CN102808171B - Quick environment-friendly phosphorus-free phosphating solution - Google Patents
Quick environment-friendly phosphorus-free phosphating solution Download PDFInfo
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- CN102808171B CN102808171B CN201210303410.4A CN201210303410A CN102808171B CN 102808171 B CN102808171 B CN 102808171B CN 201210303410 A CN201210303410 A CN 201210303410A CN 102808171 B CN102808171 B CN 102808171B
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Abstract
The invention discloses a quick environment-friendly phosphorus-free phosphating solution. The quick environment-friendly phosphorus-free phosphating solution comprises the following components in percentage by weight: 4 to 6 percent of ammonium zirconium hexafluoride, 5 to 7 percent of hydrofluoric acid, 1 to 1.5 percent of boric acid, 0.1 to 0.2 percent of ethylene diamine tetraacetic acid, 0.5 to 1.5 percent of zinc molybdate and the balance of water. Through a cross-cut tape adhesion test, the phosphorus-free phosphating solution can reach more than one grade in the aspect of increasing the adhesion of a metal base and a surface coating; through a salt spray resistance test, the salt spray resistance time of the phosphorus-free phosphating solution can reach 1,000 hours; and the phosphorus-free phosphating solution is convenient to prepare and has significance to environment friendliness.
Description
Technical field
What the present invention relates to is a kind of Phosphating Solution, in particular a kind of quick environment protection type 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 quick environment protection type 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 4%～6%, and hydrofluoric acid 5%～7%, boric acid 1%～1.5%, ethylenediamine tetraacetic acid (EDTA) 0.1%～0.2%, zinc molybdate 0.5%～1.5%, surplus is water.
As one of optimal way of the present invention, the present invention by weight, comprises following component: ammonium fluozirconate 4%, and hydrofluoric acid 5%, boric acid 1%, ethylenediamine tetraacetic acid (EDTA) 0.1%, zinc molybdate 0.5%, surplus is water.
As one of optimal way of the present invention, the present invention by weight, comprises following component: ammonium fluozirconate 5%, and hydrofluoric acid 6%, boric acid 1.25%, ethylenediamine tetraacetic acid (EDTA) 0.15%, 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 6%, and hydrofluoric acid 7%, boric acid 1.5%, ethylenediamine tetraacetic acid (EDTA) 0.2%, zinc molybdate 1.5%, surplus is water.
The Phosphating Solution of the present invention's configuration is white transparent liquid, and conductivity range is 6160us/cm～9000us/cm, and PH scope is 3.86～4.68.Model is through getting final product phosphatization after oil removing, and the time is 1min～1.5min, the model after phosphatization for evenly fine and closely woven, golden yellow, with reflective.
This Phosphating Solution is normal temperature formula, and phosphatize phosphate coat is had little or nothing to do with temperature.Along with the raising of phosphating time, the color of phosphatize phosphate coat is by yellow to golden yellow transition, and its thickness is also in continuous increase, by bringing up to two microns several microns of zero point.
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 6000us/cm, there will be phosphatization not go up.
Ammonium fluozirconate: main filmogen-zirconium dioxide can be provided;
Hydrofluoric acid: adjust pH value, provide oxidative function, as oxygenant;
Boric acid: Phosphating Solution stablizer;
Ethylenediamine tetraacetic acid (EDTA): dispersed substance, contributes to the homogeneity of phosphatize phosphate coat.
