CN101787524B - Lamina wear-resisting phosphorization agent and preparation method thereof - Google Patents

Lamina wear-resisting phosphorization agent and preparation method thereof Download PDF

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CN101787524B
CN101787524B CN2010101223545A CN201010122354A CN101787524B CN 101787524 B CN101787524 B CN 101787524B CN 2010101223545 A CN2010101223545 A CN 2010101223545A CN 201010122354 A CN201010122354 A CN 201010122354A CN 101787524 B CN101787524 B CN 101787524B
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张春晖
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Wuhan Marine Machinery Plant Co Ltd
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Wuhan Marine Machinery Plant Co Ltd
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Abstract

The invention relates to a lamina wear-resisting phosphorization agent and a preparation method thereof. The phosphorization agent has the following components and contents: 45-50g/l of manganous salt, 1-2ml/l phosphoric acid, 2-4g/l of nickel nitrate, 2-10g/l of nitrate of lime, 0.5-2g/l of zinc nitrate, 3-5g/l of scrap iron, 1-3g/l of citric acid, moderate amount of manganese carbonate for adjusting free acidity and the balance of water; total acidity of the phosphorization stands at 45-50 points, free acidity stands at 6.5-7.5 points and the proportion of the total acidity to the free acidity is 6:1 to 7:11.When the phosphorization agent is prepared, 40-45g/l of manganous salt is weighed and placed in water of 70 DEG C to be dissolved; water is supplemented after the manganous salt is completely dissolved; then the mixed solution is heated to boiling state and then cooled to 70 DEG C before adding 3-5g/l of scrap iron for carrying out reaction for 30-45min; then 0.5-2.0ml/l of phosphoric acid is added; sampling analysis is carried out and acidity of the solution is adjusted; then 2-4g/l of nickel nitrate, 2-10g/l of nitrate of lime, 0.5-2g/l of zinc nitrate are added; sampling analysis is carried out and acidity of the solution is adjusted again; after testing is passed, 1-3g/l of citric acid is added to obtain the phosphorization agent.

Description

A kind of lamina wear-resisting phosphorization agent and compound method thereof
Technical field
The present invention relates to a kind of phosphatization liquid, relate in particular to a kind of lamina wear-resisting phosphorization agent and compound method thereof, be applicable to that specifically the anti-attrition at relative movement position between toothing face, motor shell and the blade is lubricated.
Background technology
Phosphatization liquid can be used for the surface treatment of iron and steel.Iron and steel carries out bonderizing in containing the phosphatization liquid of manganese, zinc after, can generate the crystallization phosphatize phosphate coat of even compact on the surface of iron and steel, this film can improve the abrasion resistance of iron and steel, prolong the work-ing life of iron and steel, thereby phosphatization liquid is widely used in the surface treatment of part on aircraft, automobile, wheel box, transfer case and the various gear.
The Chinese patent publication number is CN101063199, the patent of invention that open day is on October 31st, 2007 discloses a kind of manganese phosphating liquor, the composition of this kind manganese phosphating liquor comprises: phosphoric acid, Mazhev salt, SODIUMNITRATE, zinc nitrate, nickelous nitrate, Sodium Nitrite, hydrogen peroxide, softening water, its ratio of weight and number is: phosphoric acid 2.0~8.0, Mazhev salt 1~10, SODIUMNITRATE 2~8, zinc nitrate 0.5~5, nickelous nitrate 3.0~5.0, Sodium Nitrite 1~4, hydrogen peroxide 0.5~6, softening water 45~60, though this kind manganese phosphating liquor can improve the anti-attrition of mechanical component, improve the abrasion resistance of mechanical component, but the Sodium Nitrite that contains in this kind manganese phosphating liquor is poisonous, can pollute, and the rete of the phosphatize phosphate coat of this kind manganese phosphating liquor formation is blocked up, hardness is not strong, wear resistance is not high.
