CN102808172B - Universal environment-friendly non-phosphorus phosphating solution - Google Patents
Universal environment-friendly non-phosphorus phosphating solution Download PDFInfo
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- CN102808172B CN102808172B CN201210303687.7A CN201210303687A CN102808172B CN 102808172 B CN102808172 B CN 102808172B CN 201210303687 A CN201210303687 A CN 201210303687A CN 102808172 B CN102808172 B CN 102808172B
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- phosphating solution
- nitric acid
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- acid
- phosphatization
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title abstract description 11
- 239000011574 phosphorus Substances 0.000 title abstract description 11
- 229910052698 phosphorus Inorganic materials 0.000 title abstract description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 40
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims abstract description 34
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 235000010288 sodium nitrite Nutrition 0.000 claims abstract description 17
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 claims abstract description 17
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004327 boric acid Substances 0.000 claims abstract description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 16
- 238000012360 testing method Methods 0.000 abstract description 17
- 239000007921 spray Substances 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract 2
- KVLZAMQCOBBPAW-UHFFFAOYSA-J N.[F-].[F-].[F-].[F-].F.F.[Zr+4] Chemical compound N.[F-].[F-].[F-].[F-].F.F.[Zr+4] KVLZAMQCOBBPAW-UHFFFAOYSA-J 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 229960001484 edetic acid Drugs 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 20
- 238000005507 spraying Methods 0.000 description 10
- 229910019142 PO4 Inorganic materials 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 6
- 239000010452 phosphate Substances 0.000 description 6
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 4
- 206010053615 Thermal burn Diseases 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 238000005554 pickling Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Landscapes
- Chemical Treatment Of Metals (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention discloses a universal environment-friendly non-phosphorus phosphating solution, which comprises the following components in percentage by weight: 3 to 5 percent of ammonium zirconium hexafluoride, 5 to 7 percent of nitric acid, 1.5 to 2 percent of boric acid, 0.4 to 0.6 percent of ethylene diamine tetraacetic acid, 3 to 3.4 percent of sodium nitrite, 1 to 2.5 percent of zinc molybdate and the balance of water. An adhesion test and a salt spray test show that the non-phosphorus phosphating solution has a good effect on improvement in the adhesion force of a metal substrate and a surface coating, the adhesion force obtained by the adhesion test is over 1 grade, and the adhesion force obtained by the salt spray test can be maintained for 1,000 hours; and the non-phosphorus phosphating solution is convenient to prepare and significant for environmental protection.
Description
Technical field
What the present invention relates to is a kind of Phosphating Solution, in particular a kind of general environment-friendly phosphating solution.
Background technology
Phosphorization treatment process traditional in metal finishing industry is subject to more and more stricter restriction to the discharge of phosphorus.Developing without phosphorus phosphating formula and technique has become the inexorable trend of industry development.At present, for the demand of without phosphorus Phosphating Solution, increasing sharply, carrying out without phosphorus phosphorization technology, to research and develop the work of without phosphorus phosphide liquid product very urgent.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of general environment-friendly phosphating solution is provided.
The present invention is achieved by the following technical solutions, and the present invention by weight, comprises following component: ammonium fluozirconate 3%～5%, nitric acid 5%～7%, boric acid 1.5%～2%, ethylenediamine tetraacetic acid (EDTA) 0.4%～0.6%, Sodium Nitrite 3%～3.4%, zinc molybdate 1%～2.5%, surplus is water.
As one of optimal way of the present invention, the present invention by weight, comprises following component: ammonium fluozirconate 3%, and nitric acid 5%, boric acid 1.5%, ethylenediamine tetraacetic acid (EDTA) 0.4%, Sodium Nitrite 3%, zinc molybdate 1%, surplus is water.
As one of optimal way of the present invention, the present invention by weight, comprises following component: ammonium fluozirconate 4%, and nitric acid 6%, boric acid 1.7%, ethylenediamine tetraacetic acid (EDTA) 0.5%, Sodium Nitrite 3.2%, zinc molybdate 2%, surplus is water.
As one of optimal way of the present invention, the present invention by weight, comprises following component: ammonium fluozirconate 5%, and nitric acid 7%, boric acid 2%, ethylenediamine tetraacetic acid (EDTA) 0.6%, Sodium Nitrite 3.4%, zinc molybdate 2.5%, surplus is water.
The Phosphating Solution of the present invention configuration is white transparent liquid and has trace suspension small-particle, and conductivity range is 6160us/cm～7440us/cm, and PH scope is 3.86～4.68.Cold-reduced sheet gets final product phosphatization through after oil removing, and the time is 2min～5min, and the model after phosphatization is for evenly fine and closely woven, for blue or golden yellow, with reflective.Soft steel hot-rolled sheet is through also can phosphatization after oil removing and pickling, and the time is 3min～5min, and the model after phosphatization is evenly fine and closely woven, is blue, dusty blue or golden yellow.
