WO2017161579A1 - 封孔剂和型材表面封孔处理工艺 - Google Patents

封孔剂和型材表面封孔处理工艺 Download PDF

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WO2017161579A1
WO2017161579A1 PCT/CN2016/077415 CN2016077415W WO2017161579A1 WO 2017161579 A1 WO2017161579 A1 WO 2017161579A1 CN 2016077415 W CN2016077415 W CN 2016077415W WO 2017161579 A1 WO2017161579 A1 WO 2017161579A1
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Prior art keywords
sealing agent
parts
hole sealing
profile
solution
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PCT/CN2016/077415
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English (en)
French (fr)
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王饶玲
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深圳市恒兆智科技有限公司
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Priority to PCT/CN2016/077415 priority Critical patent/WO2017161579A1/zh
Publication of WO2017161579A1 publication Critical patent/WO2017161579A1/zh

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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
    • C23C22/34—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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation

Definitions

  • the present invention relates to the field of surface treatment technology, and in particular, to a surface sealing treatment process for a sealing agent profile.
  • the surface treatment technology of the workpiece is usually applied.
  • the surface treatment of aluminum-magnesium and its alloys goes deep into all walks of life. Sealing is a common surface treatment process.
  • the conventional sealing method includes a boiling water method, a dichromate method, a metal salt method, etc., although the boiling water sealing method is non-polluting, it is prone to a powder frost phenomenon, affecting the combination of the quality appearance and the lacquer layer and the matrix, and Energy consumption is large.
  • the dichromate method has been polluted by the environment and has been eliminated by the existing market.
  • the metal salt method has a variety of ions, and there are some impurity ions, and the impurity ions have a certain interference to the sealing treatment.
  • the traditional sealing agent is easy to produce ash after treatment, and the gloss and hardness need to be improved.
  • a sealing agent and a surface sealing treatment process for a sealing agent and a profile with good impurity ion interference resistance, easy control, and no ashing are provided.
  • a sealing agent comprising the following components in parts by weight:
  • a profile surface sealing treatment process comprising the steps of: preparing a sealing agent as described above, dissolving the sealing agent in water and preparing a sealing agent solution of 3 to 5 g/L; The profile is immersed in the sealing agent solution, and the pH of the control solution is in the range of 5.5 to 6.8. After 1-18 minutes of treatment, a closed oxide film is formed on the surface of the profile.
  • the above sealing agent and the sealing treatment process have strong buffering resistance, good resistance to impurity ion interference, and the prepared sealing agent solution is easy to control, and the processing parameters are wide, and the process fluctuations due to the prior process are The sealing effect caused by the change of process parameters has little effect.
  • the above sealing agent can be selected from a suitable surfactant, namely polyethylene glycol and isobutanol, and the use of these good dispersing effects avoids the drawbacks such as ash ash which is common in the sealing treatment.
  • the surface of the closed profile has improved gloss and hardness, and can be widely applied to various metal profiles.
  • a sealing agent comprising the following ingredients in parts by weight:
  • the cobalt acetate or cobalt fluoride is preferably 3-5 parts by weight, preferably cobalt fluoride.
  • the parts by weight of the nickel fluoride are preferably from 750 to 1,000.
  • the parts by weight of ammonium fluoride are preferably from 75 to 100.
  • the isobutyl alcohol or polyglycol is preferably from 32 to 50 parts by weight, preferably a polyglycol.
  • the sealing agent is a powdery solid.
  • nickel fluoride is the main component of sealing
  • ammonium fluoride, cobalt acetate or cobalt fluoride is a sealing accelerator
  • isobutanol or polyglycol is a complex interference component.
  • This embodiment further provides a surface sealing treatment process for a profile, which comprises the following steps: preparing a sealing agent as described above, dissolving the sealing agent in water, and preparing a sealing agent of 3 to 5 g/L. Solution; The profile is immersed in the sealing agent solution, and the pH of the control solution is in the range of 5.5 to 6.8. After 1-18 minutes of treatment, a closed oxide film is formed on the surface of the profile.
