CN104962899A - Phosphorus-free graphene-oxide-containing metal surface pretreatment solution and application method thereof - Google Patents
Phosphorus-free graphene-oxide-containing metal surface pretreatment solution and application method thereof Download PDFInfo
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- CN104962899A CN104962899A CN201510422597.3A CN201510422597A CN104962899A CN 104962899 A CN104962899 A CN 104962899A CN 201510422597 A CN201510422597 A CN 201510422597A CN 104962899 A CN104962899 A CN 104962899A
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Abstract
The invention provides a phosphorus-free graphene-oxide-containing metal surface pretreatment solution and an application method thereof. The phosphorus-free graphene-oxide-containing metal surface pretreatment solution comprises the following components in percentage by weight: 1-2% of fluosilicic acid, 0.2-1% of sodium molybdate, 1-2% of sodium nitrate, 0.6-1.2% of metal surface oxidizer, 1-2% of disodium edetate, 0.8-1.5% of tartaric acid, 0.1-0.3% of graphene oxide and the balance of water, totaling 100%. The product has the advantages of stable and excellent properties and wide application range. The added graphene oxide can effectively enhance the paint film adhesion of the conversion coating.
Description
Technical field
The invention discloses a kind of without phosphorus environmentally friendly metal surface treating liquid that with the addition of graphene oxide, belong to pre-treatment field, metallic surface.
Background technology
Now, the metallic substance such as iron and steel are widely used in antitheft door, mechanical workout, automobile, ship industry etc. and are related in the industry of national economy, and metal pre-treatment is a procedure indispensable in process of metal working.At present, contain a large amount of heavy metals in widely used Phosphating Solution in metallic surface pre-treatment industry, and in use can produce a large amount of phosphatization waste residues, cause serious environmental problem, therefore the use of Phosphating Solution has been subjected to more and more stricter restriction.Along with society is to the concern of environment protection, metal pre-treatment industry can be increasing for the demand of phosphate-free metal surface treatment liquid, and the without phosphorus pre-treatment product of exploitation excellent performance and technique have become the inexorable trend of industry development.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of stable, excellent performance, widely applicable environment-friendly type metal surface prefinished products.Modified graphene oxide add the paint film adhesion that effectively can improve conversion film.This product using method is simple, in use produces without sediment, economy, environmental protection.
The present invention is achieved by the following technical solutions, a kind of without phosphorus containing graphene oxide metallic surface pretreatment liquid, its component and weight percentage are: in weight part for 100%, silicofluoric acid 1-2%, Sodium orthomolybdate 0.2%-1%, SODIUMNITRATE 1%-2%, oxidation on metal surface agent 0.6%-1.2%, disodium ethylene diamine tetraacetate 1%-2%, tartrate 0.8%-1.5%, graphene oxide 0.1-0.3%, surplus is water.
Preferred component and weight percentage are: in weight part for 100%, silicofluoric acid 1-2%, Sodium orthomolybdate 0.5%-0.8%, SODIUMNITRATE 1.2%-1.6%, oxidation on metal surface agent 1%-1.2%, disodium ethylene diamine tetraacetate 1.7%-2%, tartrate 0.8%-1%, graphene oxide 0.1-0.3%, surplus is water.
Preferred oxidation on metal surface agent is sodium chlorate, m-nitrobenzene sodium sulfonate, hydrogen peroxide or oxammonium sulfate.
As one of optimal way of the present invention, be 100% by weight, comprise following component: silicofluoric acid 1%, Sodium orthomolybdate 0.5%, SODIUMNITRATE 1%, sodium chlorate 1.0%, disodium ethylene diamine tetraacetate 1%, tartrate 0.8%, graphene oxide 0.1%, surplus is water.
As one of optimal way of the present invention, be 100% by weight, comprise following component: silicofluoric acid 1.5%, Sodium orthomolybdate 0.2%, SODIUMNITRATE 1.2%, m-nitrobenzene sodium sulfonate 1.2%, disodium ethylene diamine tetraacetate 1.3%, tartrate 1.0%, graphene oxide 0.2%, surplus is water.