This Phosphating Solution is normal temperature formula, and phosphatize phosphate coat has much relations with temperature.Along with the raising of temperature, the color of phosphatize phosphate coat is by blueness to golden yellow transition, and its thickness is also in continuous increase, by bringing up to two microns several microns of zero point; Temperature reaches 30 phosphatize phosphate coats while spending and trends towards the result of electroplating, and is golden yellow, even compact.
In parkerizing process, take and control the specific conductivity of Phosphating Solution and pH value as main.By test, show that PRELIMINARY RESULTS is, in use, specific conductivity reduces the Phosphating Solution of new configuration gradually, and pH value raises gradually.When specific conductivity is during lower than 5000us/cm, occur that the probability that phosphatization does not go up or phosphatize phosphate coat is inhomogeneous increases gradually.PH value was higher than 5 o'clock, and phosphatization does not go up.
Ammonium fluozirconate: main filmogen-zirconium dioxide can be provided;
Nitric acid: adjust pH value, hydrotropy ammonium fluozirconate and secondary oxidizer;
Boric acid: tank liquor stablizer;
Ethylenediamine tetraacetic acid (EDTA): dispersed substance, contributes to the homogeneity of phosphatize phosphate coat;
Sodium Nitrite and zinc molybdate: oxygenant, these two kinds of oxygenants produce different impacts to phosphatize phosphate coat, if the quantity not sufficient of Sodium Nitrite, phosphatization model is blue, the quantity not sufficient of zinc molybdate, phosphatization surface is inhomogeneous, and anti-corrosion effect greatly reduces.
The present invention has the following advantages compared to existing technology: the present invention can find out by hundred lattice tests and salt-fog test, the effect of without phosphorus Phosphating Solution aspect the sticking power of increase metal base and top coat is fine, hundred lattice tests are more than 1 grade, salt-fog resistant test can reach 1000 hours, easy to prepare, environmental protection is had to great meaning.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The Phosphating Solution of the present embodiment by weight, comprises following component: ammonium fluozirconate 3%, and nitric acid 5%, boric acid 1.5%, ethylenediamine tetraacetic acid (EDTA) 0.4%, Sodium Nitrite 3%, zinc molybdate 1%, surplus is water.Wherein: nitric acid is aqueous nitric acid, adopting 98% nitric acid to be formulated as mass concentration is 26% aqueous nitric acid.The conductivity range of controlling Phosphating Solution is 6160us/cm～7440us/cm, and PH scope is 3.86～4.68.
The phosphatization model of the present embodiment is selected cold-reduced sheet, and process selection spray, also can select immersion in other embodiment, and spraying effect is better.
Phosphatization and last handling process comprise the following steps:
(1) workpiece is carried out to oil removing;
(2) 20 ℃ of left and right of normal temperature spray phosphatization, and phosphating time is 2min;
(3) about 10 ℃ rear 40 ℃ of oven dry of cleaning of cold water;
(4) carry out electrophoretic process.
Embodiment 2
The Phosphating Solution of the present embodiment by weight, comprises following component: ammonium fluozirconate 4%, and nitric acid 6%, boric acid 1.7%, ethylenediamine tetraacetic acid (EDTA) 0.5%, Sodium Nitrite 3.2%, zinc molybdate 2%, surplus is water.Wherein: nitric acid is aqueous nitric acid, adopting 98% nitric acid to be formulated as mass concentration is 26% aqueous nitric acid.The conductivity range of controlling Phosphating Solution is 6160us/cm～7440us/cm, and PH scope is 3.86～4.68.
The phosphatization model of the present embodiment is selected cold-reduced sheet, and process selection spray, also can select immersion in other embodiment, and spraying effect is better.
Phosphatization and last handling process comprise the following steps:
(1) workpiece is carried out to oil removing;
(2) 20 ℃ of left and right of normal temperature spray phosphatization, and phosphating time is 3min;
(3) after about 10 ℃ cleanings of cold water, scald 80 ℃ of left and right of hot water;
(4) processing of spraying paint.
Embodiment 3
The Phosphating Solution of the present embodiment by weight, comprises following component: ammonium fluozirconate 5%, and nitric acid 7%, boric acid 2%, ethylenediamine tetraacetic acid (EDTA) 0.6%, Sodium Nitrite 3.4%, zinc molybdate 2.5%, surplus is water.Wherein: nitric acid is aqueous nitric acid, adopting 98% nitric acid to be formulated as mass concentration is 26% aqueous nitric acid.The conductivity range of controlling Phosphating Solution is 6160us/cm～7440us/cm, and PH scope is 3.86～4.68.
