CN102864446A - Normal-temperature phosphating solution and method for preparing same - Google Patents
Normal-temperature phosphating solution and method for preparing same Download PDFInfo
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- CN102864446A CN102864446A CN201210386179XA CN201210386179A CN102864446A CN 102864446 A CN102864446 A CN 102864446A CN 201210386179X A CN201210386179X A CN 201210386179XA CN 201210386179 A CN201210386179 A CN 201210386179A CN 102864446 A CN102864446 A CN 102864446A
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Abstract
The invention provides a normal-temperature phosphating solution and a method for preparing the same. The normal-temperature phosphating solution is mainly made from materials of hydroxylamine sulphate, phosphoric acid, sodium dihydrogen phosphate, fatty alcohol polyoxyethylene ether, cerous nitrate, zinc oxide, manganese phosphate and water. The preparation technology is simple and practicable, and the operation is convenient. The normal-temperature phosphating solution has competences of rust and oil fouling removing, and economizes the whole phosphating process by being combined with a sand blasting process; phosphating film after phosphating process has good anti-crazing, deformation resistant and shock resistant competences and a good combining capacity with an organic coating, and the phosphating film is a good base layer for the coating; and the normal temperature during a phosphating process is operable, the phosphating time is short, and the effect is good.
Description
Technical field
The present invention relates to a kind of normal-temperature phosphorizing liquid and preparation method thereof.
Background technology
Phosphatization is that iron and steel parts is processed in the solution that contains phosphoric acid salt, oxidation promotor, auxiliary agent, makes its surface form phosphatize phosphate coat.This phosphatize phosphate coat have protection against corrosion, wear-resisting, improve coating adhesion, the effect such as lubricated.Steel surface is carried out bonderizing, and the Phosphating Solution use temperature that tradition is used is high, power consumption is large, the time is long, cost is high.For resembling the large-scale workpieces such as automobile chassis and component, if carry out the medium and high temperature phosphatization, concerning some medium-sized and small enterprises, relatively more difficult especially.Along with the progress of phosphorization technology, Modern Phosphating is processed main towards low temperature, form the future development thin and phosphate layer that barrier propterty is good fast.
A kind of situation of prior art is, zinc nitrate, primary zinc phosphate are dissolved in the water by a certain percentage, uses as Phosphating Solution.Because the Phosphating Solution component is too simple, there is certain defect in the phosphorization film quality that forms thus, directly affects the quality of follow-up converted products.
Patent No. ZL200710039973.6, name is called to disclose in the Chinese invention patent of " adopting ozone as the method for bonderizing of steel iron phosphatising accelerator " uses ozone as the method for bonderizing of Phosphating Accelerant, but in the method, the soak time of workpiece in Phosphating Solution still needed more than 15 minutes, and in 0.01mol/L phenyl dioster diphosphate solution, soak 50min can be so that copper sulfate drop corrosion experiment result be 419S.Therefore this method for bonderizing length consuming time, poor effect.
Application number is 200410094007.0, name is called in the Chinese invention patent application prospectus of " process liquid for alramenting hardware " and discloses a kind of hydrogen peroxide that adopts as the method for bonderizing of Phosphating Accelerant, but the method is difficult to stablize the concentration of hydrogen peroxide in the Phosphating Solution, and produces easily phosphating dregs.
Phosphating Solution Sodium Nitrite commonly used or sodium chlorate are promotor in the prior art, and the shortcoming that the former produces easily is unstable in acid Phosphating Solution, decompose easily, if content is controlled bad meeting and greatly affected the phosphatization effect in the Phosphating Solution; The latter can be reduced into chlorion, and chlorion accumulates in tank liquor, if washing subsequently is insufficient, chlorion is stayed on the workpiece, can bring very large future trouble.Pollute electrophoresis groove liquid on the one hand, stay on the other hand under the coating, can accelerate corrosion speed.
Therefore, it is effective to seek a kind of phosphatization, and the Phosphating Solution of parkerizing process simple and fast has great importance.
Summary of the invention
The present invention aims to provide a kind of normal-temperature phosphorizing liquid and preparation method thereof, and this normal-temperature phosphorizing liquid phosphating formula is reasonable, simple for process, speed piece, effective, and applied range, the phosphatize phosphate coat corrosion resistance nature of formation is good.
Normal-temperature phosphorizing liquid of the present invention is that the raw material by following weight percent is prepared from:
Oxyammonia sulfate 0.5～1% phosphatase 11 8～24% SODIUM PHOSPHATE, MONOBASIC 2～5%
Fatty alcohol-polyoxyethylene ether 0.5～2% cerous nitrate 0.6～1% zinc oxide 4～8%
Manganous phosphate 2～4% surpluses are water.
