CN103938198B - Without phosphorus nanometer vitrified agent, preparation method and application thereof - Google Patents
Without phosphorus nanometer vitrified agent, preparation method and application thereof Download PDFInfo
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Abstract
The present invention relates to metal conditioner field, relate to a kind of without phosphorus nanometer vitrified agent, preparation method and application thereof. The without phosphorus nanometer vitrified agent of the present invention, by percentage to the quality, made by following raw material: fluorine zirconic acid 3-6%, basic zirconium chloride 3-7%, ammonium fluozirconate 0.1-0.6%, tartaric acid 0.8-2%, sodium nitrate 0.5-1%, surplus is water. The without phosphorus nanometer vitrified agent of the present invention can operate under normal temperature, and the processing time is short, and technique is simple, almost there is no sediment, and nonchoking nozzle reduces offal treatment cost; Can significantly improve the adhesive force of coating and metal, extend the corrosion-resistant time of metal.
Description
Technical field
The present invention the present invention relates to metal conditioner field, be exactly a kind of phosphate-free metal surface conditioning agent,Preparation method and application thereof.
Background technology
Increasingly important along with environmental requirement, traditional phosphating process is phosphorous, nickel and sediment are processed problem, gradually cannotMeet the demand of modern environmental protection, Phosphateless environmentally friendly conversion process of new generation can form nanoscale film in metal surface, have enhancingApplication adhesive force and corrosion-resistant function, can process iron and steel, zinc, aluminium and alloy material thereof is substitute conventional phosphatizing treatment process excellentGood selection. Current without phosphorus conversion film product, actual application in the industry such as automobile, household electrical appliances, the product of without phosphorus conversion filmBecome gradually the emphasis of the front Treatment of Metal Surface related industry development of following whole each application, bring for substituting conventional phosphatizing technologyA new ripple development climax.
Chinese patent CN102586769A discloses a kind of phosphate-free metal surface conditioning agent and using method thereof, be by underState the component composition of weight portion: 5～20 parts of the nano zirconium dioxide dispersion liquids that concentration is 28%, 6～30 parts, hydrofluoric acid, propane diols3～15 parts, eight 6～20 parts of vinyl cagelike silsesquioxanes, 3～20 parts of acetic acid, 0.03～0.5 part of cerium salt, hydrogen-oxygenChange 1～5 part, sodium, 50～76 parts of deionized waters, described a kind of phosphate-free metal surface conditioning agent, energy after metal is processedEnough without phosphorus conversion composite membranes of nanometer silane that forms in metal surface. But there is following shortcoming in this patent: cerium salt is containing heavy metalElement, thereby this formula do not meet national environmental protection policy, can not in the competition of future market, obtain one seat.
Chinese patent CN102747355A discloses a kind of metal surface vitrified agent and using method thereof, metal surface potteryAgent contains zirconium titanium salt 2.0～38.0%, silane 0.1～8.0%, and buffer 0.5～18.0%, coalescents 0.01～5.00%, antirust agent 0.1～6.1%, complexing agent 0.2～7.0%, apparent is as clear as crystal liquid, and no suspended substance; PH valueBe 1～2; Proportion is 1.05 ± 0.02g/cm3. Its useful technique effect is to generate one in metal surface under normal temperature statePlant embedded property heterozygosis indissoluble nanometer scale ceramics conversion film, have and good anti-impact force, can improve the adhesive force of coating, increaseThe corrosion resistance on strong metal surface. But there is following shortcoming in this patent: in this formula, do not add stabilizing agent, can cause productIn use procedure, often appearance is unstable for quality, while even occurring that all technical is in scope, and can not be in metal surfaceForm ceramic film.
Chinese patent CN101629286 discloses a kind of vitrified agent, and it becomes the raw material of umber to make by following quality group:Titanium zirconium composite: 20～30 parts, fluoride: 5～10 parts, complexing agent: 5～10 parts, water: 40～60 parts. Make by this patentVitrified agent good stability out, without sediment, not phosphate-containing can form one deck vitrification on the surface of iron and steel, zinc and aluminiumLayer, it is strong with the coating adhesion of each model, and spray and the immersion treatment of applicable normal temperature need not firing equipments, reach saving energySource, be easy to produce object. But there is following shortcoming in this patent: although this formula can film forming, flying power is limited, alsoThe cycle of change in other words groove, again joining groove shortens greatly, has so just increased client's use cost, has reduced product in marketMiddle competitiveness.