Summary of the invention
The objective of the invention is to overcome exist in the prior art contain toxic substance and rete is blocked up, hardness is strong, wear resistance is not high defective and problem, provide that a kind of rete is moderate, hardness is strong, wear resistance is higher, and does not comprise the lamina wear-resisting phosphorization agent and the compound method thereof of toxic substance.
For realizing above purpose, technical solution of the present invention is: a kind of lamina wear-resisting phosphorization agent, the moiety of this phosphatization liquid and content thereof are: Mazhev salt 45~50g/l, concentration of volume percent are phosphatase 11~2ml/l of 84%, nickelous nitrate 2~4g/l, nitrocalcite 2~10g/l, zinc nitrate 0.5~2g/l, iron filings 3~5g/l, citric acid 1~3g/l, an amount of in order to the manganous carbonate of adjusting free acidity, surplus is a water; The total acidity of described phosphatization liquid is 45~50 points, and free acidity is 6.5~7.5 points, and the ratio of total acidity and free acidity is 6: 1~7: 1.
The moiety of described phosphatization liquid and content thereof are: Mazhev salt 48g/l, concentration of volume percent are 84% phosphatase 11 .5ml/l, nickelous nitrate 3g/l, nitrocalcite 6g/l, zinc nitrate 1.3g/l, iron filings 4g/l, citric acid 1.2g/l, an amount of in order to the manganous carbonate of adjusting free acidity, surplus is a water.
A kind of compound method of above-mentioned lamina wear-resisting phosphorization agent, this compound method is carried out according to the following steps successively:
The first step: take by weighing Mazhev salt 40~45g/l earlier and put into 70 ℃ water and dissolve, dissolving finishes back restock water to the volume that needs preparation, then solution is heated to boiling;
Second step: above-mentioned ebullient solution is carried out naturally cooling, add iron filings 3~5g/l when being cooled to 70 ℃, react that to add concentration of volume percent after 30~45 minutes again be phosphoric acid 0.5~2.0ml/l of 84%, the total acidity of sampling analysis solution and free acidity subsequently, adding Mazhev salt, water, concentration of volume percent according to the result of sampling analysis then is the acidity that 84% phosphoric acid and manganous carbonate are adjusted solution, total acidity until solution is 40~42 points, and total acidity is 6: 1~7: 1 with the ratio of free acidity;
The 3rd step: add nickelous nitrate 2~4g/l, nitrocalcite 2~10g/l, zinc nitrate 0.5~2g/l, the total acidity of sampling analysis solution and free acidity subsequently, result according to sampling analysis adds Mazhev salt again, water, concentration of volume percent is the acidity that 84% phosphoric acid and manganous carbonate are adjusted solution, total acidity until solution is 45~50 points, free acidity is 6.5~7.5 points, and total acidity is 6: 1~7: 1 with the ratio of free acidity, produce as a trial with little test piece then, and the thickness and the corrosion stability of phosphate coating in the little test piece in back are produced in inspection, after the passed examination, in solution, add citric acid 1~3g/l again and promptly make described phosphatization liquid.
Described interpolation Mazhev salt, water, concentration of volume percent are that 84% phosphoric acid and manganous carbonate are meant with the acidity of adjusting solution:
When total acidity is high, add water, consumption A=(the M-S)/S of water, wherein M counts for the total acidity of measuring, and S is counting of required total acidity, and A is the water yield that every liter of solution should be added, and unit is for rising;
When total acidity is hanged down, add Mazhev salt, whenever add total acidity 1 point that 1 gram Mazhev salt can improve every liter of solution, can improve free acidity 0.1~0.2 point of every liter of solution simultaneously;
When free acidity is high, add manganous carbonate, whenever add free acidity 1 point that 1 gram manganous carbonate can reduce every liter of solution;
When free acidity is hanged down, add phosphoric acid, whenever add concentration of volume percent and be 0.7 milliliter of 84% phosphoric acid, can improve free acidity 1 point of every liter of solution.
