CN108179410A - A kind of electronickelling chrome-free tanning agent and preparation method thereof - Google Patents

A kind of electronickelling chrome-free tanning agent and preparation method thereof Download PDF

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Publication number
CN108179410A
CN108179410A CN201711171672.9A CN201711171672A CN108179410A CN 108179410 A CN108179410 A CN 108179410A CN 201711171672 A CN201711171672 A CN 201711171672A CN 108179410 A CN108179410 A CN 108179410A
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Prior art keywords
parts
water
chrome
electronickelling
tanning agent
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CN201711171672.9A
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Chinese (zh)
Inventor
灏や负
尤为
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Wuxi Epic Technology Co Ltd
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Wuxi Epic Technology Co Ltd
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Priority to CN201711171672.9A priority Critical patent/CN108179410A/en
Publication of CN108179410A publication Critical patent/CN108179410A/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
    • C23C22/40Chemical 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
    • C23C22/42Chemical 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
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Treatment And Processing Of Natural Fur Or Leather (AREA)

Abstract

The present invention provides a kind of electronickelling chrome-free tanning agent and preparation method thereof, including being made of the component of following parts by weight:12 20 parts of acetic acid, 28 parts of sodium citrate, 3 10 parts of cobalt nitrate, 6 15 parts of sodium phosphate, 12 parts of phosphatase 24,16 parts of the potassium ferricyanide, 49 parts of sodium molybdate, 5 15 parts of water soluble persulfates, 300 1000 parts of water.Electronickelling provided by the invention is simple and environmentally-friendly with chrome-free tanning agent ingredient, without noxious materials such as Cr VIs, it is non-volatility gas and smell in passivating process, environmentally friendly, passivation speed is fast, passivation time only needs 5 10 seconds, electronickelling product after passivation has preferable corrosion resistance and inoxidizability, and surface is smooth, glossy.