Summary of the invention
One of object of the present invention is to overcome the deficiencies in the prior art, and a kind of without phosphorus nanometer vitrified agent is provided, and this is without phosphorusThe without phosphorus pre-treating technology of nanometer vitrified agent, the waste water producing do not contain chromium, nickel and other toxic heavy metals, without nitrite,Without phosphate and volatility organic component, alleviate wastewater treatment and environmental pressure.
Two of object of the present invention is to provide the preparation method of above-mentioned without phosphorus nanometer vitrified agent.
Three of object of the present invention is to provide the using method of above-mentioned without phosphorus nanometer vitrified agent.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of without phosphorus nanometer vitrified agent, by percentage to the quality, made by following raw material:
Fluorine zirconic acid 3-6%, basic zirconium chloride 3-7%, ammonium fluozirconate 0.1-0.6%, tartaric acid 0.8-2%, sodium nitrate 0.5-1%, more thanAmount is water.
The wherein said preferred 4-5% of fluorine zirconic acid; The preferred 4-6% of described basic zirconium chloride, described ammonium fluozirconate is preferred0.3-0.6%。
The preferred technical scheme of the present invention is: a kind of without phosphorus nanometer vitrified agent, by percentage to the quality, by following raw material systemBecome:
Fluorine zirconic acid 5%, basic zirconium chloride 6%, ammonium fluozirconate 0.6%, tartaric acid 1.5%, sodium nitrate 0.8%, water 86.1%.
The preparation method of the without phosphorus nanometer vitrified agent of the present invention, in turn includes the following steps:
(1) in reactor, add water;
(2) in reactor, add fluorine zirconic acid, then stir;
(3) in reactor, add basic zirconium chloride, then stir, until dissolve completely;
(4) in reactor, add ammonium fluozirconate, stir and make solution clarification;
(5) in reactor, add tartaric acid, stir and make solution clarification;
(6) in reactor, add sodium nitrate, wait to stir and make solution clarification.
Wherein the mixing time of step (2) is 0.5-1.5 hour; The mixing time of step (3) is 1-3 hour; Step(4) mixing time is 0.5-1.5 hour; The mixing time of step (5) is 0.5-1.5 hour; The mixing time of step (6)For 20-40 minute.
The using method of without phosphorus nanometer vitrified agent of the present invention, is characterized in that by following steps, metal being carried outProcess:
(1) degreasing;
(2) twice washing;
(3) without phosphorus nanometer vitrified agent is processed and is transformed, and operating temperature is normal temperature, and processing mode, for spray or immersion, is processedTime is 3-5 minute;
(4) twice washing;
(5) dry.
Wherein in step (2) and step (4) washing for the second time of twice washing all preferably pure water wash;
In step (3), the collocation method of without phosphorus nanometer vitrified agent is: 30 kilograms of without phosphorus nanometer vitrified agents, then add 970 kilogramsWater is formulated, stirs.
While adopting spray or soaking technology in step (3), process conditions are respectively in table 1. Adopt without phosphorus nanometer of the present inventionVitrified agent is processed metal, can form the without phosphorus conversion composite membrane of nanometer on its surface.
The without phosphorus nanometer vitrified agent of table 1 is processed smithcraft condition
The present invention has following beneficial effect:
(1) without phosphorus pre-treating technology, the waste water producing do not contain chromium, nickel and other toxic heavy metals, without nitrite,Without phosphate and volatility organic component, alleviate wastewater treatment and environmental pressure;
(2) have the function that increases coating adhesion, prevents corrosion, alternative conventional iron is phosphatization;
(3) be applicable to iron and steel, zinc, the pre-treatment of aluminium various metals;
(4) under normal temperature, operate, the short processing time, adjust without surface, do not needing to change original production equipmentSituation, use nanometer non-phosphate film agent can save the cost of 15%-30%, and technique is simpler, and " table is adjusted " operation can be saved notUse;
(5) almost there is no sediment, nonchoking nozzle, reduces offal treatment cost;
(6) do not need " Chi Shui " of frequent replacing " bonderite ", when concentration is inadequate, add;
(7) can significantly improve the adhesive force of coating and metal, extend the corrosion-resistant time of metal.
