WO2019006688A1 - Blackening phosphatizing agent, metal member and surface phosphatizing method thereof - Google Patents

Blackening phosphatizing agent, metal member and surface phosphatizing method thereof Download PDF

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Publication number
WO2019006688A1
WO2019006688A1 PCT/CN2017/091756 CN2017091756W WO2019006688A1 WO 2019006688 A1 WO2019006688 A1 WO 2019006688A1 CN 2017091756 W CN2017091756 W CN 2017091756W WO 2019006688 A1 WO2019006688 A1 WO 2019006688A1
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Prior art keywords
parts
phosphating
blackening
weight
metal member
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PCT/CN2017/091756
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French (fr)
Chinese (zh)
Inventor
方招娣
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深圳市长宏泰科技有限公司
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Priority to CN201780092850.0A priority Critical patent/CN110809636A/en
Priority to PCT/CN2017/091756 priority patent/WO2019006688A1/en
Publication of WO2019006688A1 publication Critical patent/WO2019006688A1/en

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/07Chemical 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

Definitions

  • the present invention relates to the field of metal surface treatment technology, and in particular to a blackening phosphating agent, a metal member and a surface phosphating treatment method thereof.
  • the surface treatment technology of the workpiece is usually applied.
  • the surface treatment of aluminum, iron and their alloys goes deep into all walks of life.
  • most of the work needs to be pretreated before surface treatment, for example, cleaning, decontamination and degreasing, and some metal parts need to be phosphated.
  • Phosphating treatment generally uses a phosphating agent to pretreat a metal member to form a phosphating layer on the surface of the metal member for subsequent surface treatment, thereby increasing the bonding force and corrosion resistance of the subsequent film.
  • a phosphating agent for example, before painting, pipe drawing, spinning, cold forging, and anti-rust treatment of metal parts, it is necessary to form a film on the surface of the metal part to increase the corrosion resistance of the workpiece and increase the adhesion of the subsequent coating.
  • the existing surface film of metal parts is insufficient in corrosion resistance and wear resistance, and it is easy to return rust when stored in the crucible.
  • a blackening phosphating agent having a dense crystal layer, a black hair, a good corrosion resistance, a decorative property, and a good adhesion is provided, and a phosphating treatment method and a surface of the metal member are provided. Metal parts obtained after phosphating.
  • a blackening phosphating agent for forming a film on a surface of a metal member comprising 1000 parts by weight of the following components by weight: 20-50 parts of phosphoric acid, 1-4 parts of m-nitrobenzenesulfonate Sodium, 10-25 parts zinc nitrate, 1-3 parts citric acid, 2-10 parts sodium tungstate, 0.1-1.0 parts nickel nitrate, 5-10 parts zinc oxide, 0.5-2 parts sodium fluoroborate and
  • a method for phosphating a surface of a metal member comprising the steps of: formulating a blackening phosphating agent as described above, immersing the metal member in the phosphating solution, and after a predetermined inter-turn treatment, washing the metal member and drying. And a metal member having a surface having a film formed by a surface phosphating treatment of a metal member as described above.
  • the film formed by the blackening phosphating agent has a dense crystal structure, is black and bright, has good corrosion resistance and decoration, and is an advanced normal temperature blackening phosphating agent, which can store and lubricate excellently. Oil, its film thickness, high hardness, and strong corrosion resistance.
  • Embodiments of the present invention provide a blackening phosphating agent for forming a film on a surface of a metal member, which comprises, by weight of 1000 parts by weight, a component of the following parts by weight: 20-50 parts of phosphoric acid, 1-4 parts Sodium m-nitrobenzenesulfonate, 10-2 5 parts zinc nitrate, 1-3 parts citric acid, 2-10 parts sodium tungstate, 0.1-1.0 parts nickel nitrate, 5-10 parts zinc oxide, 0.5
  • the parts by weight of the phosphoric acid are preferably from 30 to 40 parts by weight.
  • the sodium m-nitrobenzenesulfonate is preferably 2-3 parts by weight.
  • the zinc nitrate is in an amount of 15 to 20 parts by weight.
  • the citric acid is preferably present in an amount of from 2 to 3 parts by weight.
  • the nickel nitrate is present in an amount of from 0.4 to 0.8 parts by weight.
  • the sodium tungstate is 4-8 parts by weight.
  • the zinc oxide is 6-8 parts by weight.