  • the ion concentration is 0.8 ⁇ 1.2g/L, F The ion concentration is 0.3 to 0.7 g/L.
  • the pH value is adjusted with dilute acetic acid or dilute hydrofluoric acid, and the pH value is adjusted with a dilute sodium hydroxide or a dilute aqueous ammonia solution.
  • the formation rate of the closed oxide film is 0.8 to 1.2 ⁇ m/ ⁇ .
  • composition range, preparation method, and use effect of the above-mentioned sealing agent are exemplified below by a plurality of examples.
  • the components are mixed according to the following parts by weight: 3 parts of cobalt acetate, 750 parts of nickel fluoride, 75 parts of ammonium fluoride, 32 parts of isobutanol, 15 parts of water, stirred, uniformly mixed, and then 3-5 g / The concentration of L is uniformly mixed to form a sealing agent.
  • sealing treatment process preparing a sealing agent; the sealing agent is dissolved in water to prepare a sealing agent solution, the sealing agent content in the sealing agent solution is 5g / L; the oxidized profile is immersed In the sealing agent solution, the pH of the sealing agent solution is controlled to be in the range of 5.5 to 6.8. After the treatment for 10 minutes, a closed oxide film is formed on the surface of the profile, and taken out and dried.
  • the ⁇ 30mg/dm 2) dyeing test results are ideal, without any residual color.
  • the components were mixed in the following parts by weight: 4 parts of cobalt acetate, 800 parts of nickel fluoride, 80 parts of ammonium fluoride, 40 parts of isobutanol, 15 parts of water, stirred, uniformly mixed, and formulated into a sealing agent.
  • sealing treatment process preparing a sealing agent; the sealing agent is dissolved in water to prepare a sealing agent solution, the sealing agent content in the sealing agent solution is 5g / L; the profile is immersed in the sealing agent In the solution, control the P of the sealing solution
  • the H value was in the range of 5.5 to 6.8. After 10 minutes of treatment, a closed oxide film was formed on the surface of the profile, and it was taken out and dried.
  • the ⁇ 30mg/dm 2) dyeing test results are ideal, without any residual color.
  • the ingredients were mixed in the following parts by weight: 5 parts of cobalt acetate, 900 parts of nickel fluoride, 90 parts of ammonium fluoride, 50 parts of isobutanol, 15 parts of water, stirred, uniformly mixed, and formulated into a sealing agent.
  • sealing treatment process preparing a sealing agent; the sealing agent is dissolved in water to prepare a sealing agent solution, the sealing agent content in the sealing agent solution is 4g / L; the profile is immersed in the sealing agent In the solution, control the P of the sealer solution
  • the H value is in the range of 5.5 to 6.8.
  • the ⁇ 30mg/dm 2) dyeing test results are ideal, without any residual color.
  • the ingredients were mixed in the following parts by weight: 5 parts of cobalt acetate, 1000 parts of nickel fluoride, 100 parts of ammonium fluoride, 55 parts of isobutanol, 18 parts of water, stirred, uniformly mixed, and formulated into a sealing agent.
  • sealing treatment process preparing a sealing agent; the sealing agent is dissolved in water to prepare a sealing agent solution, the sealing agent content in the sealing agent solution is 3g / L; the profile is immersed in the sealing agent In the solution, control the P of the sealing solution
  • the H value is in the range of 5.5 to 6.8. After 15 minutes of treatment, a closed oxide film is formed on the surface of the profile, and taken out and dried.
  • the ⁇ 30mg/dm 2) dyeing test results are ideal, without any residual color.
  • the components were mixed in the following parts by weight: 6 parts of cobalt acetate, 1200 parts of nickel fluoride, 120 parts of ammonium fluoride, 60 parts of isobutanol, 18 parts of water, stirred, uniformly mixed, and formulated into a sealing agent.
  • sealing treatment process preparing a sealing agent; the sealing agent is dissolved in water to prepare a sealing agent solution, the sealing agent content in the sealing agent solution is 3g / L; the profile is immersed in the sealing agent In the solution, control the P of the sealing solution
  • the H value is in the range of 5.5 to 6.8. After 15 minutes of treatment, a closed oxide film is formed on the surface of the profile, and taken out and dried.
  • the ⁇ 30mg/dm 2) dyeing test results are ideal, without any residual color.

