CN107475705A - A kind of ordinary steel application substrate passivator and preparation method thereof - Google Patents
A kind of ordinary steel application substrate passivator and preparation method thereof Download PDFInfo
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- CN107475705A CN107475705A CN201710824285.4A CN201710824285A CN107475705A CN 107475705 A CN107475705 A CN 107475705A CN 201710824285 A CN201710824285 A CN 201710824285A CN 107475705 A CN107475705 A CN 107475705A
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- passivator
- ordinary steel
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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
- C23C22/46—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 oxalates
- C23C22/47—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 oxalates containing also phosphates
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- Chemical Treatment Of Metals (AREA)
Abstract
The invention discloses a kind of ordinary steel application substrate passivator and preparation method thereof, belong to field of metal surface treatment technology, it is characterised in that include the component of following mass percent：Sodium dihydrogen phosphate 0.5 1.5%, sodium chloride 10 15%, oxalic acid 15 20%, ammonium oxalate 0.3 0.7%, graphene dispersing solution 1 5%, surplus is deionized water；Its preparation process prepares graphene dispersing solution using mechanical stripping method first, is then added to graphene dispersing solution in the passivator basal liquid being made up of sodium dihydrogen phosphate, sodium chloride, oxalic acid, ammonium oxalate；The passivation of the present invention is tied to form a cheap, nontoxic Chrome-free, suitable for ordinary steel application substrate, can increase substantially corrosion resistance, salt fog resistance and adhesive force after ordinary steel application.
Description
Technical field
The present invention relates to field of metal surface treatment technology, and in particular to a kind of ordinary steel application substrate passivator and its
Preparation method.
Background technology
For steel-iron components after machine-shaping, its surface-active is very high, it is easy to is corroded, has a strong impact on that its is attractive in appearance
And service life, therefore steel and iron parts usually require to be passivated processing, metal surface is generated diaphragm, slow down corrosion.Tradition
Passivation Treatment generally use chromate and metal function its Surface Creation chromium parent metal mixture oxide membranous layer, but
Chromic acid and its salt have very high toxicity and strong carcinogenicity, and the wastewater treatment containing Cr VI is complex, therefore to ring
Serious pollution is caused in border, and with the gradual enhancing of environmental consciousness, the use of chromic acid and its salt will be by strict resistance system.Mesh
The preceding replacement for sexavalence chromium passivating mainly has two kinds of chromium-free deactivation and trivalent chromium passivation, wherein, chromium-free deactivation generally use titanium
Hydrochlorate, molybdate, rare earth, silicate etc., but shortcoming is that outward appearance and corrosion resistance are bad, and trivalent chromium passivator is to use organic complex
Agent, and other metals are added, corrosion resistance is improved, hole sealing agent is added in passivating solution in addition, is allowed to be filled into passivating film skeleton,
Overcome the shortcomings that trivalent chromium passivation is without self-healing ability.
In the prior art, the Chinese invention patent of Application No. 201410120126.2 discloses a kind of electrodeposited chromium steel and iron parts
With passivation treating agent, its component includes potassium hydroxide, chromic nitrate, n-octaldehyde, graphene, malonic acid, oxalic acid, silica gel load sulfuric acid
Zirconium and the tert-butyl alcohol, effectively it is passivated composition and uses chromic nitrate and oxalic acid, although trivalent chromium passivator has reached quality requirement, corrosion resistant
Erosion, but the potential hazard of heavy metal chromium still be present, and also the system employs substantial amounts of catalyst and the tertiary fourth of toxic solvents
Alcohol, manufacturing cost is higher, is particularly unsuitable for ordinary steel application substrate use.Phytic acid and the organic matter passivating solution feature of environmental protection are good, no weight
Metal ion treatment problem, but corrosion resistance is poor.Therefore, cheap, the environment-protecting and non-poisonous ordinary steel application of cost is lacked at present
Substrate passivator.