  • the sodium fluoroborate is used in an amount of from 1 to 2 parts by weight.
  • a preferable film forming effect is achieved by controlling the balance of the respective distribution ratios.
  • Phosphoric acid provides the main acidity, stabilizes the pH of the bath and is the primary film-forming component.
  • Sodium tungstate, zinc nitrate, and zinc oxide are the main film-forming components.
  • Sodium nitrobenzenesulfonate, citric acid, and nickel nitrate can increase the corrosion resistance of the phosphating film.
  • Sodium fluoroborate acts as an auxiliary film former and increases the film formation rate.
  • the manganese-based phosphating film has a large thickness, a small number of pores, and the phosphating grains are densely granulated, and can be widely applied to decorative treatment and anti-corrosion treatment.
  • the blackening phosphating agent is a combination of sodium tungstate, zinc salt, phosphate and various additives.
  • the metal workpiece is immersed in a weakly acidic treatment liquid composed of the phosphating solution, and the metal interacts with the acid and the salt to form a protective black film layer which is insoluble in water on the surface of the workpiece.
  • the film is densely crystallized and has good corrosion resistance, decorativeness and adhesion.
  • Embodiments of the present invention also provide a metal component surface phosphating treatment method, comprising the steps of: preparing a blackening phosphating agent as described above; immersing the metal member in the phosphating solution, after a predetermined daytime treatment , Washed metal parts, dry.
  • the metal member is immersed in a phosphating solution.
  • the metal member is immersed in the mash of the phosphating solution preferably for 6 to 9 minutes.
  • the metal workpiece is degreased and pickled.
  • Embodiments of the present invention also provide a metal member which is processed by a surface phosphating treatment of a metal member as described above to form a film on the surface of the metal member.
  • the film is formed to a thickness of 2 to 10 ⁇ m.
  • the film protects the metal, gives it a bright, bright, and has good corrosion, decorative and adhesion. It can be used together with anti-rust oil for better anti-rust effect.
  • the components are mixed in the following parts by weight (total amount is 1000 parts by weight): 20 parts of phosphoric acid, 1 part of sodium m-nitrobenzenesulfonate, 10 parts of zinc nitrate, 1 part of citric acid, 2 parts of sodium tungstate , 0.1 parts of nickel nitrate, 5 parts of zinc oxide, 0.5 parts of sodium fluoroborate and the balance of water, stirred, uniformly mixed, and formulated into a phosphating agent.
  • Phosphating treatment method According to the above method, the blackening phosphating agent is prepared; the metal parts are iron parts, for example, the iron parts are degreased, washed with water, then pickled and washed, and then immersed in the phosphating solution at room temperature. Next, after 8 minutes of treatment, the metal parts are washed and dried. During the treatment, phosphating agent can be added to ensure the effect of the working fluid.
  • the film is fine, copper sulfate drip test does not change color for 100 seconds.
  • the ingredients are mixed in the following parts by weight (total amount 1000 parts by weight): 30 parts of phosphoric acid, 2 parts of sodium m-nitrobenzenesulfonate, 15 parts of zinc nitrate, 2 parts of citric acid, 5 parts of sodium tungstate , 0.4 parts of nickel nitrate, 7 parts of zinc oxide, 1 part of sodium fluoroborate and the balance of water, stirred, mixed evenly, formulated into a phosphating agent.
  • Phosphating treatment method according to the above method, the blackening phosphating agent is prepared; the metal parts are iron parts, for example, the iron parts are degreased, washed with water, then pickled and washed, and then immersed in the phosphating solution at room temperature. Next, after 8 minutes of treatment, the metal parts are washed and dried. During the treatment, phosphating agent can be added to ensure the effect of the working fluid. [0025] After the phosphating solution is treated, the surface of the workpiece is observed, and the surface of the workpiece is found to be black and bright, and the color is uniform.
  • the film is fine, copper sulfate drip test does not change color for 160 seconds.
  • the components are mixed in the following parts by weight (total amount 1000 parts by weight): 40 parts of phosphoric acid, 3 parts of sodium m-nitrobenzenesulfonate, 20 parts of zinc nitrate, 2 parts of citric acid, 7 parts of sodium tungstate , 0.7 parts of nickel nitrate, 8 parts of zinc oxide, 1. 5 parts of sodium fluoroborate and the balance of water, stirred, evenly mixed, formulated into a phosphating agent.