Description

A kind of electronickelling chrome-free tanning agent and preparation method thereof
Technical field
The present invention relates to chrome-free tanning agent technical field more particularly to a kind of electronickelling chrome-free tanning agent and its preparation sides Method.
Background technology
Since chemical nickel plating and electronickelling have excellent hardness, wearability, corrosion resistance, electric conductivity and special magnetics etc. Comprehensive performance, so being widely used in the key areas such as automobile, oil, space flight, mechanized equipment, computer and electronic communication.But It is under air or corrosive environment, nickel plating surface easily forms the oxide or sulfide of nickel, this layer of oxide makes coating surface Metallic luster is lost, turns to be yellow dimmed or spot occurs, seriously affects the appearance of coating.For PCB fields, this layer of oxide Not only increase the contact resistance of nickel plating layer surface, also reduce the welding performance of nickel coating, influence wire bonding intensity and Reliability be easy to cause coming off for weldment.Thus, it will usually processing is passivated to nickel plating layer surface, to improve coating Corrosion resistance and inoxidizability can just put into production use.
The prior art is frequently with sexavalence chromium type passivator as passivator.But sexavalence chromium type passivator passivation effect is with sexavalence The changes of contents of chromium is larger, while passivation effect also less stable, and corrosion resistance is poor, can not effectively protect nickel layer surface. Simultaneously as hexavalent chromium compound is easily absorbed by the body, can human body be invaded by digestive system, respiratory tract, skin and mucous membrane, Therefore it is larger to environment and human body harm.Chrome-free tanning agent becomes one of direction of passivator Future Development.
In view of this, it is necessary to chrome-free tanning agent of the prior art be improved, to solve the above problems.
Invention content
The purpose of the present invention one is a kind of public electronickelling chrome-free tanning agent, and ingredient is simple and environmentally-friendly, without Cr VI etc. Noxious material, the non-volatile odorlessness of passivator, non-environmental-pollution in passivating process, the electronickelling after passivation have preferable anti-corrosion Property and inoxidizability, and be electroplated nickel surface it is smooth, glossy.
To achieve the above object, the present invention provides a kind of electronickelling chrome-free tanning agent, including by following parts by weight Component composition:12-20 parts of acetic acid, 2-8 parts of sodium citrate, 3-10 parts of cobalt nitrate, 6-15 parts of sodium phosphate, -12 parts of phosphatase 24, iron 1-6 parts of potassium cyanide, 4-9 parts of sodium molybdate, 5-15 parts of water soluble persulfates, 300-1000 parts of water.
In some embodiments, including being made of the component of following parts by weight:15 parts of acetic acid, 6 parts of sodium citrate, nitre Sour 7 parts of cobalt, 11 parts of sodium phosphate, 7 parts of phosphoric acid, 4 parts of the potassium ferricyanide, 6 parts of sodium molybdate, 13 parts of water soluble persulfates, 800 parts of water.
In some embodiments, the water soluble persulfates are water-soluble sodium peroxydisulfate or water-soluble potassium peroxydisulfate Or water-soluble ammonium persulfate.
The purpose of the present invention two is to disclose a kind of preparation method of electronickelling chrome-free tanning agent, is used to prepare ingredient letter Monocyclic guarantor, without noxious materials such as Cr VIs, the chromium-free deactivation of the non-volatile odorlessness of passivator, non-environmental-pollution in passivating process Agent.
To achieve the above object, the present invention provides a kind of preparation method of electronickelling chrome-free tanning agent, including as follows Step:
Step 1:Each component is weighed in parts by weight;
Step 2:Acetic acid, sodium citrate, sodium phosphate, phosphoric acid, sodium molybdate are sequentially added in water, stirred, mixing time is 30-40 minutes, agitator speed was 400-550 revs/min, and whipping temp is 20-25 DEG C;
Step 3:In mixture obtained by step 2, cobalt nitrate is added in, stirs evenly, sequentially adds the potassium ferricyanide, water Dissolubility persulfate, stirring, mixing time are 5-10 minutes, and agitator speed is 200-300 revs/min, then is warming up to 75- 95 DEG C, keep the temperature 10-15 minutes;
Step 4:Mixture obtained by step 3 is concentrated in vacuo 3-5 minutes, obtains chrome-free tanning agent.
Compared with prior art, the beneficial effects of the invention are as follows:Electronickelling provided by the invention chrome-free tanning agent ingredient It is simple and environmentally-friendly, without noxious materials such as Cr VIs, non-volatility gas and smell, environmentally friendly, passivation speed in passivating process Degree is fast, and passivation time only needs 5-10 seconds, and the electronickelling product after passivation has preferable corrosion resistance and inoxidizability, and surface It is smooth, glossy.
Specific embodiment
With reference to each embodiment, the present invention is described in detail, but it should explanation, these embodiments are simultaneously Non- limitation of the present invention, those of ordinary skill in the art are according in these embodiment institute work energy, method or structures Equivalent transformation or replacement, all belong to the scope of protection of the present invention within.
Embodiment one:
A kind of electronickelling chrome-free tanning agent is present embodiments provided, including being made of the component of following parts by weight:Second 12 parts of acid, 2 parts of sodium citrate, 3 parts of cobalt nitrate, 6 parts of sodium phosphate, phosphatase 24 part, 1 part of the potassium ferricyanide, 4 parts of sodium molybdate, water-soluble mistake 5 parts of sulfate, 300 parts of water.
The water soluble persulfates are water-soluble sodium peroxydisulfate.
Embodiment two:
A kind of electronickelling chrome-free tanning agent is present embodiments provided, including being made of the component of following parts by weight:Second 15 parts of acid, 6 parts of sodium citrate, 7 parts of cobalt nitrate, 11 parts of sodium phosphate, 7 parts of phosphoric acid, 4 parts of the potassium ferricyanide, 6 parts of sodium molybdate are water-soluble 13 parts of persulfate, 800 parts of water.
The water soluble persulfates are water-soluble potassium peroxydisulfate.
Embodiment three:
A kind of electronickelling chrome-free tanning agent is present embodiments provided, including being made of the component of following parts by weight:Second 20 parts of acid, 8 parts of sodium citrate, 10 parts of cobalt nitrate, 15 parts of sodium phosphate, 2 parts of phosphatase 11,6 parts of the potassium ferricyanide, 9 parts of sodium molybdate are water-soluble 15 parts of persulfate of property, 1000 parts of water.
The water soluble persulfates are water-soluble ammonium persulfate.
Example IV:
A kind of preparation method of electronickelling chrome-free tanning agent is present embodiments provided, is included the following steps:
Step 1:Each component is weighed in parts by weight;
Step 2:Acetic acid, sodium citrate, sodium phosphate, phosphoric acid, sodium molybdate are sequentially added in water, stirred, mixing time is 30-40 minutes, agitator speed was 400-550 revs/min, and whipping temp is 20-25 DEG C;Specifically, mixing time is 35 points Clock, agitator speed are 480 revs/min, and whipping temp is 23 DEG C;
Step 3:In mixture obtained by step 2, cobalt nitrate is added in, stirs evenly, sequentially adds the potassium ferricyanide, water Dissolubility persulfate, stirring, mixing time are 5-10 minutes, and agitator speed is 200-300 revs/min, then is warming up to 75- 95 DEG C, keep the temperature 10-15 minutes;Specifically, mixing time is 8 minutes, and agitator speed is 250 revs/min, then is warming up to 80 DEG C, keep the temperature 12 minutes;
Step 4:Mixture obtained by step 3 is concentrated in vacuo 3-5 minutes, obtains chrome-free tanning agent, specifically, is concentrated in vacuo 4 minutes.
The performance parameter of chrome-free tanning agent is as shown in the table obtained by each embodiment:
Embodiment one Embodiment two Embodiment three
Anti-corrosion number of days 40 35 48
Appearance It is smooth, it is glossy It is smooth, it is glossy It is smooth, it is glossy
Adhesive force Level-one Level-one Level-one
Salt fog resistance It is excellent It is excellent It is excellent
Cross cut test It is qualified It is qualified It is qualified
Those listed above is a series of to be described in detail only for feasibility embodiment of the invention specifically Bright, they are not to limit the scope of the invention, all equivalent implementations made without departing from skill spirit of the present invention Or change should all be included in the protection scope of the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should It considers the specification as a whole, the technical solutions in each embodiment can also be properly combined.