Groundwork principle of the present invention is as follows:
Burning is without phosphorus conversion film, is that electrochemical reaction and the indifferent oxide colloid of metal in acid solution existsMetal (iron, zinc, aluminium and alloy thereof) surface, cohesion deposition changes into has nano level composite metal oxide rete, and toolThere is ZrO2Conversion film processing be at acid H2ZrF6In solution, carry out, key reaction is as follows:
Acid etching reaction H2ZrF6+Me+2H2O→ZrO2+Me2++4H++6F++H2Me:Fe, Zn, Al goldBelong to base material
The reaction 1. hydrolysis ZrOCl of indifferent oxide2+H2O→ZrO(OH)2+ 2HCl zirconium hydroxide isA kind of white gels, may be dissolved in diluted acid, and generates colloidal sol
2. polycondensation reaction Me ≡ Zr-OH+HO-Zr ≡ Me → Me ≡ Zr-O-Zr ≡ Me+H2O
Above-mentioned reaction, according to sol gel processing, forms a kind of ZrO2-Me-ZrO2Sol particles structure, sol particlesThere is very strong cohesion function. Along with the carrying out of reaction, form gradually three-dimensional netted ZrO2-Me-ZrO2Collosol structure, cohesionDeposition produces has nano level ZrO2Conversion film.
Bath maintenance: at ordinary times by adding, guarantee that tank liquor concentration is normal. Suggestion tank liquor, through circulating filtration equipment mistake, is avoidedImpurity accumulation. In the time accumulating more impurity in groove, recommended replacement tank liquor.
Detailed description of the invention
Embodiment 1
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 30Kg, basic zirconium chloride 30Kg, ammonium fluozirconate 1Kg, tartaric acid 8Kg, sodium nitrate 5Kg, water 926Kg。
Its preparation method in turn includes the following steps:
(in 1 reactor, add water;
(2) in reactor, add fluorine zirconic acid, then stir mixing time 1-1.5 hour;
(3) in reactor, add basic zirconium chloride, then stir, until dissolve completely, the time is 1-3 hour;
(4) in reactor, add ammonium fluozirconate, stir and make solution clarification, the time is 0.5-1.5 hour;
(5) in reactor, add tartaric acid, stir and make solution clarification, the time is 0.5-1.5 hour;
(6) in reactor, add sodium nitrate, wait to stir and make solution clarification, the time is 20-40 minute;
(7) product is carried out to physical and chemical index detection, packaging warehouse-in.
Without phosphorus nanometer vitrified agent of the present invention is processed metal by following steps:
(1) degreasing;
(2) twice washing;
(3) without phosphorus nanometer vitrified agent is processed and is transformed, and operating temperature is normal temperature, and processing mode is for soaking, and the processing time is 3-5Minute;
(4) twice washing;
(5) dry.
Wherein in step (2) and step (4), the washing for the second time of twice washing all adopts pure water to wash; Step (3)In the collocation method of without phosphorus nanometer vitrified agent be: 30 kilograms of without phosphorus nanometer vitrified agents, then it is formulated to add 970 kg of water, stirsEvenly.
Embodiment 2
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 40Kg, basic zirconium chloride 40Kg, ammonium fluozirconate 3Kg, tartaric acid 9Kg, sodium nitrate 6Kg, water 902Kg。
Preparation method and metal is carried out to treatment step with embodiment 1.
Embodiment 3
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 50Kg, basic zirconium chloride 50Kg, ammonium fluozirconate 4Kg, tartaric acid 9Kg, sodium nitrate 7Kg, water 880Kg。
Preparation method and metal is carried out to treatment step with embodiment 1.
Embodiment 4
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 60Kg, basic zirconium chloride 50Kg, ammonium fluozirconate 4Kg, tartaric acid 9Kg, sodium nitrate 7Kg, water 870Kg。
Preparation method and metal is carried out to treatment step with embodiment 1.
Embodiment 5
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 40Kg, basic zirconium chloride 60Kg, ammonium fluozirconate 5Kg, tartaric acid 10Kg, sodium nitrate 7Kg, water 878Kg。
Preparation method and metal is carried out to treatment step with embodiment 1.
Preparation method is with embodiment 1.
Embodiment 6
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 50Kg, basic zirconium chloride 60Kg, ammonium fluozirconate 6Kg, tartaric acid 15Kg, sodium nitrate 8Kg, water 861Kg。
Preparation method and metal is carried out to treatment step with embodiment 1.
Embodiment 7
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 50Kg, basic zirconium chloride 60Kg, ammonium fluozirconate 5Kg, tartaric acid 17Kg, sodium nitrate 9Kg, water 859Kg。
Preparation method and metal is carried out to treatment step with embodiment 1.