Normal-temperature phosphorizing liquid of the present invention is prepared from by following preferred weight percent raw material:
Oxyammonia sulfate 0.6 phosphoric acid 22% SODIUM PHOSPHATE, MONOBASIC 4%
Fatty alcohol-polyoxyethylene ether 1% cerous nitrate 0.8% zinc oxide 6%
Manganous phosphate 3% surplus is water.
Normal-temperature phosphorizing liquid of the present invention is prepared from by following methods:
Get zinc oxide and add a small amount of water furnishing pasty state, phosphoric acid is slowly added wherein, constantly stir, until become the liquid of transparent clear, mix; Then add successively manganous phosphate, cerous nitrate, SODIUM PHOSPHATE, MONOBASIC, oxyammonia sulfate and fatty alcohol-polyoxyethylene ether, the limit edged stirs, and mixes, and adds the water of surplus, mixes, leave standstill 2 ~ 6 hours after, and get final product.
The method of normal-temperature phosphorizing liquid phosphatization steel of the present invention may further comprise the steps:
After steel are carried out sandblasting, immerse in the Phosphating Solution, the Phosphating Solution temperature is controlled at 20 ~ 30 ℃, soaks 5 ~ 15 minutes.
Normal-temperature phosphorizing liquid of the present invention, fatty alcohol-polyoxyethylene ether cooperate phosphoric acid salt, can remove preferably the residual greasy dirt of steel surface after the sandblasting, promote the phosphatization effect; Higher acidity control can be removed the residual rusty stain of steel surface after the sandblasting; Oxyammonia sulfate is the promotor of reaction, is used for accelerating the carrying out of phosphating reaction, and cerous nitrate can make the metallic surface produce unpolarizing, for phosphating reaction certain promoter action is arranged also; SODIUM PHOSPHATE, MONOBASIC is used for the phosphoric acid that generation is carried out in the slowly-releasing reaction, keeps potential of hydrogen; Zinc, manganese phosphate coating have effectively increased corrosion resistance and the wear resistance of phosphatize phosphate coat after having added the suitable cerium ion of consumption.
Normal-temperature phosphorizing liquid of the present invention has certain removal rusty stain and the ability of greasy dirt, in conjunction with sandblasting technique, has saved whole phosphatization operation, does not need to carry out special degreasing and acidification etc. again; The sediment of phosphating solution is few, easy maintenance; The working temperature of phosphating solution is normal temperature, less energy consumption, and production cost is low; The phosphatize phosphate coat that produces behind the bonderizing has good shatter-resistant, anti-distortion, shock proof ability, with organic coating film good binding ability is arranged, and is the good bottom of filming; Parkerizing process normal temperature can operate, and phosphating time is short, and is effective.The present invention has outstanding substantive distinguishing features and significant progressive with respect to prior art.
Embodiment
Embodiment 1
Oxyammonia sulfate 0.5% phosphatase 11 8% SODIUM PHOSPHATE, MONOBASIC 2%
Fatty alcohol-polyoxyethylene ether 0.5% cerous nitrate 0.6% zinc oxide 4%
Manganous phosphate 2% surplus is water.
Get zinc oxide and add a small amount of water furnishing pasty state, phosphoric acid is slowly added wherein, constantly stir, until become the liquid of transparent clear, mix; Then add successively manganous phosphate, cerous nitrate, SODIUM PHOSPHATE, MONOBASIC, oxyammonia sulfate and fatty alcohol-polyoxyethylene ether, the limit edged stirs, and mixes, and adds the water of surplus, mixes, leave standstill 2 hours after, and get final product.
Embodiment 2
Oxyammonia sulfate 0.1% phosphoric acid 24% SODIUM PHOSPHATE, MONOBASIC 5%
Fatty alcohol-polyoxyethylene ether 2% cerous nitrate 1% zinc oxide 8%
Manganous phosphate 4% surplus is water.
Get zinc oxide and add a small amount of water furnishing pasty state, phosphoric acid is slowly added wherein, constantly stir, until become the liquid of transparent clear, mix; Then add successively manganous phosphate, cerous nitrate, SODIUM PHOSPHATE, MONOBASIC, oxyammonia sulfate and fatty alcohol-polyoxyethylene ether, the limit edged stirs, and mixes, and adds the water of surplus, mixes, leave standstill 6 hours after, and get final product.
Embodiment 3
Oxyammonia sulfate 0.6 phosphoric acid 22% SODIUM PHOSPHATE, MONOBASIC 4%
Fatty alcohol-polyoxyethylene ether 1% cerous nitrate 0.8% zinc oxide 6%
Manganous phosphate 3% surplus is water.