As one of optimal way of the present invention, be 100% by weight, comprise following component: silicofluoric acid 2%, Sodium orthomolybdate 0.8%, SODIUMNITRATE 1.6%, sodium chlorate 0.6%, disodium ethylene diamine tetraacetate 1.7%, tartrate 1.5%, graphene oxide 0.2%, surplus is water.
As one of optimal way of the present invention, be 100% by weight, comprise following component: silicofluoric acid 1.5%, Sodium orthomolybdate 0.5%, SODIUMNITRATE 1.6%, oxammonium sulfate 1%, disodium ethylene diamine tetraacetate 2%, tartrate 1.5%, graphene oxide 0.2%, surplus is water.
As one of optimal way of the present invention, be 100% by weight, comprise following component: silicofluoric acid 2%, Sodium orthomolybdate 1%, SODIUMNITRATE 2%, hydrogen peroxide 1.2%, disodium ethylene diamine tetraacetate 2%, tartrate 1.5%, graphene oxide 0.3%, surplus is water.
The using method of a kind of universal metallic surface of high anti-corrosion environmental protection of the present invention pretreatment liquid, step is as follows: after carrying out oil removing, washing, pickling, secondary washing process to pending metallic surface, be soaked in the pretreatment liquid of described metallic surface at normal temperatures, naturally dry after the metal washing after immersion or dry, namely completing metal finishing.
The present invention has the following advantages compared to prior art: not phosphorous in (1) this product, can well solve the problem of the rich phosphorus pollution that now widely used Phosphating Solution causes; (2) cause the heavy metal of Heavy environmental pollution in this product without nickel, chromium etc., effectively can alleviate the heavy metal contamination in metal pre-treatment industry; (3) do not contain nitrite in this product, effectively can reduce Phosphating Solution in use to the Health hazard of site operation personnel; (4) this product is in use without the generation of sediment, greatly reduces the environmental protection cost in use of client.
Embodiment
Below by specific embodiment, the present invention will be further described, but be not limited thereto.
Raw material described in embodiment is convenient source, commercial products.
Of the present invention without phosphorus containing graphene oxide metallic surface pretreatment liquid, its component and weight part, be 100%, silicofluoric acid 1-2%, Sodium orthomolybdate 0.2%-1% by weight, SODIUMNITRATE 1%-2%, oxidation on metal surface agent 0.6%-1.2%, disodium ethylene diamine tetraacetate 1%-2%, tartrate 0.8%-1.5%, graphene oxide 0.1-0.3%, surplus is water.
Preferred component and weight percentage are further: in weight part for 100%, silicofluoric acid 1-2%, Sodium orthomolybdate 0.5%-0.8%, SODIUMNITRATE 1.2%-1.6%, oxidation on metal surface agent 1%-1.2%, disodium ethylene diamine tetraacetate 1.7%-2%, tartrate 0.8%-1%, graphene oxide 0.1-0.3%, surplus is water.
Described oxidation on metal surface agent is sodium chlorate, m-nitrobenzene sodium sulfonate, hydrogen peroxide or oxammonium sulfate.
The metallic surface pretreatment liquid of the present invention's preparation is colourless transparent liquid, and pH is between 1.8 to 4.Cold-reduced sheet is that available product of the present invention carries out processing (soaking or spray) after oil removing, washing, and the time is 2-5 minute.Cold-reduced sheet surface presentation through treatment solution process disclosed in this invention is uniform yellow to blue membrane.The cold-reduced sheet got rusty in a large number needs to carry out acid pickling and rust removing operation.Workpiece after rust cleaning is through this product process (soaking or spray) 2-5 minute, and Surface Creation mazarine is to the even rete of grey black.