Compared with prior art, beneficial effect of the present invention is:
1. the moiety owing to phosphatization liquid in a kind of lamina wear-resisting phosphorization agent of the present invention and the compound method thereof is that Mazhev salt, concentration are 84% phosphoric acid, nickelous nitrate, nitrocalcite, zinc nitrate, iron filings, citric acid and manganous carbonate, do not have Sodium Nitrite, so the present invention does not comprise toxic substance.
2. the moiety owing to phosphatization liquid in a kind of lamina wear-resisting phosphorization agent of the present invention and the compound method thereof comprises nitrocalcite, and nitrocalcite can obviously improve the hardness and the wear resistance of rete, compare with the market like product, use this phosphatization liquid to prolong the friction durability of phosphate coating more than 80%, therefore not only hardness is stronger for the rete of the present invention's formation, and wear resistance is higher.
3. because the thicknesses of layers of a kind of lamina wear-resisting phosphorization agent of the present invention and the formed phosphatize phosphate coat of compound method thereof is 6~12 μ m, thickness is comparatively moderate, therefore the phosphatize phosphate coat that forms of the present invention neither can cause owing to thickness is blocked up crystal grain thick frangible, influence the life-span, can not cause the life-span short owing to thickness is thin excessively yet, and the rete crystal grain densification of the phosphatize phosphate coat of the present invention's formation, difficult broken, so the thicknesses of layers of the phosphatize phosphate coat of the present invention's formation is moderate, the life-span is longer.
A kind of lamina wear-resisting phosphorization agent, the moiety of this phosphatization liquid and content thereof are: Mazhev salt 45~50g/l, concentration of volume percent is phosphatase 11~2ml/l of 84%, nickelous nitrate 2~4g/l, nitrocalcite 2~10g/l, zinc nitrate 0.5~2g/l, iron filings 3~5g/l, citric acid 1~3g/l, an amount of in order to the manganous carbonate of adjusting free acidity, surplus is a water; The total acidity of described phosphatization liquid is 45~50 points, and free acidity is 6.5~7.5 points, and the ratio of total acidity and free acidity is 6: 1~7: 1.
Embodiment
The moiety of described phosphatization liquid and content thereof are: Mazhev salt 48g/l, concentration of volume percent are 84% phosphatase 11 .5ml/l, nickelous nitrate 3g/l, nitrocalcite 6g/l, zinc nitrate 1.3g/l, iron filings 4g/l, citric acid 1~3g/l, an amount of in order to the manganous carbonate of adjusting free acidity, surplus is a water.
The effect of each moiety is as follows:
Mazhev salt: chemical formula is nFe (H 2PO 4) 2MMn (H 2PO 4) 2, its Mn that provides 2+Ion can improve hardness, sticking power and the solidity to corrosion of phosphatize phosphate coat, and can make the color burn of phosphatize phosphate coat, and crystallization is even.
Concentration of volume percent is 84% phosphoric acid: chemical formula is H 3PO 4, can improve the free acidity of solution, every interpolation concentration of volume percent is 0.7 milliliter of 84% a phosphoric acid, can improve free acidity 1 point of every liter of solution.
Nickelous nitrate: chemical formula is Ni (NO 3) 26H 2O, it can strengthen the solidity to corrosion of phosphatize phosphate coat, and its content is high more, and phosphatize phosphate coat is just thin more.
Nitrocalcite: chemical formula is Ca (NO 3) 24H 2O, it can obviously improve the hardness and the wear resistance of phosphorization film layer.
Zinc nitrate: chemical formula is Zn (NO 3) 26H 2O, the Zn that it provided 2+Ion can be accelerated the speed of response of phosphatization, and makes the rete crystal grain densification of phosphatize phosphate coat, crystallization flicker that light be arranged, when zinc ion content is low, and the then loose obfuscation of film, too high levels is especially at Fe 2+And P 2O 5Content when also higher, crystal grain then can thick, arrangement disorder on the film, film is fragile and wherein lime is more, the more demonstration precipitated impurities of lime is more, this can cause rete loose, corrosion stability is defective.