  • Phosphating treatment method according to the above method, the blackening phosphating agent is prepared; the metal parts are iron parts, for example, the iron parts are degreased, washed with water, then pickled and washed, and then immersed in the phosphating solution at room temperature. Next, after 8 minutes of treatment, the metal parts are washed and dried. During the treatment, phosphating agent can be added to ensure the effect of the working fluid.
  • the film is fine, copper sulfate drip test does not change color for 190 seconds.
  • the components are mixed in the following parts by weight (total amount 1000 parts by weight): 50 parts of phosphoric acid, 4 parts of sodium m-nitrobenzenesulfonate, 25 parts of zinc nitrate, 3 parts of citric acid, 10 parts of sodium tungstate , 1 part of nickel nitrate, 10 parts of zinc oxide, 2 parts of sodium fluoroborate and the balance of water, stirred, mixed evenly, formulated into a phosphating agent.
  • Phosphating treatment method According to the above method, the blackening phosphating agent is prepared; the metal parts are taken as iron, the iron parts are degreased, washed with water, then pickled and washed, and then immersed in the phosphating solution at room temperature. Next, after 8 minutes of treatment, the metal parts are washed and dried. During the treatment, phosphating agent can be added to ensure the effect of the working fluid.
  • the film is fine, copper sulfate drip test does not change color for 190 seconds.

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  • Chemical & Material Sciences (AREA)
  • 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

A blackening phosphatizing agent, a metal member and a surface phosphatizing method thereof. The blackening phosphatizing agent is used for forming a film on the surface of a metal member. The black phosphatizing agent comprises, based on 1,000 parts by weight, the following components in parts by weight: 20-50 parts of phosphoric acid, 1-4 parts of nitrobenzenesulfonic acid sodium salt, 10-25 parts of zinc nitrate, 1-3 parts of citric acid, 2-10 parts of sodium tungstate, 0.1-1.0 parts of nickel nitrate, 5-10 parts of zinc oxide, and 0.5-2 parts of sodium fluoroborate, with the balance being water. The film layer formed by the blackening phosphatizing agent is densely crystallized, capable of blackening and brightening, and has good corrosion resistance and decorative properties.

Description

发黑磷化剂、 金属件及其表面磷化处理方法 技术领域  Black phosphating agent, metal parts and surface phosphating treatment method thereof
[0001] 本发明涉及金属表面处理技术领域, 具体涉及一种发黑磷化剂、 金属件及其表 面磷化处理方法。  [0001] The present invention relates to the field of metal surface treatment technology, and in particular to a blackening phosphating agent, a metal member and a surface phosphating treatment method thereof.
背景技术  Background technique
[0002] 为提高产品表面性能或者外观, 通常对工件表面处理技术。 例如, 铝、 铁及其 合金的表面处理工艺深入各行各业中。 而且, 大多数工作在进行表面处理前还 需要经过预处理, 例如, 进行清洗, 除污除油, 某些用途的金属件还需要进行 磷化处理。  [0002] In order to improve the surface properties or appearance of a product, the surface treatment technology of the workpiece is usually applied. For example, the surface treatment of aluminum, iron and their alloys goes deep into all walks of life. Moreover, most of the work needs to be pretreated before surface treatment, for example, cleaning, decontamination and degreasing, and some metal parts need to be phosphated.
[0003] 磷化处理一般采用磷化剂对金属件进行预处理, 以在金属件表面形成磷化层, 以便进行后续的表面处理, 增加后续膜的结合力和防腐力。 例如, 对金属件进 行涂装、 抽管、 抽丝、 冷锻、 防锈处理之前, 需要在金属件表面形成皮膜, 以 对工件增加防腐性和增加后续涂装的附着力。 然而, 现有的金属件表面皮膜在 耐腐蚀性、 耐磨性等方面表现不足, 存放吋间长了容易返锈。  [0003] Phosphating treatment generally uses a phosphating agent to pretreat a metal member to form a phosphating layer on the surface of the metal member for subsequent surface treatment, thereby increasing the bonding force and corrosion resistance of the subsequent film. For example, before painting, pipe drawing, spinning, cold forging, and anti-rust treatment of metal parts, it is necessary to form a film on the surface of the metal part to increase the corrosion resistance of the workpiece and increase the adhesion of the subsequent coating. However, the existing surface film of metal parts is insufficient in corrosion resistance and wear resistance, and it is easy to return rust when stored in the crucible.