Treatment solution disclosed by the invention is in use adjusted to film quality mainly through control ph.The pH value of the treatment solution of new preparation is about 1.8, and along with the increasing of quantity of process workpiece, pH can progressively rise, and when pH value is elevated to more than 4, there will be the phenomenon that film forming is uneven.In use answer control ph between 1.8 to 4.
In the present invention, each component is mutually promoted, synergy.Adding of silicofluoric acid makes the acidity of this product be middle strong acid, first the gas-evolving electrodes of metal can be there is when ferrous materials is immersed in film forming liquid, cause the ionization equilibrium of silicofluoric acid to move right, the silicon-dioxide that hydrolysis produces effectively can be deposited on steel surface.SODIUMNITRATE effectively can promote the generation of evolving hydrogen reaction as oxygenant, accelerates the sedimentation velocity of silicon-dioxide, increases the thickness of silicon dioxide film.And Sodium orthomolybdate and adding of oxidation on metal surface agent can be the passivation effects that steel surface produces to a certain degree while silica deposit, improve the corrosion resistance nature of silicon dioxide film.Effectively can improve the adsorption of graphene oxide simultaneously, strengthen the paint film adhesion performance of conversion film.Disodium ethylene diamine tetraacetate, adding of the complexing agents such as tartrate can play stable tank liquor, the effect increased the service life.Each component in product can be mutually promoted in the concentration range of defined, jointly plays a role, and forms the chemical conversion film of excellent effect.
embodiment 1
With the addition of a without phosphorus environmentally friendly metal surface treating liquid for graphene oxide, raw materials quality per-cent is as follows:
Silicofluoric acid 1%, Sodium orthomolybdate 0.5%, SODIUMNITRATE 1%, sodium chlorate 1.0%, disodium ethylene diamine tetraacetate 1%, tartrate 0.8%, graphene oxide 0.1%, surplus is water.
Process cold-reduced sheet surface after the treatment solution of the present embodiment is prepared (pH=1.8), step is as follows:
(1) oil removing is carried out to cold-reduced sheet surface, washing, pickling, secondary washing;
(2) cold-reduced sheet after step (1) being processed under normal temperature is placed in treatment solution immersion treatment 5 minutes;
(3) the cold-reduced sheet washing post-drying after step (2) being processed, namely completes surface treatment.
embodiment 2
With the addition of a without phosphorus environmentally friendly metal surface treating liquid for graphene oxide, raw materials quality per-cent is as follows:
Silicofluoric acid 1.5%, Sodium orthomolybdate 0.2%, SODIUMNITRATE 1.2%, m-nitrobenzene sodium sulfonate 1.2%, disodium ethylene diamine tetraacetate 1.3%, tartrate 1.0%, graphene oxide 0.2%, surplus is water.
Process cold-reduced sheet surface after the treatment solution of the present embodiment being prepared (pH=1.8), step is as follows:
(1) oil removing is carried out to cold-reduced sheet surface, washing, pickling, secondary washing;
(2) cold-reduced sheet after step (1) being processed under normal temperature is placed in treatment solution immersion treatment 4 minutes;
(3) the cold-reduced sheet washing post-drying after step (2) being processed, namely completes surface treatment.
embodiment 3
That with the addition of graphene oxide, a without phosphorus environmentally friendly metal surface treating liquid, raw materials quality per-cent is as follows:
Silicofluoric acid 2%, Sodium orthomolybdate 0.8%, SODIUMNITRATE 1.6%, sodium chlorate 0.6%, disodium ethylene diamine tetraacetate 1.7%, tartrate 1.5%, graphene oxide 0.2%, surplus is water.
Process cold-reduced sheet surface after the treatment solution of the present embodiment being prepared (pH=1.8), step is as follows:
(1) oil removing is carried out to cold-reduced sheet surface, washing, pickling, secondary washing;
(2) cold-reduced sheet after step (1) being processed under normal temperature is placed in treatment solution and sprays process 3 minutes;
(3) the cold-reduced sheet washing post-drying after step (2) being processed, namely completes surface treatment.
embodiment 4
With the addition of a without phosphorus environmentally friendly metal surface treating liquid for graphene oxide, raw materials quality per-cent is as follows:
Silicofluoric acid 2%, Sodium orthomolybdate 1%, SODIUMNITRATE 2%, oxammonium sulfate 1.2%, disodium ethylene diamine tetraacetate 2%, tartrate 1.5%, graphene oxide 0.3%, surplus is water.