Get zinc oxide and add a small amount of water furnishing pasty state, phosphoric acid is slowly added wherein, constantly stir, until become the liquid of transparent clear, mix; Then add successively manganous phosphate, cerous nitrate, SODIUM PHOSPHATE, MONOBASIC, oxyammonia sulfate and fatty alcohol-polyoxyethylene ether, the limit edged stirs, and mixes, and adds the water of surplus, mixes, leave standstill 4 hours after, and get final product.
Embodiment 4
Prescription in inventive embodiments is the phosphatization antirust effect in neutral salt spray test:
Experimental program: in specific proofing box (electroplating device), to contain (5 scholar 0.5) % sodium-chlor, pH value and be 6.5～7.2 salt solution sprays by spraying plant, allow salt fog be deposited on to be tested, observed its surface corrosion state in per 12 hours.The temperature of proofing box is controlled at (35 ± 2) ℃, and humidity is greater than 95%, and falling the mist amount is 1～2mL/ (hcm2), and nozzle pressure is 78.5～137.3kPa (0.8～1.4kgf/cm2); Directly do not contact with casing when testpieces is placed in case, be placed on the special-purpose shelf, carry out in a continuous manner spray testing, per 12 hours is an observation phase.
Preparation of samples: the trade mark is 4 in the steel disc sample of Q295B, processes respectively through embodiment 1,2,3 Phosphating Solution, jointly carries out salt mist experiment with undressed steel disc;
The trade mark is 4 in the steel disc sample of Q345B, processes respectively through embodiment 1,2,3 Phosphating Solution, jointly carries out salt mist experiment with undressed steel disc;
The trade mark is 4 in the steel disc sample of Q390B, processes respectively through embodiment 1,2,3 Phosphating Solution, jointly carries out salt mist experiment with undressed steel disc;
Parkerizing method: after steel are carried out sandblasting, immerse in the Phosphating Solution, the Phosphating Solution temperature is controlled at 25 ℃, soaks 10 minutes, and taking-up cleans up, and get final product.
Experimental result sees the following form
| The sample title | Salt fog 12h | Salt fog 24h | Salt fog 36h | Salt fog 48h | Salt fog 60h |
| Q295B is phosphatization not | Without considerable change | Micro-rusty stain appears | A small amount of rusty stain appears | A small amount of rusty stain appears | More rusty stain appears |
| Q295B embodiment 1 | Without considerable change | Without considerable change | Without considerable change | Without considerable change | Without considerable change |
| Q295B embodiment 2 | Without considerable change | Without considerable change | Without considerable change | Without considerable change | Without considerable change |
| Q295B embodiment 3 | Without considerable change | Without considerable change | Without considerable change | Without considerable change | Without considerable change |
| Q345B is phosphatization not | Without considerable change | Micro-rusty stain appears | A small amount of rusty stain appears | A small amount of rusty stain appears | More rusty stain appears |
| Q345B embodiment 1 | Without considerable change | Without considerable change | Without considerable change | Without considerable change | Without considerable change |
| Q345B embodiment 2 | Without considerable change | Without considerable change | Without considerable change | Without considerable change | Without considerable change |
| Q345B embodiment 3 | Without considerable change | Without considerable change | Without considerable change | Without considerable change | Without considerable change |
| Q390B is phosphatization not | Without considerable change | Micro-rusty stain appears | A small amount of rusty stain appears | A small amount of rusty stain appears | More rusty stain appears |
| Q390B embodiment 1 | Without considerable change | Without considerable change | Without considerable change | Without considerable change | Without considerable change |
| Q390B embodiment 2 | Without considerable change | Without considerable change | Without considerable change | Without considerable change | Without considerable change |
| Q390B embodiment 3 | Without considerable change | Without considerable change | Without considerable change | Without considerable change | Without considerable change |
As seen from the above table, used the steel after the described Phosphating Solution of the embodiment of the invention is processed, its resistance to corrosion all has larger lifting.
Claims (4)
1. normal-temperature phosphorizing liquid is characterized in that it is that raw material by following weight percent is prepared from:
Oxyammonia sulfate 0.5～1% phosphatase 11 8～24% SODIUM PHOSPHATE, MONOBASIC 2～5%
Fatty alcohol-polyoxyethylene ether 0.5～2% cerous nitrate 0.6～1% zinc oxide 4～8%
Manganous phosphate 2～4% surpluses are water.