Iron filings: chemical formula is Fe, and it can increase the content of ferrous ion.
Citric acid: chemical formula is C 6H 8O 7H 2O, but as the total acidity and the free acidity of its stabilizing solution of stablizer.
Manganous carbonate: chemical formula is MnCO 3, can reduce the free acidity of solution, whenever add free acidity 1 point that 1 gram manganous carbonate can reduce every liter of solution.
The total acidity of described phosphatization liquid is 45~50 points, and free acidity is 6.5~7.5 points, and the ratio of total acidity and free acidity is 6: 1~7: 1.
The effect of total acidity and free acidity is as follows:
Total acidity: improve the accelerated reaction of total acidity energy, and can make rete thin and careful, total acidity is too high, then rete attenuation, and total acidity is low excessively, and then speed of response is slow, and rete is thick and coarse.
Free acidity: free acidity is too high, then can prolong the time of reaction, and the thick porous of rete crystal grain, solidity to corrosion reduce, and in addition, also causes the content of ferrous ion to rise easily, increases the throw out in the solution, and that free acid is spent is low, and then film is thin even do not have a film.
A kind of compound method of described lamina wear-resisting phosphorization agent, this compound method is carried out according to the following steps successively:
The first step: take by weighing Mazhev salt 40~45g/l earlier and put into 70 ℃ water and dissolve, dissolving finishes back restock water to the volume that needs preparation, then solution is heated to boiling;
Second step: above-mentioned ebullient solution is carried out naturally cooling, add iron filings 3~5g/l when being cooled to 70 ℃, react that to add concentration of volume percent after 30~45 minutes again be phosphoric acid 0.5~2.0ml/l of 84%, the total acidity of sampling analysis solution and free acidity subsequently, adding Mazhev salt, water, concentration of volume percent according to the result of sampling analysis then is the acidity that 84% phosphoric acid and manganous carbonate are adjusted solution, total acidity until solution is 40~42 points, and total acidity is 6: 1~7: 1 with the ratio of free acidity;
The 3rd step: add nickelous nitrate 2~4g/l, nitrocalcite 2~10g/l, zinc nitrate 0.5~2g/l, the total acidity of sampling analysis solution and free acidity subsequently, result according to sampling analysis adds Mazhev salt again, water, concentration of volume percent is the acidity that 84% phosphoric acid and manganous carbonate are adjusted solution, total acidity until solution is 45~50 points, free acidity is 6.5~7.5 points, and total acidity is 6: 1~7: 1 with the ratio of free acidity, produce as a trial with little test piece then, and the thickness and the corrosion stability of phosphate coating in the little test piece in back are produced in inspection, after the passed examination, in solution, add citric acid 1~3g/l again and promptly make described phosphatization liquid.
Described interpolation Mazhev salt, water, concentration are that 84% phosphoric acid and manganous carbonate are meant with the acidity of adjusting solution:
When total acidity is high, add water, consumption A=(the M-S)/S of water, wherein M counts for the total acidity of measuring, and S is counting of required total acidity, and A is the water yield that every liter of solution should be added, and unit is for rising;
When total acidity is hanged down, add Mazhev salt, whenever add total acidity 1 point that 1 gram Mazhev salt can improve every liter of solution, can improve free acidity 0.1~0.2 point of every liter of solution simultaneously;
When free acidity is high, add manganous carbonate, whenever add free acidity 1 point that 1 gram manganous carbonate can reduce every liter of solution;
When free acidity is hanged down, add phosphoric acid, whenever add concentration of volume percent and be 0.7 milliliter of 84% phosphoric acid, can improve free acidity 1 point of every liter of solution.
Embodiment 1:
The lamina wear-resisting phosphorization agent of a kind of 1000l, the moiety of this phosphatization liquid and content thereof are: Mazhev salt 50000g, concentration of volume percent are 84% phosphatase 11 700ml, nickelous nitrate 3000g, nitrocalcite 3000g, zinc nitrate 500g, iron filings 5000g, citric acid 1000g, surplus is a water.