Claims (4)

1. a kind of electronickelling chrome-free tanning agent, which is characterized in that including being made of the component of following parts by weight:Acetic acid 12- 20 parts, 2-8 parts of sodium citrate, 3-10 parts of cobalt nitrate, 6-15 parts of sodium phosphate, -12 parts of phosphatase 24,1-6 parts of the potassium ferricyanide, sodium molybdate 4-9 parts, 5-15 parts of water soluble persulfates, 300-1000 parts of water.
2. electronickelling chrome-free tanning agent according to claim 1, which is characterized in that including the group by following parts by weight It is grouped as:15 parts of acetic acid, 6 parts of sodium citrate, 7 parts of cobalt nitrate, 11 parts of sodium phosphate, 7 parts of phosphoric acid, 4 parts of the potassium ferricyanide, sodium molybdate 6 Part, 13 parts of water soluble persulfates, 800 parts of water.
3. electronickelling chrome-free tanning agent according to claim 2, which is characterized in that the water soluble persulfates are water Dissolubility sodium peroxydisulfate either water-soluble potassium peroxydisulfate or water-soluble ammonium persulfate.
4. a kind of preparation method of electronickelling chrome-free tanning agent as described in any one of claim 1-3, which is characterized in that Include the following steps:
Step 1:Each component is weighed in parts by weight;
Step 2:Acetic acid, sodium citrate, sodium phosphate, phosphoric acid, sodium molybdate are sequentially added in water, stirred, mixing time 30- 40 minutes, agitator speed was 400-550 revs/min, and whipping temp is 20-25 DEG C;
Step 3:In mixture obtained by step 2, cobalt nitrate is added in, stirs evenly, sequentially adds the potassium ferricyanide, water solubility Persulfate, stirring, mixing time are 5-10 minutes, and agitator speed is 200-300 revs/min, then is warming up to 75-95 DEG C, Heat preservation 10-15 minutes;
Step 4:Mixture obtained by step 3 is concentrated in vacuo 3-5 minutes, obtains chrome-free tanning agent.
CN201711171672.9A 2017-11-22 2017-11-22 A kind of electronickelling chrome-free tanning agent and preparation method thereof Withdrawn CN108179410A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109778170A (en) * 2019-01-30 2019-05-21 北方民族大学 The treatment fluid and film layer preparation method of Mg alloy surface iron cyanide chemical composition coating

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Publication number Priority date Publication date Assignee Title
CN104388920A (en) * 2014-11-12 2015-03-04 华南理工大学 Chromate-free passivation method for chemically-plated Ni-P coating
CN104404488A (en) * 2014-11-14 2015-03-11 无锡伊佩克科技有限公司 Aluminum alloy chromium-free passivating agent and preparation method thereof
CN105839093A (en) * 2016-05-31 2016-08-10 太原工业学院 Normal-temperature chromium-free passivation liquid for electroplated copper and passivation technology of normal-temperature chromium-free passivation liquid
CN105839099A (en) * 2016-05-19 2016-08-10 华南理工大学 Chromate-free passivation treating agent for nickel-plated surface and treating process
CN107313101A (en) * 2017-06-08 2017-11-03 华南理工大学 A kind of preparation method of environmentally friendly nickel envelope chromium-free deactivation layer

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Publication number Priority date Publication date Assignee Title
CN104388920A (en) * 2014-11-12 2015-03-04 华南理工大学 Chromate-free passivation method for chemically-plated Ni-P coating
CN104404488A (en) * 2014-11-14 2015-03-11 无锡伊佩克科技有限公司 Aluminum alloy chromium-free passivating agent and preparation method thereof
CN105839099A (en) * 2016-05-19 2016-08-10 华南理工大学 Chromate-free passivation treating agent for nickel-plated surface and treating process
CN105839093A (en) * 2016-05-31 2016-08-10 太原工业学院 Normal-temperature chromium-free passivation liquid for electroplated copper and passivation technology of normal-temperature chromium-free passivation liquid
CN107313101A (en) * 2017-06-08 2017-11-03 华南理工大学 A kind of preparation method of environmentally friendly nickel envelope chromium-free deactivation layer

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109778170A (en) * 2019-01-30 2019-05-21 北方民族大学 The treatment fluid and film layer preparation method of Mg alloy surface iron cyanide chemical composition coating

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