发明的限定。
表1为实施例1-5、对比例1-2的配方，单位为wt％。
表1实施例1-5、对比例1-2的配方
以上实施例、对比例磷化液的制备方法：将各组分称量，共混、搅拌溶解均匀即可。
对比例3
实施例1：在磷化槽中，倒入300份(每份1Kg，以下同)水，然后将30份马日夫盐
加入槽中，在不断搅拌状态下，加入30份磷酸二氢锌，待二者充分溶解后，倒入300份水进行稀释；将45份硝酸锌倒入磷化槽中，搅拌溶解后，将溶液加热至70℃，依次加入2份柠檬酸、3份酒石酸、3份磺基水杨酸，充分搅拌，混匀；然后将2份三聚磷酸钠和2份间硝基苯磺酸钠依次加入至磷化槽中，搅拌溶解后，倒入400份水，慢慢加入1.5份硝酸胍，充分搅拌，混合均匀后即可得到本刹车片五金件的微晶磷化处理液。
以上高温黑色锰系磷化液的使用方法如下：将上述制备好的磷化液按11wt％配制成槽液，加温至65-95℃，把除油除锈好的V175高铬合金钢石油管箍浸泡其中20分钟后取出，用清水洗净，热风吹干。
以上实施例、对比例的使用效果如下：
表2
表2中各项目的测试方法如下：
耐硫酸铜点滴试验；GB/T15519，
氯化钠浸渍试验；GB/T 6807，
中性盐雾试验：GB/T10125－1997，
磷化膜挂白灰情况：目测，
石油管箍“卡死”情况：管箍拧接试验。
Claims (5)
1.一种高温黑色锰系磷化液，其特征在于以重量百分比计，包括以下成分：
2.根据权利要求1所述的高温黑色锰系磷化液，其特征在于还包括2.3-5.1％的高锰酸钾。
3.根据权利要求1所述的高温黑色锰系磷化液，其特征在于，由以下成分制成：
4.根据权利要求1所述高温黑色锰系磷化液的制备方法，其特征在于包括如下步骤：将各成分称量，共混、搅拌溶解均匀即可。
5.根据权利要求1所述高温黑色锰系磷化液在高铬合金钢表面处理中的应用。
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| CN112899672A (zh) * | 2021-01-14 | 2021-06-04 | 厦门腾兴隆化工有限公司 | 一种黑色磷化剂及其制备方法 |
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| JPS58123882A (ja) * | 1982-01-20 | 1983-07-23 | Toyota Motor Corp | リン酸マンガン皮膜化成処理方法 |
| US5595611A (en) * | 1996-02-14 | 1997-01-21 | Henkel Corporation | Moderate temperature manganese phosphate conversion coating composition and process |
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