The phosphatization model of the present embodiment is selected cold-reduced sheet, and process selection spray, also can select immersion in other embodiment, and spraying effect is better.
Phosphatization and last handling process comprise the following steps:
(1) workpiece is carried out to oil removing;
(2) 20 ℃ of left and right of normal temperature spray phosphatization, and phosphating time is 5min;
(3) after about 10 ℃ cleanings of cold water, scald 90 ℃ of left and right of hot water;
(4) carry out electrophoretic process;
(5) processing of spraying paint.
Embodiment 4
The Phosphating Solution of the present embodiment by weight, comprises following component: ammonium fluozirconate 3%, and nitric acid 5%, boric acid 1.5%, ethylenediamine tetraacetic acid (EDTA) 0.4%, Sodium Nitrite 3%, zinc molybdate 1%, surplus is water.Wherein: nitric acid is aqueous nitric acid, adopting 98% nitric acid to be formulated as mass concentration is 26% aqueous nitric acid.The conductivity range of controlling Phosphating Solution is 6160us/cm～7440us/cm, and PH scope is 3.86～4.68.
The phosphatization model of the present embodiment is selected hot-rolled sheet, and process selection spray, also can select immersion in other embodiment, and spraying effect is better.
Phosphatization and last handling process comprise the following steps:
(1) workpiece is carried out to oil removing and pickling;
(2) 20 ℃ of left and right of normal temperature spray phosphatization, and phosphating time is 3min;
(3) about 10 ℃ rear 40 ℃ of oven dry of cleaning of cold water;
(4) carry out electrophoretic process.
Embodiment 5
The Phosphating Solution of the present embodiment by weight, comprises following component: ammonium fluozirconate 4%, and nitric acid 6%, boric acid 1.7%, ethylenediamine tetraacetic acid (EDTA) 0.5%, Sodium Nitrite 3.2%, zinc molybdate 2%, surplus is water.Wherein: nitric acid is aqueous nitric acid, adopting 98% nitric acid to be formulated as mass concentration is 26% aqueous nitric acid.The conductivity range of controlling Phosphating Solution is 6160us/cm～7440us/cm, and PH scope is 3.86～4.68.
The phosphatization model of the present embodiment is selected hot-rolled sheet, and process selection spray, also can select immersion in other embodiment, and spraying effect is better.
Phosphatization and last handling process comprise the following steps:
(1) workpiece is carried out to oil removing and pickling;
(2) 20 ℃ of left and right of normal temperature spray phosphatization, and phosphating time is 4min;
(3) after about 10 ℃ cleanings of cold water, scald 90 ℃ of left and right of hot water;
(4) processing of spraying paint.
Embodiment 6
The Phosphating Solution of the present embodiment by weight, comprises following component: ammonium fluozirconate 5%, and nitric acid 7%, boric acid 2%, ethylenediamine tetraacetic acid (EDTA) 0.6%, Sodium Nitrite 3.4%, zinc molybdate 2.5%, surplus is water.Wherein: nitric acid is aqueous nitric acid, adopting 98% nitric acid to be formulated as mass concentration is 26% aqueous nitric acid.The conductivity range of controlling Phosphating Solution is 6160us/cm～7440us/cm, and PH scope is 3.86～4.68.
The phosphatization model of the present embodiment is selected hot-rolled sheet, and process selection spray, also can select immersion in other embodiment, and spraying effect is better.
Phosphatization and last handling process comprise the following steps:
(1) workpiece is carried out to oil removing and pickling;
(2) 20 ℃ of left and right of normal temperature spray phosphatization, and phosphating time is 5min;
(3) after about 10 ℃ cleanings of cold water, scald 80 ℃ of left and right of hot water;
(4) carry out electrophoretic process;
(5) processing of spraying paint.
Use hundred lattice devices that the one side of the model of embodiment 1～6 is done to hundred lattice tests, hundred lattice test effects are fine, and after use adhesive tape is sticky, its expulsion rate is zero.Then at the another side of model, draw fork and do 400～1000 hours salt-fog tests.Since 400 hours, every increase was taken out one from the model of every kind of classification in 100 hours, remove out the rust of top, find after dry, and the cut not diffusion of getting rusty, As time goes on, cut slowly expands to both sides, and the situation that specifically expands is as shown in table 1:
Table 1 salt-fog test results of corrosion-resistance
By above-mentioned hundred lattice tests and salt-fog test, can find out, the effect of without phosphorus Phosphating Solution aspect the sticking power of increase metal base and top coat is fine, and hundred lattice tests are more than 1 grade, and salt-fog resistant test can reach 1000 hours.