Embodiment 8
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 50Kg, basic zirconium chloride 40Kg, ammonium fluozirconate 6Kg, tartaric acid 20Kg, sodium nitrate 10Kg, water 874Kg。
Preparation method and metal is carried out to treatment step with embodiment 1.
Embodiment 9
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 50Kg, basic zirconium chloride 40Kg, ammonium fluozirconate 4Kg, tartaric acid 16Kg, sodium nitrate 6Kg, water 884Kg。
Preparation method and metal is carried out to treatment step with embodiment 1.
Embodiment 10
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 40Kg, basic zirconium chloride 50Kg, ammonium fluozirconate 5Kg, tartaric acid 10Kg, sodium nitrate 9Kg, water 886Kg。
Preparation method and metal is carried out to treatment step with embodiment 1.
Embodiment 11
The without phosphorus nanometer vitrified agent of every 1000Kg, made by following raw material:
Fluorine zirconic acid 40Kg, basic zirconium chloride 70Kg, ammonium fluozirconate 3Kg, tartaric acid 12Kg, sodium nitrate 8Kg, water 867Kg。
Preparation method and metal is carried out to treatment step with embodiment 1.
The formula of embodiment of the present invention 1-6 in Table 2(with the without phosphorus nanometer vitrified agent of 1000Kg), the formula of embodiment 7-11 is shown inTable 3.
The formula of table 2 embodiment 1-6
| Raw material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Fluorine zirconic acid | 30 | 40 | 50 | 60 | 40 | 50 |
| Five nitric hydrate zirconiums | 30 | 40 | 50 | 50 | 60 | 60 |
| Ammonium fluozirconate | 1 | 3 | 4 | 4 | 5 | 6 |
| Tartaric acid | 8 | 9 | 9 | 9 | 10 | 15 |
| Sodium nitrate | 5 | 6 | 7 | 7 | 7 | 8 5 --> |
| Water | 926 | 902 | 880 | 870 | 878 | 861 |
The formula of table 3 embodiment 7-11
| Raw material | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 |
| Fluorine zirconic acid | 50 | 50 | 50 | 40 | 40 |
| Five nitric hydrate zirconiums | 60 | 40 | 40 | 50 | 70 |
| Ammonium fluozirconate | 5 | 6 | 4 | 5 | 3 |
| Tartaric acid | 17 | 20 | 16 | 10 | 12 |
| Sodium nitrate | 9 | 10 | 6 | 9 | 8 |
| Water | 859 | 874 | 884 | 886 | 867 |
Embodiment of the present invention 1-6 to the treatment effect of metal in table 4, embodiment 7-11 to the treatment effect of metal in table 5.
The metal treatment effect of table 4 embodiment 1-6
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Processing time | 4min | 4min | 4min | 4min | 4min | 4min |
| Serviceability temperature | Normal temperature | Normal temperature | Normal temperature | Normal temperature | Normal temperature | Normal temperature |
| Sediment weight after processing | 164mg/㎡ | 158mg/㎡ | 125mg/㎡ | 79mg/㎡ | 101mg/㎡ | 62mg/㎡ |
| Vitrification film thickness | 26nm | 31nm | 29nm | 35nm | 28nm | 42nm |
| Paint film adhesion grade | 0 grade | 0 grade | 0 grade | 0 grade | 0 grade | 0 grade |
| Paint film neutral salt spray test | 500h | 500h | 500h | 500h | 500h | 800h |
The treatment effect of table 5 embodiment 7-11 to metal
| Project | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 |
| Processing time | 4min | 4min | 4min | 4min | 4min |
| Serviceability temperature | Normal temperature | Normal temperature | Normal temperature | Normal temperature | Normal temperature |
| Sediment weight after processing | 87mg/㎡ | 115mg/㎡ | 126mg/㎡ | 95mg/㎡ | 88mg/㎡ |
| Vitrification film thickness | 25nm | 37nm | 33nm | 31nm | 30nm |
| Paint film adhesion grade | 0 grade | 0 grade | 0 grade | 0 grade | 0 grade |
| Paint film neutral salt spray test | 500h | 500h | 500h | 500h | 500h |
From table 4, table 5 can find out that the without phosphorus nanometer vitrified agent of the present invention is at same treatment time and temperature, and embodiment 6 makesWith after effect be best. Wherein vitrification thicknesses of layers reaches 42nm, and it applies rear enamelled coating adhesive force grade is 0 grade, neutral salt sprayTest reaches more than 800 hours, all more has superiority than other embodiment effects. The effect of embodiment 6 is best in sum.