Process cold-reduced sheet surface after the treatment solution of the present embodiment is prepared (pH=1.8), step is as follows:
(1) oil removing is carried out to cold-reduced sheet surface, washing, pickling, secondary washing;
(2) cold-reduced sheet after step (1) being processed under normal temperature is placed in treatment solution and sprays process 2 minutes;
(3) the cold-reduced sheet washing post-drying after step (2) being processed, namely completes surface treatment.
embodiment 5
With the addition of a without phosphorus environmentally friendly metal surface treating liquid for graphene oxide, raw materials quality per-cent is as follows:
Silicofluoric acid 1.5%, Sodium orthomolybdate 0.5%, SODIUMNITRATE 1.6%, hydrogen peroxide 1%, disodium ethylene diamine tetraacetate 2%, tartrate 1.5%, graphene oxide 0.2%, surplus is water.
Process cold-reduced sheet surface after the treatment solution of the present embodiment is prepared (pH=1.8), step is as follows:
(1) oil removing is carried out to cold-reduced sheet surface, washing, pickling, secondary washing;
(2) cold-reduced sheet after step (1) being processed under normal temperature is placed in treatment solution and sprays process 4 minutes;
(3) the cold-reduced sheet washing post-drying after step (2) being processed, namely completes surface treatment.
interpretation of result
Performance Detection is carried out to the cold-reduced sheet after the surface treatment in embodiment 1-5, test event and result as follows:
A () outward appearance: after cold-reduced sheet is treated, surface all generates nattier blue, the uniform chemical conversion film of one deck.
B () copper sulfate drop is tested:
Copper-bath is prepared according to national standard:
CuSO
4·5H
2O：41 g/L；
NaCl：35g/L；
0.1 mol/L HCl：13 mL/L
The copper sulfate titration time of the cold-reduced sheet after treatment solution process of the present invention:
Embodiment 1:30 second
Embodiment 2:28 second
Embodiment 3:35 second
Embodiment 4:30 second
Embodiment 5:32 second
(c) 3.5 wt% brine soaking experiment:
Through the cold-reduced sheet of present treatment liquid process at the brine soaking experiment of 3.5 wt%:
A large amount of rust spot is there is not in embodiment 1:90 minute
A large amount of rust spot is there is not in embodiment 2:85 minute
A large amount of rust spot is there is not in embodiment 3:95 minute
A large amount of rust spot is there is not in embodiment 4:90 minute
A large amount of rust spot is there is not in embodiment 5:90 minute
All can be up to state standards.
D () paint film adhesion is tested:
After electrostatic dusting process, paint film adhesion experiment is carried out to the cold-reduced sheet processed in embodiment 1-5.
E () draws lattice experiment: use hundred lattice devices that the cold-reduced sheet after embodiment 1-5 process is carried out hundred lattice tests, after use adhesive tape is sticky, can reach more than 1 grade.
F () anti-impact force is tested: 49 N/cm of the cold-reduced sheet after embodiment 1-5 process
2power carry out surging force test after, the back side is all "dead" crackle occurs.
Claims (9)
1. one kind without phosphorus containing graphene oxide metallic surface pretreatment liquid, it is characterized in that, its component and weight percentage are: in weight part for 100%, silicofluoric acid 1-2%, Sodium orthomolybdate 0.2%-1%, SODIUMNITRATE 1%-2%, oxidation on metal surface agent 0.6%-1.2%, disodium ethylene diamine tetraacetate 1%-2%, tartrate 0.8%-1.5%, graphene oxide 0.1-0.3%, surplus is water.