技术问题  technical problem
[0004] 有鉴于此, 提供一种膜层结晶致密、 发黑发亮、 具有良好的耐蚀性、 装饰性、 附着力良好的发黑磷化剂, 以及金属件表面磷化处理方法和经过磷化处理后制 得的金属件。  [0004] In view of the above, a blackening phosphating agent having a dense crystal layer, a black hair, a good corrosion resistance, a decorative property, and a good adhesion is provided, and a phosphating treatment method and a surface of the metal member are provided. Metal parts obtained after phosphating.
问题的解决方案  Problem solution
技术解决方案  Technical solution
[0005] 一种发黑磷化剂, 用于在金属件表面形成皮膜, 以 1000重量份计, 其包括如下 重量份数的成分: 20-50份磷酸, 1-4份间硝基苯磺酸钠, 10-25份的硝酸锌, 1-3 份柠檬酸, 2-10份钨酸钠, 0.1-1.0份硝酸镍, 5-10份氧化锌, 0.5-2份氟硼酸钠和余  [0005] A blackening phosphating agent for forming a film on a surface of a metal member, comprising 1000 parts by weight of the following components by weight: 20-50 parts of phosphoric acid, 1-4 parts of m-nitrobenzenesulfonate Sodium, 10-25 parts zinc nitrate, 1-3 parts citric acid, 2-10 parts sodium tungstate, 0.1-1.0 parts nickel nitrate, 5-10 parts zinc oxide, 0.5-2 parts sodium fluoroborate and
[0006] 一种金属件表面磷化处理方法, 其包括下列步骤: 配制如上所述的发黑磷化剂 将金属件浸入磷化溶液中, 经过预定吋间处理后, 水洗金属件, 干燥。 [0007] 以及, 一种金属件, 其表面具有通过如上所述的金属件表面磷化处理方法形成 的皮膜。 [0006] A method for phosphating a surface of a metal member, comprising the steps of: formulating a blackening phosphating agent as described above, immersing the metal member in the phosphating solution, and after a predetermined inter-turn treatment, washing the metal member and drying. And a metal member having a surface having a film formed by a surface phosphating treatment of a metal member as described above.
发明的有益效果  Advantageous effects of the invention
有益效果  Beneficial effect
[0008] 上述发黑磷化剂形成的膜层结晶致密, 发黑发亮, 具有良好的耐蚀性、 装饰性 、 是一种先进的常温型发黑磷化剂, 能够极好的储存润滑油, 其膜厚, 硬度高 , 耐蚀性强。  [0008] The film formed by the blackening phosphating agent has a dense crystal structure, is black and bright, has good corrosion resistance and decoration, and is an advanced normal temperature blackening phosphating agent, which can store and lubricate excellently. Oil, its film thickness, high hardness, and strong corrosion resistance.
本发明的实施方式 Embodiments of the invention
[0009] 以下将结合具体实施例对本发明进行详细说明。 The present invention will be described in detail below with reference to specific embodiments.
[0010] 本发明实施例提供一种发黑磷化剂, 用于在金属件表面形成皮膜, 以 1000重量 份计, 其包括如下重量份数的成分: 20-50份磷酸, 1-4份间硝基苯磺酸钠, 10-2 5份的硝酸锌, 1-3份柠檬酸, 2-10份钨酸钠, 0.1-1.0份硝酸镍, 5-10份氧化锌, 0.5 [0010] Embodiments of the present invention provide a blackening phosphating agent for forming a film on a surface of a metal member, which comprises, by weight of 1000 parts by weight, a component of the following parts by weight: 20-50 parts of phosphoric acid, 1-4 parts Sodium m-nitrobenzenesulfonate, 10-2 5 parts zinc nitrate, 1-3 parts citric acid, 2-10 parts sodium tungstate, 0.1-1.0 parts nickel nitrate, 5-10 parts zinc oxide, 0.5
-2份氟硼酸钠和余量水。 - 2 parts sodium fluoroborate and the balance water.