In table 4, table 5, comparative run object method of testing is as follows:
Sediment weight calculates: after sediment is dried, after weighing, show that sediment quality divided by processing area is with assay balanceCan.
Paint film neutral salt spray test: carry out according to GB10125-1997 artificial atmosphere corrosion test salt spray test standardTest;
Paint film adhesion grade: survey according to the cross cut test standard of GB9286-1998 paint and varnish paint filmExamination;
Above content description general principle of the present invention and principal character, the present invention is not restricted to the described embodiments,Without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these changes and improvements allFall in the claimed scope of the invention. The claimed scope of the present invention is by appending claims and equivalent circle thereofFixed.
Claims (8)
1. a without phosphorus nanometer vitrified agent, is characterized in that by percentage to the quality, is made up of following raw material:
Fluorine zirconic acid 3-6%, basic zirconium chloride 3-7%, ammonium fluozirconate 0.1-0.6%, tartaric acid 0.8-2%, sodium nitrate 0.5-1%, surplus isWater.
2. without phosphorus nanometer vitrified agent according to claim 1, is characterized in that described fluorine zirconic acid consumption is 4-5%.
3. without phosphorus nanometer vitrified agent according to claim 1, is characterized in that described basic zirconium chloride consumption is 4-6%.
4. without phosphorus nanometer vitrified agent according to claim 1, is characterized in that described ammonium fluozirconate consumption is 0.3-0.6%。
5. without phosphorus nanometer vitrified agent according to claim 1, is characterized in that by percentage to the quality, by following raw material systemBecome: fluorine zirconic acid 5%, basic zirconium chloride 6%, ammonium fluozirconate 0.6%, tartaric acid 1.5%, sodium nitrate 0.8%, water 86.1%.
6. the preparation method of without phosphorus nanometer vitrified agent according to claim 1, in turn includes the following steps:
(1) in reactor, add water;
(2) in reactor, add fluorine zirconic acid, then stir;
(3) in reactor, add basic zirconium chloride, then stir, until dissolve completely;
(4) in reactor, add ammonium fluozirconate, stir and make solution clarification;
(5) in reactor, add tartaric acid, stir and make solution clarification;
(6) in reactor, add sodium nitrate, wait to stir and make solution clarification.
7. the preparation method of without phosphorus nanometer vitrified agent according to claim 6, is characterized in that the mixing time of step (2) is0.5-1.5 hour; The mixing time of step (3) is 1-3 hour; The mixing time of step (4) is 0.5-1.5 hour; Step(5) mixing time is 0.5-1.5 hour; The mixing time of step (6) is 20-40 minute.
8. the application of without phosphorus nanometer vitrified agent in Treatment of Metal Surface according to claim 1.
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| CN104233252B (en) * | 2014-09-16 | 2016-08-24 | 南京华锐化工有限公司 | A kind of room temperature non-phosphate film agent |
| CN104726859A (en) * | 2014-12-31 | 2015-06-24 | 重庆建设摩托车股份有限公司 | Method for treating surface of oil tank under continuous production condition |
| CN106702361A (en) * | 2016-04-18 | 2017-05-24 | 佛山瑞箭体育器材有限公司 | Nanometer ceramic conversion agent and preparation method thereof |
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| CN107937903A (en) * | 2017-12-07 | 2018-04-20 | 佛山市高明高盛铝业有限公司 | A kind of preparation method of corrosive protection of aluminium alloy layer |
| CN108047939A (en) * | 2017-12-25 | 2018-05-18 | 湖南德莱恩新材料科技有限公司 | Vitrified agent and preparation method thereof and application method |
| CN109868466A (en) * | 2019-01-31 | 2019-06-11 | 中锆纳米材料股份有限公司 | A kind of nano zircite metal rust preventing vitrification liquid |
| CN113215558A (en) * | 2021-05-18 | 2021-08-06 | 中山市壹桥环保科技有限公司 | Washing-free vitrification agent and use method thereof |
| CN113235078A (en) * | 2021-05-18 | 2021-08-10 | 中山市壹桥环保科技有限公司 | Washing-free silane agent and using method thereof |
| CN114016013A (en) * | 2021-09-23 | 2022-02-08 | 东莞市岩奥新材料有限公司 | Metal vitrification agent and preparation method and use method thereof |
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