The content of the invention
The technical problems to be solved by the invention are in view of the shortcomings of the prior art, there is provided a kind of cost is cheap, nontoxic nothing
Ordinary steel application substrate passivator of the environment-friendly type of chromium and preparation method thereof.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：A kind of ordinary steel application substrate passivator, it is special
Sign is, includes the component of following mass percent：Sodium dihydrogen phosphate 0.5-1.5%, sodium chloride 10-15%, oxalic acid 15-20%, grass
Sour ammonium 0.3-0.7%, graphene dispersing solution 1-5%, surplus are deionized water.
Further, the ordinary steel application substrate includes the component of following mass percent with passivator：Biphosphate
Sodium 0.8-1.5%, sodium chloride 12-15%, oxalic acid 18-20%, ammonium oxalate 0.5-0.7%, graphene dispersing solution 3-5%, surplus for go from
Sub- water.
Further, the ordinary steel application substrate includes the component of following mass percent with passivator：Biphosphate
Sodium 0.8%, sodium chloride 12%, oxalic acid 18%, ammonium oxalate 0.5%, graphene dispersing solution 3%, surplus are deionized water, this ratio formula
Strong bonded between graphene-oxalic acid-aluminum metal in lower passivation system, and the Ionization Chamber of oxalate denominationby is matched somebody with somebody with the passivation system
5 property are more preferable so that passivation system is more coated on metal surface even compact.
Further, the concentration of the graphene dispersing solution is 1-10mg/ml, the solvent of graphene dispersing solution using go from
Sub- water.
And a kind of preparation method of ordinary steel application substrate passivator as described above, it is characterised in that including as follows
Step：
（1）It is dissolved in 0.5-2 part dispersants are agitated in 85-90 part deionized waters；
（2）By 1-5 part expanded graphites add to（1）In, 1-60min is peeled off under high-speed shearing machine 8000-12000r/min, is obtained mixed
Close liquid；
（3）Separated after above-mentioned mixed liquor is stood, obtain upper strata graphene dispersing solution；
（4）Sodium dihydrogen phosphate, sodium chloride, oxalic acid, ammonium oxalate are dissolved in proportion respectively in deionized water, passivator base is made
Plinth liquid；
（5）Graphene dispersing solution is taken to be proportionally added into passivator basal liquid, dispersion mixing 1-3 is small under high speed dispersor normal temperature
When, ordinary steel application substrate passivator is obtained, during adding graphene dispersing solution into passivator basal liquid, at a high speed
Under peptizaiton, graphene is combined with a carboxyl in oxalic acid, graphene is uniformly distributed in securely with lamellar structure
In passivator basal liquid, another carboxyl in oxalic acid forms lubricity then as the active group chelated with ordinary steel Base Metal
Passivator good, metallic cohesion is strong.
Further, the step（1）In dispersant using SDS, CTAB, CMC, sodium alginate, carboxymethyl cellulose
It is more than one or both of sodium, methylcellulose, polyvinyl alcohol, PVP etc..
Further, the step（2）The rotating speed of high speed cutter is 8000-12000r/min.
Further, the step（5）The rotating speed of high speed dispersion machine is 2000-4000r/min.
The beneficial effects of the invention are as follows：
1. the nontoxic Chrome-free of each component of the present invention, using oxalic acid as main deactivation matter, ammonium oxalate is auxiliary deactivation matter, blunt in oxalic acid
Add graphene in change system, oxalic acid contains 2 carboxyls, one end connection graphene, the other end and metal chelant, under synergy
The Chrome-free base passivation film of densification is formed in common steel surface；
2. ammonium oxalate as auxiliary film forming matter, can carry out different degrees of ionization according to the content of system oxalate, and then
Reach the purpose of control reaction speed so that passivating film is finer and close；
3. sodium dihydrogen phosphate is pH buffer, can with reaction carry out cushioning effect is played to the pH of system, to passivating process
Acid environment-guarantee is provided；
4. mutually acted synergistically between the oxalic acid, ammonium oxalate, graphene, sodium dihydrogen phosphate each component in passivation system of the present invention, greatly
Amplitude improves corrosion resistance, salt fog resistance and the adhesive force after ordinary steel application, and cost is cheap, and the feature of environmental protection is good, suitable for common
Steel application substrate.