2. normal-temperature phosphorizing liquid as claimed in claim 1 is characterized in that it is that raw material by following weight percent is prepared from:
Oxyammonia sulfate 0.6 phosphoric acid 22% SODIUM PHOSPHATE, MONOBASIC 4%
Fatty alcohol-polyoxyethylene ether 1% cerous nitrate 0.8% zinc oxide 6%
Manganous phosphate 3% surplus is water.
3. normal-temperature phosphorizing liquid as claimed in claim 1 is characterized in that it is prepared from by following methods:
Get zinc oxide and add a small amount of water furnishing pasty state, phosphoric acid is slowly added wherein, constantly stir, until become the liquid of transparent clear, mix; Then add successively manganous phosphate, cerous nitrate, SODIUM PHOSPHATE, MONOBASIC, oxyammonia sulfate and fatty alcohol-polyoxyethylene ether, the limit edged stirs, and mixes, and adds the water of surplus, mixes, leave standstill 2 ~ 6 hours after, and get final product.
4. the method for normal-temperature phosphorizing liquid phosphatization steel as claimed in claim 1 is characterized in that may further comprise the steps:
After steel are carried out sandblasting, immerse in the Phosphating Solution, the Phosphating Solution temperature is controlled at 20 ~ 30 ℃, soaks 5 ~ 15 minutes, and taking-up cleans up, and get final product.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103255401A (en) * | 2013-05-28 | 2013-08-21 | 广西建工集团第五建筑工程有限责任公司 | Phosphating solution and preparation method thereof |
| CN104988477A (en) * | 2015-07-14 | 2015-10-21 | 武汉富诗特科技有限公司 | Normal-temperature phosphating fluid for drawing steel |
| CN105543826A (en) * | 2015-12-29 | 2016-05-04 | 钢铁研究总院 | Normal-temperature phosphating solution forming phosphating film highly resistant to corrosion, preparing method and phosphating technology |
| CN107904605A (en) * | 2017-12-18 | 2018-04-13 | 河北工业大学 | A kind of environment-friendly type acid pickling and rust removing antirust agent |
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| US4762572A (en) * | 1985-10-18 | 1988-08-09 | Gerhard Collardin Gmbh | Process for phosphating electrolytically zinc-coated metals |
| CN101724838A (en) * | 2008-10-17 | 2010-06-09 | 仪征威业油泵油嘴有限公司 | Preparation method of phosphating liquid |
| CN102719872A (en) * | 2012-06-08 | 2012-10-10 | 南京派诺金属表面处理技术有限公司 | Slag-free low-temperature rapid electrolytic phosphorizing liquid and phosphorizing process thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4762572A (en) * | 1985-10-18 | 1988-08-09 | Gerhard Collardin Gmbh | Process for phosphating electrolytically zinc-coated metals |
| CN101724838A (en) * | 2008-10-17 | 2010-06-09 | 仪征威业油泵油嘴有限公司 | Preparation method of phosphating liquid |
| CN102719872A (en) * | 2012-06-08 | 2012-10-10 | 南京派诺金属表面处理技术有限公司 | Slag-free low-temperature rapid electrolytic phosphorizing liquid and phosphorizing process thereof |
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| 谭旭翔: "钢铁常温磷化研究", 《中国优秀硕士学位论文全文数据库（电子期刊）》, no. 03, 15 March 2008 (2008-03-15) * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103255401A (en) * | 2013-05-28 | 2013-08-21 | 广西建工集团第五建筑工程有限责任公司 | Phosphating solution and preparation method thereof |
| CN104988477A (en) * | 2015-07-14 | 2015-10-21 | 武汉富诗特科技有限公司 | Normal-temperature phosphating fluid for drawing steel |
| CN104988477B (en) * | 2015-07-14 | 2018-12-07 | 武汉富诗特科技有限公司 | A kind of steel drawing group normal temperature phosphating treatment fluid |
| CN105543826A (en) * | 2015-12-29 | 2016-05-04 | 钢铁研究总院 | Normal-temperature phosphating solution forming phosphating film highly resistant to corrosion, preparing method and phosphating technology |
| CN105543826B (en) * | 2015-12-29 | 2018-05-01 | 钢铁研究总院 | A kind of normal-temperature phosphorizing liquid, preparation method and phosphating process for forming high anti-corrosion phosphating coat |
| CN107904605A (en) * | 2017-12-18 | 2018-04-13 | 河北工业大学 | A kind of environment-friendly type acid pickling and rust removing antirust agent |
| CN107904605B (en) * | 2017-12-18 | 2019-11-05 | 河北工业大学 | A kind of environment-friendly type acid pickling and rust removing antirust agent |
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Application publication date: 20130109 |