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 4%, and hydrofluoric acid 5%, boric acid 1%, ethylenediamine tetraacetic acid (EDTA) 0.1%, zinc molybdate 0.5%, surplus is water.Wherein: hydrofluoric acid is hydrofluoric acid aqueous solution, adopting 46% hydrofluoric acid to be formulated as mass concentration is 24.5% hydrofluoric acid aqueous solution.The conductivity range of controlling Phosphating Solution is 6160us/cm～9000us/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 1min;
(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 5%, and hydrofluoric acid 6%, boric acid 1.25%, ethylenediamine tetraacetic acid (EDTA) 0.15%, zinc molybdate 1%, surplus is water.Wherein: hydrofluoric acid is hydrofluoric acid aqueous solution, adopting 46% hydrofluoric acid to be formulated as mass concentration is 24.5% hydrofluoric acid aqueous solution.The conductivity range of controlling Phosphating Solution is 6160us/cm～9000us/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 1.5min;
(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 6%, and hydrofluoric acid 7%, boric acid 1.5%, ethylenediamine tetraacetic acid (EDTA) 0.2%, zinc molybdate 1.5%, surplus is water.Wherein: hydrofluoric acid is hydrofluoric acid aqueous solution, adopting 46% hydrofluoric acid to be formulated as mass concentration is 24.5% hydrofluoric acid aqueous solution.The conductivity range of controlling Phosphating Solution is 6160us/cm～9000us/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 1.5min;
(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 4%, and hydrofluoric acid 5%, boric acid 1%, ethylenediamine tetraacetic acid (EDTA) 0.1%, zinc molybdate 0.5%, surplus is water.Wherein: hydrofluoric acid is hydrofluoric acid aqueous solution, adopting 46% hydrofluoric acid to be formulated as mass concentration is 24.5% hydrofluoric acid aqueous solution.The conductivity range of controlling Phosphating Solution is 6160us/cm～9000us/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;
(2) 20 ℃ of left and right of normal temperature spray phosphatization, and phosphating time is 1min;
(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 5%, and hydrofluoric acid 6%, boric acid 1.25%, ethylenediamine tetraacetic acid (EDTA) 0.15%, zinc molybdate 1%, surplus is water.Wherein: hydrofluoric acid is hydrofluoric acid aqueous solution, adopting 46% hydrofluoric acid to be formulated as mass concentration is 24.5% hydrofluoric acid aqueous solution.The conductivity range of controlling Phosphating Solution is 6160us/cm～9000us/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;
(2) 20 ℃ of left and right of normal temperature spray phosphatization, and phosphating time is 1min;
(3) after about 10 ℃ cleanings of cold water, scald 85 ℃ 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 6%, and hydrofluoric acid 7%, boric acid 1.5%, ethylenediamine tetraacetic acid (EDTA) 0.2%, zinc molybdate 1.5%, surplus is water.Wherein: hydrofluoric acid is hydrofluoric acid aqueous solution, adopting 46% hydrofluoric acid to be formulated as mass concentration is 24.5% hydrofluoric acid aqueous solution.The conductivity range of controlling Phosphating Solution is 6160us/cm～9000us/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;
(2) 20 ℃ of left and right of normal temperature spray phosphatization, and phosphating time is 1.5min;
(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, specifically expands
Situation 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 quick environment protection type Phosphating Solution, it is characterized in that, by weight, comprise following component: ammonium fluozirconate 4%～6%, hydrofluoric acid 5%～7%, boric acid 1%～1.5%, ethylenediamine tetraacetic acid (EDTA) 0.1%～0.2%, zinc molybdate 0.5%～1.5%, surplus is water, the conductivity range of described Phosphating Solution is 6160us/cm～9000us/cm, and PH scope is 3.86～4.68.
2. quick environment protection type Phosphating Solution according to claim 1, is characterized in that: by weight, comprise following component: ammonium fluozirconate 4%, and hydrofluoric acid 5%, boric acid 1%, ethylenediamine tetraacetic acid (EDTA) 0.1%, zinc molybdate 0.5%, surplus is water.
3. quick environment protection type Phosphating Solution according to claim 1, is characterized in that: by weight, comprise following component: ammonium fluozirconate 5%, and hydrofluoric acid 6%, boric acid 1.25%, ethylenediamine tetraacetic acid (EDTA) 0.15%, zinc molybdate 1%, surplus is water.
4. quick environment protection type Phosphating Solution according to claim 1, is characterized in that: by weight, comprise following component: ammonium fluozirconate 6%, and hydrofluoric acid 7%, boric acid 1.5%, ethylenediamine tetraacetic acid (EDTA) 0.2%, zinc molybdate 1.5%, surplus is water.
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| CN104962899B (en) * | 2015-07-17 | 2017-10-31 | 青岛格瑞烯金属防护科技有限公司 | One kind is without phosphorous oxyacid graphite alkene metal surface pretreatment liquid and application method |
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| ES2448829T3 (en) * | 2002-12-24 | 2014-03-17 | Chemetall Gmbh | Chemical conversion coating agent and surface treated metal |
| JP2008174807A (en) * | 2007-01-19 | 2008-07-31 | Nippon Hyomen Kagaku Kk | Chromium-free metal surface treatment liquid |
| CN101487117B (en) * | 2009-02-25 | 2010-12-08 | 西安建筑科技大学 | Preparation of aluminum alloy surface fluoroaluminate conversion film |
| CN101701336B (en) * | 2009-11-26 | 2011-04-13 | 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 |
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Non-Patent Citations (2)
| Title |
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| 满瑞林等.镀锌钢板表面无铬钝化研究进展.《河南化工》.2008,第25卷(第11期),第6-10页. |
| 镀锌钢板表面无铬钝化研究进展;满瑞林等;《河南化工》;20081231;第25卷(第11期);第6-10页 * |
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Denomination of invention: Quick environment-friendly phosphorus-free 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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Date of cancellation: 20190530 Granted publication date: 20140402 Pledgee: Huizhou Merchants Bank, Hefei Shuguang Road subbranch Pledgor: Anhui Qiming Surface Technology Co., Ltd. Registration number: 2017340000074 |