[0011] 具体地, 所述磷酸的重量份数优选为 30-40份。 所述间硝基苯磺酸钠的重量份 数优选为 2-3份。 所述硝酸锌的重量份数为 15-20份。 所述柠檬酸的重量份数优选 为 2-3份。 所述硝酸镍的重量份数为 0.4-0.8份。 所述钨酸钠的重量份数为 4-8份。 所述氧化锌的重量份数为 6-8份。 所述氟硼酸钠的重量份数为 1-2份。  [0011] Specifically, the parts by weight of the phosphoric acid are preferably from 30 to 40 parts by weight. The sodium m-nitrobenzenesulfonate is preferably 2-3 parts by weight. The zinc nitrate is in an amount of 15 to 20 parts by weight. The citric acid is preferably present in an amount of from 2 to 3 parts by weight. The nickel nitrate is present in an amount of from 0.4 to 0.8 parts by weight. The sodium tungstate is 4-8 parts by weight. The zinc oxide is 6-8 parts by weight. The sodium fluoroborate is used in an amount of from 1 to 2 parts by weight.
[0012] 在上述发黑磷化剂中, 通过控制各成分配比平衡, 以达到较佳成膜效果。 磷酸 提供主要酸度、 稳定槽液 PH值并且为主要成膜成分。 钨酸钠、 硝酸锌、 氧化锌 为主要成膜成分。 间硝基苯磺酸钠、 柠檬酸, 硝酸镍可以增加磷化膜的耐蚀性 。 氟硼酸钠作为辅助成膜剂, 增加成膜速度。  [0012] In the above blackening phosphating agent, a preferable film forming effect is achieved by controlling the balance of the respective distribution ratios. Phosphoric acid provides the main acidity, stabilizes the pH of the bath and is the primary film-forming component. Sodium tungstate, zinc nitrate, and zinc oxide are the main film-forming components. Sodium nitrobenzenesulfonate, citric acid, and nickel nitrate can increase the corrosion resistance of the phosphating film. Sodium fluoroborate acts as an auxiliary film former and increases the film formation rate.
[0013] 本实施例中, 锰系磷化膜厚度大、 孔隙少, 磷化晶粒呈密集颗状, 可广泛应用 于装饰处理和防腐处理。 发黑磷化剂是由钨酸钠, 锌盐, 磷酸盐和多种添加剂 复配而成。 将金属工件浸入由该磷化液配成的弱酸性处理液中, 金属与酸及盐 相互作用, 在工件表面生成一层不溶于水的保护性黑色膜层。 该膜层结晶致密 , 具有良好的耐蚀性、 装饰性和的附着力。 可配合防锈油使用, 防锈效果更佳 [0014] 本发明实施例还提供一种金属件表面磷化处理方法, 其包括下列步骤: 配制如 上所述的发黑磷化剂; 将金属件浸入磷化溶液中, 经过预定吋间处理后, 水洗 金属件, 干燥。 [0013] In the present embodiment, the manganese-based phosphating film has a large thickness, a small number of pores, and the phosphating grains are densely granulated, and can be widely applied to decorative treatment and anti-corrosion treatment. The blackening phosphating agent is a combination of sodium tungstate, zinc salt, phosphate and various additives. The metal workpiece is immersed in a weakly acidic treatment liquid composed of the phosphating solution, and the metal interacts with the acid and the salt to form a protective black film layer which is insoluble in water on the surface of the workpiece. The film is densely crystallized and has good corrosion resistance, decorativeness and adhesion. Can be used with anti-rust oil, better anti-rust effect [0014] Embodiments of the present invention also provide a metal component surface phosphating treatment method, comprising the steps of: preparing a blackening phosphating agent as described above; immersing the metal member in the phosphating solution, after a predetermined daytime treatment , Washed metal parts, dry.
[0015] 在金属件浸入磷化溶液吋。 金属件浸入磷化溶液的吋间优选为 6-9分钟。 在金 属件浸入磷化溶液前, 先对金属工件进行除油、 酸洗处理。  [0015] The metal member is immersed in a phosphating solution. The metal member is immersed in the mash of the phosphating solution preferably for 6 to 9 minutes. Before the metal parts are immersed in the phosphating solution, the metal workpiece is degreased and pickled.
[0016] 本发明实施例还提供一种金属件, 其通过如上所述的金属件表面磷化处理方法 进行处理, 在金属件表面形成皮膜。 形成皮膜的厚度为 2-10微米。 皮膜可对金属 件进行保护, 发黑发亮, 具有良好的耐蚀性、 装饰性和附着力。 可配合防锈油 使用, 防锈效果更佳。  [0016] Embodiments of the present invention also provide a metal member which is processed by a surface phosphating treatment of a metal member as described above to form a film on the surface of the metal member. The film is formed to a thickness of 2 to 10 μm. The film protects the metal, gives it a bright, bright, and has good corrosion, decorative and adhesion. It can be used together with anti-rust oil for better anti-rust effect.