Embodiment
Embodiment 1
A kind of ordinary steel application substrate passivator, include the component of following mass percent：Sodium dihydrogen phosphate 0.5%, sodium chloride
10%, oxalic acid 15%, ammonium oxalate 0.3%, graphene dispersing solution 1%, surplus is deionized water.
The preparation method of the present embodiment ordinary steel application substrate passivator comprises the following steps：
（1）It is dissolved in 0.5 part of dispersant SDS is agitated in 90 parts of deionized waters；
（2）By 5 parts of expanded graphites add to（1）In, high-speed shearing machine 12000r/min peels off 1min, obtains mixed liquor；
（3）Separated after above-mentioned mixed liquor is stood, obtain the graphene dispersing solution that upper strata concentration is 1mg/ml；
（4）Sodium dihydrogen phosphate, sodium chloride, oxalic acid, ammonium oxalate are dissolved in proportion respectively in deionized water, passivator base is made
Plinth liquid；
（5）Graphene dispersing solution is taken to be proportionally added into passivator basal liquid, 2000r/min disperses under high speed dispersor normal temperature
Mixing 1 hour, obtains ordinary steel application substrate passivator.
Embodiment 2
A kind of ordinary steel application substrate passivator, include the component of following mass percent：Sodium dihydrogen phosphate 1.5%, sodium chloride
15%, oxalic acid 20%, ammonium oxalate 0.7%, graphene dispersing solution 5%, surplus is deionized water.
The preparation method of the present embodiment ordinary steel application substrate passivator comprises the following steps：
（1）It is dissolved in 1 part of dispersant sodium alginate is agitated in 85 parts of deionized waters；
（2）By 1 part of expanded graphite add to（1）In, high-speed shearing machine 8000r/min peels off 60min, obtains mixed liquor；
（3）Separated after above-mentioned mixed liquor is stood, obtain the graphene dispersing solution that upper strata concentration is 10mg/ml；
（4）Sodium dihydrogen phosphate, sodium chloride, oxalic acid, ammonium oxalate are dissolved in proportion respectively in deionized water, passivator base is made
Plinth liquid；
（5）Graphene dispersing solution is taken to be proportionally added into passivator basal liquid, 4000r/min disperses under high speed dispersor normal temperature
Mixing 3 hours, obtains ordinary steel application substrate passivator.
Embodiment 3
A kind of ordinary steel application substrate passivator, include the component of following mass percent：Sodium dihydrogen phosphate 0.8%, sodium chloride
12%, oxalic acid 18%, ammonium oxalate 0.5%, graphene dispersing solution 3%, surplus is deionized water.
The preparation method of the present embodiment ordinary steel application substrate passivator comprises the following steps：
（1）It is dissolved in 2 parts of polyethylene of dispersing agent alcohol are agitated in 90 parts of deionized waters；
（2）By 3 parts of expanded graphites add to（1）In, high-speed shearing machine 10000r/min peels off 30min, obtains mixed liquor；
（3）Separated after above-mentioned mixed liquor is stood, obtain the graphene dispersing solution that upper strata concentration is 5mg/ml；
（4）Sodium dihydrogen phosphate, sodium chloride, oxalic acid, ammonium oxalate are dissolved in proportion respectively in deionized water, passivator base is made
Plinth liquid；
（5）Graphene dispersing solution is taken to be proportionally added into passivator basal liquid, 3000r/min disperses under high speed dispersor normal temperature
Mixing 2 hours, obtains ordinary steel application substrate passivator.
Comparative example 1
Using 3% oxalic acid stoste as passivator.
Comparative example 2
With embodiment 3, except that being not added with graphene dispersing solution.
Comparative example 3
With embodiment 3, except that being not added with ammonium oxalate.
Comparative example 4
With embodiment 3, except that being not added with ammonium oxalate and graphene dispersing solution.