Abstract

本发明涉及一种封孔剂及型材表面封孔处理工艺，该封孔剂包括按照重量份数配比的下列成分：3-6份醋酸钴或氟化钴，750-1200份氟化镍，75-120份氟化铵，32-60份异丁醇或聚二醇，15-18份水。上述封孔剂和封孔处理工艺耐缓冲能力强，耐杂质离子干扰性好，而且制成的封孔剂溶液易于控制，处理时，工艺参数较宽，对因前工序工艺波动、工艺参数变化而造成的封闭效果影响不大。上述封孔剂可选用合适的表面活化剂即聚乙二醇和异丁醇，利用它们良好的分散效果，避免了封闭处理常见的挂灰等弊病。经过上述封孔剂的封孔处理后，封闭后的型材表面光泽和硬度提高，可广泛应用于各种金属型材。

Description

封孔剂和型材表面封孔处理工艺
技术领域
[0001] 本发明涉及表面处理技术领域， 具体涉及一种封孔剂型材表面封孔处理工艺。
背景技术
[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， 铝镁及其合 金的表面处理工艺深入各行各业中。 封孔处理就是一种常见的表面处理工艺。
[0003] 传统的封孔方法有沸水法、 重铬酸盐法、 金属盐法等， 沸水封闭法虽然无污染 ， 但易出现粉霜现象， 影响质量外观与漆层和基体的结合力， 且能源清耗大。 重铬酸盐法对环境污染大， 已经被现有市场淘汰。 金属盐法有多种离子， 存在 一些杂质离子， 杂质离子对封孔处理具有一定的干扰性。 传统的封孔剂处理后 容易产生挂灰， 光泽度和硬度有待提高。
技术问题
[0004] 有鉴于此， 提供一种耐杂质离子干扰性好、 易于控制、 无挂灰的封孔剂和型材 表面封孔处理工艺。
问题的解决方案
技术解决方案
[0005] 一种封孔剂， 其包括按照重量份数配比的下列成分：
[0006] 醋酸钴或氟化钴 3-6
[0007] 氟化镍 750-1200
[0008] 氟化铵 75-120
[0009] 异丁醇或聚二醇 32-60
[0010] 水 15-18。
[0011] 以及， 一种型材表面封孔处理工艺， 其包括如下步骤： 配制如上所述的封孔剂 ， 将封孔剂溶于水中并配制成 3~5g/L的封孔剂溶液； 将型材浸入于封孔剂溶液中 ， 控制溶液的 PH值在 5.5〜6.8范围内， 处理 1-18分钟后， 即在型材表面形成封闭 氧化膜。 发明的有益效果
有益效果
[0012] 上述封孔剂和封孔处理工艺耐缓冲能力强， 耐杂质离子干扰性好， 而且制成的 封孔剂溶液易于控制， 处理吋， 工艺参数较宽， 对因前工序工艺波动、 工艺参 数变化而造成的封闭效果影响不大。 上述封孔剂可选用合适的表面活化剂即聚 乙二醇和异丁醇， 利用它们良好的分散效果， 避免了封闭处理常见的挂灰等弊 病。 经过上述封孔剂的封孔处理后， 封闭后的型材表面光泽和硬度提高， 可广 泛应用于各种金属型材。
本发明的实施方式
[0013] 以下将结合具体实施例对本发明进行详细说明。
[0014] 一种封孔剂， 其包括按照重量份数配比的下列成分：
[0015] 醋酸钴或氟化钴 3-6
[0016] 氟化镍 750-1200
[0017] 氟化铵 75-120
[0018] 异丁醇或聚二醇 32-60
[0019] 水 15-18。
[0020] 具体地， 醋酸钴或氟化钴的重量份数优选为 3-5， 优选为氟化钴。 所述氟化镍 的重量份数优选为 750-1000。 氟化铵的重量份数优选为 75-100。 异丁醇或聚二醇 的重量份数优选为 32-50， 优选为聚二醇。 封孔剂为粉状固体。 其中， 氟化镍为 封孔主要成分， 氟化铵、 醋酸钴或氟化钴为封孔促进剂， 异丁醇或聚二醇为络 合干扰成分。
[0021] 本实施例还提供一种型材表面封孔处理工艺， 其包括如下步骤： 配制如上所述 的封孔剂， 将封孔剂溶于水中并配制成 3~5g/L的封孔剂溶液； 将型材浸入于封孔 剂溶液中， 控制溶液的 PH值在 5.5〜6.8范围内， 处理 1-18分钟后， 即在型材表面 形成封闭氧化膜。
[0022] 其中， 在封孔剂溶液浸渍处理过程中， 控制封孔剂溶液中 Ni 2+