2. one according to claim 1 is without phosphorus containing graphene oxide metallic surface pretreatment liquid, it is characterized in that, its component and weight percentage are: in weight part for 100%, silicofluoric acid 1-2%, Sodium orthomolybdate 0.5%-0.8%, SODIUMNITRATE 1.2%-1.6%, oxidation on metal surface agent 1%-1.2%, disodium ethylene diamine tetraacetate 1.7%-2%, tartrate 0.8%-1%, graphene oxide 0.1-0.3%, surplus is water.
3. one according to claim 1 is without phosphorus containing graphene oxide metallic surface pretreatment liquid, and it is characterized in that, described oxidation on metal surface agent is sodium chlorate, m-nitrobenzene sodium sulfonate, hydrogen peroxide or oxammonium sulfate.
4. one according to claim 3 is without phosphorus containing graphene oxide metallic surface pretreatment liquid, it is characterized in that, its component and weight percentage are: in weight part for 100%, silicofluoric acid 1%, Sodium orthomolybdate 0.5%, SODIUMNITRATE 1%, sodium chlorate 1.0%, disodium ethylene diamine tetraacetate 1%, tartrate 0.8%, graphene oxide 0.1%, surplus is water.
5. one according to claim 3 is without phosphorus containing graphene oxide metallic surface pretreatment liquid, it is characterized in that, its component and weight percentage are: silicofluoric acid 1.5%, Sodium orthomolybdate 0.2%, SODIUMNITRATE 1.2%, m-nitrobenzene sodium sulfonate 1.2%, disodium ethylene diamine tetraacetate 1.3%, tartrate 1.0%, graphene oxide 0.2%, surplus is water.
6. one according to claim 3 is without phosphorus containing graphene oxide metallic surface pretreatment liquid, it is characterized in that, its component and weight percentage are: silicofluoric acid 2%, Sodium orthomolybdate 0.8%, SODIUMNITRATE 1.6%, sodium chlorate 0.6%, disodium ethylene diamine tetraacetate 1.7%, tartrate 1.5%, graphene oxide 0.2%, surplus is water.
7. one according to claim 3 is without phosphorus containing graphene oxide metallic surface pretreatment liquid, it is characterized in that, its component and weight percentage are: silicofluoric acid 1.5%, Sodium orthomolybdate 0.5%, SODIUMNITRATE 1.6%, oxammonium sulfate 1%, disodium ethylene diamine tetraacetate 2%, tartrate 1.5%, graphene oxide 0.2%, surplus is water.
8. one according to claim 3 is without phosphorus containing graphene oxide metallic surface pretreatment liquid, it is characterized in that, its component and weight percentage are: silicofluoric acid 2%, Sodium orthomolybdate 1%, SODIUMNITRATE 2%, hydrogen peroxide 1.2%, disodium ethylene diamine tetraacetate 2%, tartrate 1.5%, graphene oxide 0.3%, surplus is water.
9. the using method of a kind of universal metallic surface of high anti-corrosion environmental protection according to claim 1 pretreatment liquid, step is as follows: after carrying out oil removing, washing, pickling, secondary washing process to pending metallic surface, be soaked in the pretreatment liquid of described metallic surface at normal temperatures, naturally dry after the metal washing after immersion or dry, namely completing metal finishing.
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| CN106011824A (en) * | 2016-08-11 | 2016-10-12 | 太仓市凯福士机械有限公司 | Environment-friendly passivating solution used for mechanical plating |
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| WO2020015475A1 (en) * | 2018-07-17 | 2020-01-23 | 中国原子能科学研究院 | Method for preparing graphene coating on the surface of metal |
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| CN109594071A (en) * | 2018-12-28 | 2019-04-09 | 湖北博新材料保护有限公司 | A kind of the metal pretreatment liquid and preparation method of the polymer modified graphene oxide containing bisamination |
| CN113136574A (en) * | 2021-04-07 | 2021-07-20 | 常州工程职业技术学院 | Composite passivation solution and preparation method thereof |
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