Comparative example 5
With embodiment 3, except that the sodium dihydrogen phosphate in component is replaced with into tertiary sodium phosphate.
Comparative example 6
With embodiment 3, except that the sodium dihydrogen phosphate in component is replaced with into sodium acid carbonate.
Above-described embodiment and comparative example are fitted into deactivation slot, the steel plate after polishing is cleaned is soaked into deactivation slot
In 5min, steel plate is taken out after washing drying again, corrosion resistance, salt fog resistance and adhesive force test is carried out respectively, wherein anti-corrosion
Property testing standard with reference to GBT 10834-2008, salt fog resistance testing standard is with reference to GBT 10125-2012, adhesive force test ginseng
According to GB1720-79 (89).Test result is shown in Table 1.
The test result of table 1
| Corrosion resistance | Salt fog resistance | Adhesive force | |
| Embodiment 1 | 278h starts to corrode | 126h starts to corrode | 0 grade |
| Embodiment 2 | 295h starts to corrode | 167h starts to corrode | 0 grade |
| Embodiment 3 | 338h starts to corrode | 196h starts to corrode | 0 grade |
| Comparative example 1 | 106h starts to corrode | 53h starts to corrode | 2 grades |
| Comparative example 2 | 154h starts to corrode | 67h starts to corrode | 1 grade |
| Comparative example 3 | 167h starts to corrode | 81h starts to corrode | 2 grades |
| Comparative example 4 | 128h starts to corrode | 65h starts to corrode | 3 grades |
| Comparative example 5 | 8h starts to corrode | 9h starts to corrode | 5 grades |
| Comparative example 6 | 6h starts to corrode | 3h starts to corrode | 5 grades |
From the data in table 1, it can be seen that compared with prior art, anti-corrosion time, salt-fog resistant time and the passivating film of the embodiment of the present invention
Adhesive force have conspicuousness raising, especially sodium dihydrogen phosphate 0.8%, sodium chloride 12%, oxalic acid 18%, ammonium oxalate 0.5%, graphite
Passivator under alkene dispersion liquid 3%, balance deionized water formula, there is significant creative feature.Comparative example 1 is with oxalic acid stoste
To be passivated system, corrosion resistance and salt fog resistance effect are poor, though because oxalic acid has passivation effect, pure oxalic acid solution
Slow in passivation of metal surfaces, effect is poor；Graphene dispersing solution is not added with comparative example 2, the hole of passivating film cannot improve, and cause
Close property is poor, and anti-corrosion and salt tolerant fog effect certainly will be bad；Film forming auxiliary substance is not added with comparative example 3, passivating film can be caused slightly
Defect, compactness are affected, and passivation effect is poor；Auxiliary film forming matter and graphene, passivating film hole are not added in comparative example 4
More, anti-corrosion effect is also poor；Sodium dihydrogen phosphate is replaced with into tertiary sodium phosphate in comparative example 5, because sodium dihydrogen phosphate is blunt at this
PH buffer is used as in change system, and tertiary sodium phosphate is almost completely decomposed into disodium hydrogen phosphate and sodium hydroxide in water, belongs to
Strong base-weak acid salt, therefore passivating film can not be formed in the basic conditions；Sodium dihydrogen phosphate is replaced with into bicarbonate in comparative example 6
Sodium, sodium acid carbonate is also strong base-weak acid salt, and oxalic acid etc. is faintly acid, can not be passivated film forming in the basic conditions.
The present invention is without using component containing chromium, and using oxalic acid as main deactivation matter, ammonium oxalate is auxiliary deactivation matter, and oxalic acid contains
There are 2 carboxyls, one end connection graphene, the other end and metal chelant, form the blunt of densification in common steel surface under synergy
Change film, ammonium oxalate can carry out different degrees of ionization, Jin Erda as auxiliary film forming matter according to the content of system oxalate
To the purpose of control reaction speed so that passivating film is finer and close, and sodium dihydrogen phosphate is pH buffer, can be carried out pair with reaction
The pH of system plays cushioning effect, and acid environment-guarantee, therefore, the grass in passivation system of the present invention are provided to passivating process
Synergy between acid, ammonium oxalate, graphene, sodium dihydrogen phosphate each component be present so that the corrosion resistance of passivator, salt fog resistance and
Adhesive force is obviously improved.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changed, replacing and modification.