Claims (4)
1. a general environment-friendly phosphating solution, it is characterized in that, by weight, comprise following component: ammonium fluozirconate 3%～5%, nitric acid 5%～7%, boric acid 1.5%～2%, ethylenediamine tetraacetic acid (EDTA) 0.4%～0.6%, Sodium Nitrite 3%～3.4%, zinc molybdate 1%～2.5%, surplus is water, and the conductivity range of described Phosphating Solution is 6160us/cm～7440us/cm, and PH scope is 3.86～4.68.
2. general environment-friendly phosphating solution according to claim 1, is characterized in that: by weight, comprise following component: ammonium fluozirconate 3%, and nitric acid 5%, boric acid 1.5%, ethylenediamine tetraacetic acid (EDTA) 0.4%, Sodium Nitrite 3%, zinc molybdate 1%, surplus is water.
3. general environment-friendly phosphating solution according to claim 1, is characterized in that: by weight, comprise following component: ammonium fluozirconate 4%, and nitric acid 6%, boric acid 1.7%, ethylenediamine tetraacetic acid (EDTA) 0.5%, Sodium Nitrite 3.2%, zinc molybdate 2%, surplus is water.
4. general environment-friendly phosphating solution according to claim 1, is characterized in that: by weight, comprise following component: ammonium fluozirconate 5%, and nitric acid 7%, boric acid 2%, ethylenediamine tetraacetic acid (EDTA) 0.6%, Sodium Nitrite 3.4%, zinc molybdate 2.5%, surplus is water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210303687.7A CN102808172B (en) | 2012-08-24 | 2012-08-24 | Universal environment-friendly non-phosphorus phosphating solution |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210303687.7A CN102808172B (en) | 2012-08-24 | 2012-08-24 | Universal environment-friendly non-phosphorus phosphating solution |
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| CN102808172A CN102808172A (en) | 2012-12-05 |
| CN102808172B true CN102808172B (en) | 2014-04-02 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106939418A (en) * | 2016-01-04 | 2017-07-11 | 陈江清 | A kind of wire drawing film agent and application method |
| CN108866527A (en) * | 2017-05-09 | 2018-11-23 | 句容市博远电子有限公司 | A kind of without phosphorus phosphating solution and preparation method thereof |
| 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 |
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| CN1510166A (en) * | 2002-12-24 | 2004-07-07 | �ձ�������ʽ���� | Chemical conversion coating agent and metal with surface treatment |
| CN101487117A (en) * | 2009-02-25 | 2009-07-22 | 西安建筑科技大学 | Preparation of aluminum alloy surface fluoroaluminate conversion film |
| CN101701336A (en) * | 2009-11-26 | 2010-05-05 | 芜湖市瑞杰环保材料科技有限公司 | Environment-friendly metal surface treating agent and using method thereof |
| CN102199766A (en) * | 2011-04-22 | 2011-09-28 | 哈尔滨工程大学 | Method for preparing magnesium lithium alloy cerium salt and molybdate-phosphate-zirconium fluoride conversion coating |
| CN102433559A (en) * | 2011-10-24 | 2012-05-02 | 宁波科苑鑫泰表面处理新技术有限公司 | Rare earth cerium-containing metal treatment fluid and production method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4429936A1 (en) * | 1994-08-24 | 1996-02-29 | Metallgesellschaft Ag | Preparation of metal surfaces for enamelling |
| JP2008174807A (en) * | 2007-01-19 | 2008-07-31 | Nippon Hyomen Kagaku Kk | Chromium-free metal surface treatment liquid |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1510166A (en) * | 2002-12-24 | 2004-07-07 | �ձ�������ʽ���� | Chemical conversion coating agent and metal with surface treatment |
| CN101487117A (en) * | 2009-02-25 | 2009-07-22 | 西安建筑科技大学 | Preparation of aluminum alloy surface fluoroaluminate conversion film |
| CN101701336A (en) * | 2009-11-26 | 2010-05-05 | 芜湖市瑞杰环保材料科技有限公司 | Environment-friendly metal surface treating agent and using method thereof |
| CN102199766A (en) * | 2011-04-22 | 2011-09-28 | 哈尔滨工程大学 | Method for preparing magnesium lithium alloy cerium salt and molybdate-phosphate-zirconium fluoride conversion coating |
| CN102433559A (en) * | 2011-10-24 | 2012-05-02 | 宁波科苑鑫泰表面处理新技术有限公司 | Rare earth cerium-containing metal treatment fluid and production method thereof |
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Denomination of invention: Universal environment-friendly non-phosphorus phosphating solution Effective date of registration: 20170526 Granted publication date: 20140402 Pledgee: Huizhou Merchants Bank, Hefei Shuguang Road subbranch Pledgor: ANHUI QIMING SURFACE TECHNOLOGY Co.,Ltd. Registration number: 2017340000074 |
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