The total acidity of above-mentioned phosphatization liquid is 48.5, and free acidity is 7.0, and total acidity is 6.9: 1 with the ratio of free acidity.
A kind of compound method of above-mentioned lamina wear-resisting phosphorization agent, this compound method is carried out according to the following steps successively:
The first step: take by weighing Mazhev salt 45000g earlier and put into 70 ℃ 800l water and dissolve, dissolving finishes back restock water to 1000l, then solution is heated to boiling;
Second step: above-mentioned ebullient solution is carried out naturally cooling, add iron filings 5000g when being cooled to 70 ℃, react that to add concentration of volume percent after 45 minutes again be 84% phosphoric acid 500ml, the total acidity of sampling analysis solution and free acidity subsequently, the total acidity that records solution is 41.5, free acidity is 4.7, adding concentration of volume percent again is 84% phosphatase 11 200ml, the total acidity that records solution then is 41.5, and free acidity is 6.4, and total acidity is 6.4: 1 with the ratio of free acidity;
The 3rd step: in solution, add nickelous nitrate 3000g, nitrocalcite 3000g, zinc nitrate 500g again, the total acidity of sampling analysis solution and free acidity subsequently, the total acidity that records solution is 43.5, free acidity is 6.5, add Mazhev salt 5000g again, the total acidity that records solution then is 48.5, free acidity is 7.0, produce as a trial with little test piece subsequently, little test piece was reacted in solution 15 minutes, and the thickness that records phosphate coating in the little test piece is 6-8 μ m, against corrosion 3 minutes and 10 seconds, it is qualified to detect, and adds citric acid 1000g then and promptly make described phosphatization liquid in solution.
Embodiment 2:
The lamina wear-resisting phosphorization agent of a kind of 1000l, the moiety of this phosphatization liquid and content thereof are: Mazhev salt 48000g, concentration of volume percent are 84% phosphatase 11 500ml, nickelous nitrate 3000g, nitrocalcite 6000g, zinc nitrate 1300g, iron filings 4000g, citric acid 1200g, surplus is a water.
The total acidity of above-mentioned phosphatization liquid is 49, and free acidity is 7.1, and total acidity is 6.9: 1 with the ratio of free acidity.
A kind of compound method of above-mentioned lamina wear-resisting phosphorization agent, this compound method is carried out according to the following steps successively:
The first step: take by weighing Mazhev salt 44000g earlier and put into 70 ℃ 800l water and dissolve, dissolving finishes back restock water to 1000l, then solution is heated to boiling;
Second step: above-mentioned ebullient solution is carried out naturally cooling, add iron filings 4000g when being cooled to 70 ℃, react that to add concentration of volume percent after 40 minutes again be 84% phosphatase 11 000ml, the total acidity of sampling analysis solution and free acidity subsequently, the total acidity that records solution is 41.2, free acidity is 5.7, add concentration of volume percent again and be 84% phosphoric acid 500ml, the total acidity that records solution then is 41.3, and free acidity is 6.4, and total acidity is 6.4: 1 with the ratio of free acidity;
The 3rd step: in solution, add nickelous nitrate 3000g, nitrocalcite 6000g, zinc nitrate 1300g again, the total acidity of sampling analysis solution and free acidity subsequently, the total acidity that records solution is 45, free acidity is 6.4, add Mazhev salt 4000g again, the total acidity that records solution then is 49, free acidity is 7.1, produce as a trial with little test piece subsequently, little test piece was reacted in solution 9 minutes, and the thickness that records phosphate coating in the little test piece is 8-10 μ m, against corrosion 3 minutes and 5 seconds, it is qualified to detect, and adds citric acid 1200g then and promptly make described phosphatization liquid in solution.