Claims (8)
1. a kind of ordinary steel application substrate passivator, it is characterised in that include the component of following mass percent：Biphosphate
Sodium 0.5-1.5%, sodium chloride 10-15%, oxalic acid 15-20%, ammonium oxalate 0.3-0.7%, graphene dispersing solution 1-5%, surplus for go from
Sub- water.
2. ordinary steel application substrate passivator according to claim 1, it is characterised in that including following mass percent
Component：Sodium dihydrogen phosphate 0.8-1.5%, sodium chloride 12-15%, oxalic acid 18-20%, ammonium oxalate 0.5-0.7%, graphene dispersion
Liquid 3-5%, surplus are deionized water.
3. ordinary steel application substrate passivator according to claim 2, it is characterised in that including following mass percent
Component：Sodium dihydrogen phosphate 0.8%, sodium chloride 12%, oxalic acid 18%, ammonium oxalate 0.5%, graphene dispersing solution 3%, surplus for go from
Sub- water.
4. the ordinary steel application substrate passivator according to claim any one of 1-3, it is characterised in that the graphene
The concentration of dispersion liquid is 1-10mg/ml, and the solvent of graphene dispersing solution uses deionized water.
5. a kind of preparation method of ordinary steel application substrate passivator as described in claim any one of 1-3, its feature exist
In comprising the following steps：
（1）It is dissolved in 0.5-2 part dispersants are agitated in 85-90 part deionized waters；
（2）By 1-5 part expanded graphites add to（1）In, 1-60min is peeled off under high-speed shearing machine 8000-12000r/min, is obtained mixed
Close liquid；
（3）Separated after above-mentioned mixed liquor is stood, obtain upper strata graphene dispersing solution；
（4）Sodium dihydrogen phosphate, sodium chloride, oxalic acid, ammonium oxalate are dissolved in proportion respectively in deionized water, passivator base is made
Plinth liquid；
（5）Graphene dispersing solution is taken to be proportionally added into passivator basal liquid, dispersion mixing 1-3 is small under high speed dispersor normal temperature
When, obtain ordinary steel application substrate passivator.
6. the preparation method of ordinary steel application substrate passivator according to claim 5, it is characterised in that the step
（1）In dispersant using SDS, CTAB, CMC, sodium alginate, sodium carboxymethylcellulose, methylcellulose, polyvinyl alcohol, poly-
Tie up more than one or both of ketone etc..
7. the preparation method of ordinary steel application substrate passivator according to claim 5, it is characterised in that the step
（2）The rotating speed of high speed cutter is 8000-12000r/min.
8. the preparation method of ordinary steel application substrate passivator according to claim 5, it is characterised in that the step
（5）The rotating speed of high speed dispersion machine is 2000-4000r/min.
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Cited By (3)
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| CN108570672A (en) * | 2018-05-08 | 2018-09-25 | 湖北安登环保科技有限公司 | A method of forming the Chrome-free film forming of oxidation film on aluminum or aluminum alloy surface |
| CN111155076A (en) * | 2020-01-14 | 2020-05-15 | 山东建筑大学 | Process for preparing metal phosphating film based on ultrasonic waves |
| CN114622195A (en) * | 2022-02-21 | 2022-06-14 | 华鼎国联四川动力电池有限公司 | Method for passivating zinc matrix |
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| CN108570672A (en) * | 2018-05-08 | 2018-09-25 | 湖北安登环保科技有限公司 | A method of forming the Chrome-free film forming of oxidation film on aluminum or aluminum alloy surface |
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| CN114622195A (en) * | 2022-02-21 | 2022-06-14 | 华鼎国联四川动力电池有限公司 | Method for passivating zinc matrix |
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Application publication date: 20171215 |