[0017] 以下通过具体实例说明本发明实施例的发黑磷化剂及其处理方法等方面。  [0017] The blackening phosphating agent and the treatment method thereof and the like in the embodiments of the present invention are described below by way of specific examples.
[0018] 实施例 1  Embodiment 1
[0019] 按照下列重量份数混合各成分 (总量为 1000重量份) : 20份磷酸, 1份间硝基 苯磺酸钠, 10份的硝酸锌, 1份柠檬酸, 2份钨酸钠, 0.1份硝酸镍, 5份氧化锌, 0. 5份氟硼酸钠和余量水, 搅拌, 混合均匀, 配制成磷化剂。  [0019] The components are mixed in the following parts by weight (total amount is 1000 parts by weight): 20 parts of phosphoric acid, 1 part of sodium m-nitrobenzenesulfonate, 10 parts of zinc nitrate, 1 part of citric acid, 2 parts of sodium tungstate , 0.1 parts of nickel nitrate, 5 parts of zinc oxide, 0.5 parts of sodium fluoroborate and the balance of water, stirred, uniformly mixed, and formulated into a phosphating agent.
[0020] 磷化处理方法: 按照上述方法配制好发黑磷化剂; 金属件以铁件为例, 将铁件 除油, 水洗, 再酸洗并水洗后, 浸入磷化溶液中, 在常温下, 经过 8分钟处理后 , 水洗金属件, 干燥。 在处理过程中, 可及吋添加磷化剂, 以保证工作液的效 果。  [0020] Phosphating treatment method: According to the above method, the blackening phosphating agent is prepared; the metal parts are iron parts, for example, the iron parts are degreased, washed with water, then pickled and washed, and then immersed in the phosphating solution at room temperature. Next, after 8 minutes of treatment, the metal parts are washed and dried. During the treatment, phosphating agent can be added to ensure the effect of the working fluid.
[0021] 经过上述磷化溶液处理后, 观察工件表面, 发现工件表面发黑发亮, 颜色均匀 [0021] After the treatment of the phosphating solution, the surface of the workpiece was observed, and the surface of the workpiece was found to be black and bright, and the color was uniform.
, 皮膜细致, 硫酸铜点滴实验 100秒不变色。 , the film is fine, copper sulfate drip test does not change color for 100 seconds.
[0022] 实施例 2 Embodiment 2
[0023] 按照下列重量份数混合各成分 (总量为 1000重量份) : 30份磷酸, 2份间硝基 苯磺酸钠, 15份的硝酸锌, 2份柠檬酸, 5份钨酸钠, 0.4份硝酸镍, 7份氧化锌, 1 份氟硼酸钠和余量水, 搅拌, 混合均匀, 配制成磷化剂。  [0023] The ingredients are mixed in the following parts by weight (total amount 1000 parts by weight): 30 parts of phosphoric acid, 2 parts of sodium m-nitrobenzenesulfonate, 15 parts of zinc nitrate, 2 parts of citric acid, 5 parts of sodium tungstate , 0.4 parts of nickel nitrate, 7 parts of zinc oxide, 1 part of sodium fluoroborate and the balance of water, stirred, mixed evenly, formulated into a phosphating agent.
[0024] 磷化处理方法: 按照上述方法配制好发黑磷化剂; 金属件以铁件为例, 将铁件 除油, 水洗, 再酸洗并水洗后, 浸入磷化溶液中, 在常温下, 经过 8分钟处理后 , 水洗金属件, 干燥。 在处理过程中, 可及吋添加磷化剂, 以保证工作液的效 果。 [0025] 经过上述磷化溶液处理后, 观察工件表面, 发现工件表面发黑发亮, 颜色均匀[0024] Phosphating treatment method: according to the above method, the blackening phosphating agent is prepared; the metal parts are iron parts, for example, the iron parts are degreased, washed with water, then pickled and washed, and then immersed in the phosphating solution at room temperature. Next, after 8 minutes of treatment, the metal parts are washed and dried. During the treatment, phosphating agent can be added to ensure the effect of the working fluid. [0025] After the phosphating solution is treated, the surface of the workpiece is observed, and the surface of the workpiece is found to be black and bright, and the color is uniform.
, 皮膜细致, 硫酸铜点滴实验 160秒不变色。 , the film is fine, copper sulfate drip test does not change color for 160 seconds.