离子浓度为 0.8~1.2g/L， F 离子浓度为 0.3~0.7g/L。 在封孔处理过程中， 当溶液 PH值过高吋， 用稀醋酸或稀 氢氟酸调节其 PH值， 过低吋用稀氢氧化钠或稀氨水溶液调节其 PH值。 封闭氧化 膜厚度形成速率为 0.8〜1.2μηι/ηήη。
[0023] 以下通过多个实施例来举例说明上述封孔剂的组成范围、 配制方法以及使用效 果等方面。
[0024] 实施例 1
[0025] 按照下列重量份数混合各成分： 3份醋酸钴， 750份氟化镍， 75份氟化铵， 32份 异丁醇， 15份水， 搅拌， 混合均匀， 再以 3-5g/L的浓度搅拌均匀配制成封孔剂。
[0026] 封孔处理工艺： 配制好封孔剂； 将封孔剂溶于水中配制成封孔剂溶液， 在封孔 剂溶液中封孔剂的含量为 5g/L; 将氧化后的型材浸入封孔剂溶液中， 控制封孔剂 溶液的 PH值在 5.5〜6.8范围内， 处理 10分钟后， 即在型材表面形成封闭氧化膜， 取出干燥。
[0027] 经过处理后的型材经过失重试验和观察型材表面， 发现失重结果符合标准 （即
< 30mg/dm 2)染色试验结果非常理想， 没有任何残留颜色。
[0028] 实施例 2
[0029] 按照下列重量份数混合各成分： 4份醋酸钴， 800份氟化镍， 80份氟化铵， 40份 异丁醇， 15份水， 搅拌， 混合均匀， 配制成封孔剂。
[0030] 封孔处理工艺： 配制好封孔剂； 将封孔剂溶于水中配制成封孔剂溶液， 在封孔 剂溶液中封孔剂的含量为 5g/L; 将型材浸入封孔剂溶液中， 控制封孔剂溶液的 P
H值在 5.5〜6.8范围内， 处理 10分钟后， 即在型材表面形成封闭氧化膜， 取出干 燥。
[0031] 经过处理后的型材经过失重试验和观察型材表面， 发现失重结果符合标准 （即
< 30mg/dm 2)染色试验结果非常理想， 没有任何残留颜色。
[0032] 实施例 3
[0033] 按照下列重量份数混合各成分： 5份醋酸钴， 900份氟化镍， 90份氟化铵， 50份 异丁醇， 15份水， 搅拌， 混合均匀， 配制成封孔剂。
[0034] 封孔处理工艺： 配制好封孔剂； 将封孔剂溶于水中配制成封孔剂溶液， 在封孔 剂溶液中封孔剂的含量为 4g/L; 将型材浸入封孔剂溶液中， 控制封孔剂溶液的 P H值在 5.5〜6.8范围内， 处理 10分钟后， 即在型材表面形成封闭氧化膜， 取出干 燥。
[0035] 经过处理后的型材经过失重试验和观察型材表面， 发现失重结果符合标准 （即
< 30mg/dm 2)染色试验结果非常理想， 没有任何残留颜色。
[0036] 实施例 4
[0037] 按照下列重量份数混合各成分： 5份醋酸钴， 1000份氟化镍， 100份氟化铵， 55 份异丁醇， 18份水， 搅拌， 混合均匀， 配制成封孔剂。
[0038] 封孔处理工艺： 配制好封孔剂； 将封孔剂溶于水中配制成封孔剂溶液， 在封孔 剂溶液中封孔剂的含量为 3g/L; 将型材浸入封孔剂溶液中， 控制封孔剂溶液的 P
H值在 5.5〜6.8范围内， 处理 15分钟后， 即在型材表面形成封闭氧化膜， 取出干 燥。
[0039] 经过处理后的型材经过失重试验和观察型材表面， 发现失重结果符合标准 （即
< 30mg/dm 2)染色试验结果非常理想， 没有任何残留颜色。
[0040] 实施例 5
[0041] 按照下列重量份数混合各成分： 6份醋酸钴， 1200份氟化镍， 120份氟化铵， 60 份异丁醇， 18份水， 搅拌， 混合均匀， 配制成封孔剂。
[0042] 封孔处理工艺： 配制好封孔剂； 将封孔剂溶于水中配制成封孔剂溶液， 在封孔 剂溶液中封孔剂的含量为 3g/L; 将型材浸入封孔剂溶液中， 控制封孔剂溶液的 P
H值在 5.5〜6.8范围内， 处理 15分钟后， 即在型材表面形成封闭氧化膜， 取出干 燥。
[0043] 经过处理后的型材经过失重试验和观察型材表面， 发现失重结果符合标准 （即
< 30mg/dm 2)染色试验结果非常理想， 没有任何残留颜色。
[0044] 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。