[0026] 实施例 3 Embodiment 3
[0027] 按照下列重量份数混合各成分 (总量为 1000重量份) : 40份磷酸, 3份间硝基 苯磺酸钠, 20份的硝酸锌, 2份柠檬酸, 7份钨酸钠, 0.7份硝酸镍, 8份氧化锌, 1. 5份氟硼酸钠和余量水, 搅拌, 混合均匀, 配制成磷化剂。  [0027] The components are mixed in the following parts by weight (total amount 1000 parts by weight): 40 parts of phosphoric acid, 3 parts of sodium m-nitrobenzenesulfonate, 20 parts of zinc nitrate, 2 parts of citric acid, 7 parts of sodium tungstate , 0.7 parts of nickel nitrate, 8 parts of zinc oxide, 1. 5 parts of sodium fluoroborate and the balance of water, stirred, evenly mixed, formulated into a phosphating agent.
[0028] 磷化处理方法: 按照上述方法配制好发黑磷化剂; 金属件以铁件为例, 将铁件 除油, 水洗, 再酸洗并水洗后, 浸入磷化溶液中, 在常温下, 经过 8分钟处理后 , 水洗金属件, 干燥。 在处理过程中, 可及吋添加磷化剂, 以保证工作液的效 果。  [0028] Phosphating treatment method: according to the above method, the blackening phosphating agent is prepared; the metal parts are iron parts, for example, the iron parts are degreased, washed with water, then pickled and washed, and then immersed in the phosphating solution at room temperature. Next, after 8 minutes of treatment, the metal parts are washed and dried. During the treatment, phosphating agent can be added to ensure the effect of the working fluid.
[0029] 经过上述磷化溶液处理后, 观察工件表面, 发现工件表面发黑发亮, 颜色均匀 [0029] After the treatment of the phosphating solution, the surface of the workpiece was observed, and the surface of the workpiece was found to be black and bright, and the color was uniform.
, 皮膜细致, 硫酸铜点滴实验 190秒不变色。 , the film is fine, copper sulfate drip test does not change color for 190 seconds.
[0030] 实施例 4 Embodiment 4
[0031] 按照下列重量份数混合各成分 (总量为 1000重量份) : 50份磷酸, 4份间硝基 苯磺酸钠, 25份的硝酸锌, 3份柠檬酸, 10份钨酸钠, 1份硝酸镍, 10份氧化锌, 2 份氟硼酸钠和余量水, 搅拌, 混合均匀, 配制成磷化剂。  [0031] The components are mixed in the following parts by weight (total amount 1000 parts by weight): 50 parts of phosphoric acid, 4 parts of sodium m-nitrobenzenesulfonate, 25 parts of zinc nitrate, 3 parts of citric acid, 10 parts of sodium tungstate , 1 part of nickel nitrate, 10 parts of zinc oxide, 2 parts of sodium fluoroborate and the balance of water, stirred, mixed evenly, formulated into a phosphating agent.
[0032] 磷化处理方法: 按照上述方法配制好发黑磷化剂; 金属件以铁件为例, 将铁件 除油, 水洗, 再酸洗并水洗后, 浸入磷化溶液中, 在常温下, 经过 8分钟处理后 , 水洗金属件, 干燥。 在处理过程中, 可及吋添加磷化剂, 以保证工作液的效 果。  [0032] Phosphating treatment method: According to the above method, the blackening phosphating agent is prepared; the metal parts are taken as iron, the iron parts are degreased, washed with water, then pickled and washed, and then immersed in the phosphating solution at room temperature. Next, after 8 minutes of treatment, the metal parts are washed and dried. During the treatment, phosphating agent can be added to ensure the effect of the working fluid.
[0033] 经过上述磷化溶液处理后, 观察工件表面, 发现工件表面发黑发亮, 颜色均匀 [0033] After the phosphating solution was processed, the surface of the workpiece was observed, and the surface of the workpiece was found to be black and bright, and the color was uniform.
, 皮膜细致, 硫酸铜点滴实验 190秒不变色。 , the film is fine, copper sulfate drip test does not change color for 190 seconds.
[0034] 需要说明的是, 本发明并不局限于上述实施方式, 根据本发明的创造精神, 本 领域技术人员还可以做出其他变化, 这些依据本发明的创造精神所做的变化, 都应包含在本发明所要求保护的范围之内。 [0034] It should be noted that the present invention is not limited to the above embodiments, and other changes may be made by those skilled in the art according to the creative spirit of the present invention, and the changes according to the creative spirit of the present invention should be It is intended to be included within the scope of the invention as claimed.

Claims

权利要求书 Claim
[权利要求 1] 一种发黑磷化剂, 用于在金属件表面形成皮膜, 其特征在于, 以 1000 重量份计, 其包括如下重量份数的成分: 20-50份磷酸, 1-4份间硝基 苯磺酸钠, 10-25份的硝酸锌, 1-3份柠檬酸, 2-10份钨酸钠, 0.1-1.0 份硝酸镍, 5-10份氧化锌, 0.5-2份氟硼酸钠和余量水。  [Claim 1] A blackening phosphating agent for forming a film on a surface of a metal member, which comprises, by weight of 1000 parts by weight, a component of the following parts by weight: 20-50 parts of phosphoric acid, 1-4 Sodium nitrobenzene sulfonate, 10-25 parts zinc nitrate, 1-3 parts citric acid, 2-10 parts sodium tungstate, 0.1-1.0 parts nickel nitrate, 5-10 parts zinc oxide, 0.5-2 parts Sodium fluoroborate and the balance of water.
[权利要求 2] 如权利要求 1所述的发黑磷化剂, 其特征在于, 所述磷酸的重量份数 为 30-40份。  [Claim 2] The blackening phosphating agent according to claim 1, wherein the phosphoric acid is in a range of 30 to 40 parts by weight.
[权利要求 3] 如权利要求 1所述的发黑磷化剂, 其特征在于, 所述间硝基苯磺酸钠 的重量份数为 2-3份, 所述硝酸镍的重量份数为 0.4-0.8份。 [Claim 3] The blackening phosphating agent according to claim 1, wherein the sodium nitrobenzenesulfonate is 2-3 parts by weight, and the nickel nitrate is in parts by weight. 0.4-0.8 parts.
[权利要求 4] 如权利要求 1所述的发黑磷化剂, 其特征在于, 所述硝酸锌的重量份 数为 15-20份。 [Claim 4] The blackening phosphating agent according to claim 1, wherein the zinc nitrate is in an amount of 15 to 20 parts by weight.
[权利要求 5] 如权利要求 1所述的发黑磷化剂, 其特征在于, 所述柠檬酸的重量份 数为 2-3份。 [Claim 5] The blackening phosphating agent according to claim 1, wherein the citric acid is in an amount of from 2 to 3 parts by weight.
[权利要求 6] 如权利要求 1所述的发黑磷化剂, 其特征在于, 所述钨酸钠的重量份 数为 4-8份。 [Claim 6] The blackening phosphating agent according to claim 1, wherein the sodium tungstate is 4-8 parts by weight.
[权利要求 7] 如权利要求 1所述的发黑磷化剂, 其特征在于, 所述钨酸钠的重量份 数为 4-8份。 [Claim 7] The blackening phosphating agent according to claim 1, wherein the sodium tungstate is 4-8 parts by weight.
[权利要求 8] 一种金属件表面磷化处理方法, 其包括下列步骤: 配制如权利要求 1- 7任一项所述的发黑磷化剂; 将金属件浸入磷化溶液中, 经过预定吋 间处理后, 水洗金属件, 干燥。 [Claim 8] A method for phosphating a surface of a metal member, comprising the steps of: formulating the blackening phosphating agent according to any one of claims 1 to 7; immersing the metal member in the phosphating solution, after predetermined After the daytime treatment, the metal parts are washed and dried.
[权利要求 9] 如权利要求 8所述的金属件表面磷化处理方法, 其特征在于, 在金属 件浸入磷化溶液前, 先对金属工件进行除油、 酸洗处理, 所述预定吋 间为 5-12分钟。  [Claim 9] The method for phosphating a surface of a metal member according to claim 8, wherein the metal workpiece is degreased and pickled before the metal member is immersed in the phosphating solution, and the predetermined daytime It is 5-12 minutes.
[权利要求 10] 一种金属件, 其特征在于, 所述金属件表面通过如权利要求 8所述的 金属件表面磷化处理方法形成有皮膜。  [Claim 10] A metal member characterized in that the surface of the metal member is formed with a film by the surface phosphating treatment method of the metal member according to claim 8.
PCT/CN2017/091756 2017-07-04 2017-07-04 Blackening phosphatizing agent, metal member and surface phosphatizing method thereof WO2019006688A1 (en)

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