Claims

权利要求书
一种封孔剂， 其包括按照重量份数配比的下列成分：
醋酸钴或氟化钴 3-6
氟化镍 750-1200
氟化铵 75-120
异丁醇或聚二醇 32-60
水 15-18。
如权利要求 1所述的封孔剂， 其特征在于， 所述封孔剂包括重量份数 配比的下列成分：
氟化钴 3-6
氟化镍 750-1200
氟化铵 75-120
聚二醇 32-60
水 15-18。
如权利要求 1或 2所述的封孔剂， 其特征在于， 所述氟化镍的重量份数 为 750- 100。
如权利要求 1或 2所述的封孔剂， 其特征在于， 所述氟化铵的重量份数 为 75-100。
如权利要求 1所述的封孔剂， 其特征在于， 所述异丁醇或聚二醇的重 量份数为 32-50。
如权利要求 1所述的封孔剂， 其特征在于， 所述封孔剂为粉状固体。 一种型材表面封孔处理工艺， 其特征在于， 所述工艺包括如下步骤： 配制如权利要求 1-6任一项所述的封孔剂， 将封孔剂溶于水中并配制 成 3~5g/L的封孔剂溶液； 将型材浸入于封孔剂溶液中， 控制溶液的 P H值在 5.5〜6.8范围内， 处理 1-18分钟后， 即在型材表面形成封闭氧化
[权利要求 8] 如权利要求 7所述的型材表面封孔处理工艺， 其特征在于， 在封孔剂 溶液浸渍处理过程中， 控制封孔剂溶液中 Ni2+离子浓度为 0.8~1.2g/L ， F-离子浓度为 0.3~0.7g/L。
[权利要求 9] 如权利要求 7所述的型材表面封孔处理工艺， 其特征在于， 当溶液 PH 值过高吋， 用 1-5^%稀醋酸或 1-5^%稀氢氟酸调节其 PH值， 过低吋 用 l-5wt%稀氢氧化钠或 l-5wt%稀氨水溶液调节其 PH值。
[权利要求 10] 如权利要求 7所述的型材表面封孔处理工艺， 其特征在于， 所述封闭 氧化膜厚度形成速率为 0.8〜1.2 m/min。
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6247947B2 (zh) * 1984-05-29 1987-10-12 Usui Kokusai Sangyo Kk
CN101665970A (zh) * 2008-09-03 2010-03-10 中国科学院宁波材料技术与工程研究所 铝及铝合金阳极氧化膜常温封闭剂及封闭方法
CN102304743A (zh) * 2011-09-16 2012-01-04 南南铝业股份有限公司 一种铝及铝合金表面电化学氧化膜封孔方法
CN105200494A (zh) * 2015-09-24 2015-12-30 马鞍山杰创塑胶科技有限公司 一种易成膜抗菌铝合金阳极氧化膜无镍封孔剂及其制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6247947B2 (zh) * 1984-05-29 1987-10-12 Usui Kokusai Sangyo Kk
CN101665970A (zh) * 2008-09-03 2010-03-10 中国科学院宁波材料技术与工程研究所 铝及铝合金阳极氧化膜常温封闭剂及封闭方法
CN102304743A (zh) * 2011-09-16 2012-01-04 南南铝业股份有限公司 一种铝及铝合金表面电化学氧化膜封孔方法
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