Embodiment 3:
The lamina wear-resisting phosphorization agent of a kind of 1000l, the moiety of this phosphatization liquid and content thereof are: Mazhev salt 50000g, concentration of volume percent are 84% phosphatase 11 000ml, nickelous nitrate 3000g, nitrocalcite 3000g, zinc nitrate 500g, iron filings 3000g, citric acid 1000g, surplus is a water.
The total acidity of above-mentioned phosphatization liquid is 49.0, and free acidity is 7.2, and total acidity is 6.8: 1 with the ratio of free acidity.
A kind of compound method of above-mentioned lamina wear-resisting phosphorization agent, this compound method is carried out according to the following steps successively:
The first step: take by weighing Mazhev salt 43000g earlier and put into 70 ℃ 800l water and dissolve, dissolving finishes back restock water to 1000l, then solution is heated to boiling;
Second step: above-mentioned ebullient solution is carried out naturally cooling, add iron filings 3000g when being cooled to 70 ℃, react that to add concentration of volume percent after 30 minutes again be 84% phosphoric acid 500ml, the total acidity of sampling analysis solution and free acidity subsequently, the total acidity that records solution is 40, free acidity is 5.2, add concentration of volume percent again and be 84% phosphoric acid 500ml, the total acidity that records solution then is 40.1, and free acidity is 5.9, and total acidity is 6.8: 1 with the ratio of free acidity;
The 3rd step: in solution, add nickelous nitrate 3000g again, nitrocalcite 3000g, zinc nitrate 500g, the total acidity of sampling analysis solution and free acidity subsequently, the total acidity that records solution is 42.1, free acidity is 6.0, add Mazhev salt 7000g again, the total acidity that records solution then is 49.0, free acidity is 7.2, produce as a trial with little test piece subsequently, little test piece was reacted in solution 13 minutes, and the thickness that records phosphate coating in the little test piece is 9-11 μ m, against corrosion 3 minutes and 30 seconds, it is qualified to detect, and adds citric acid 1000g then and promptly make described phosphatization liquid in solution.
Embodiment 4:
The lamina wear-resisting phosphorization agent of a kind of 1000l, the moiety of this phosphatization liquid and content thereof are: Mazhev salt 46000g, concentration of volume percent is 84% phosphoric acid 2000ml, nickelous nitrate 3000g, nitrocalcite 3000g, zinc nitrate 500g, iron filings 3000g, citric acid 1000g, in order to adjust the manganous carbonate 800g of free acidity, surplus is a water.
The total acidity of above-mentioned phosphatization liquid is 45, and free acidity is 6.8, and total acidity is 6.6: 1 with the ratio of free acidity.
A kind of compound method of above-mentioned lamina wear-resisting phosphorization agent, this compound method is carried out according to the following steps successively:
The first step: take by weighing Mazhev salt 43000g earlier and put into 70 ℃ 800l water and dissolve, dissolving finishes back restock water to 1000l, then solution is heated to boiling;
Second step: above-mentioned ebullient solution is carried out naturally cooling, add iron filings 3000g when being cooled to 70 ℃, react that to add concentration of volume percent after 32 minutes again be 84% phosphoric acid 500ml, the total acidity of sampling analysis solution and free acidity subsequently, the total acidity that records solution is 40, free acidity is 5.2, add concentration of volume percent again and be 84% phosphatase 11 500ml, the total acidity that records solution is 40.1, free acidity is 7.3, adds manganous carbonate 800g again, and the total acidity that records solution is 40.1, free acidity is 6.5, and total acidity is 6.2: 1 with the ratio of free acidity;
The 3rd step: in solution, add nickelous nitrate 3000g, nitrocalcite 3000g, zinc nitrate 500g again, the total acidity of sampling analysis solution and free acidity subsequently, the total acidity that records solution is 42.1, free acidity is 6.5, add Mazhev salt 3000g again, the total acidity that records solution then is 45, free acidity is 6.8, produce as a trial with little test piece subsequently, little test piece was reacted in solution 15 minutes, and the thickness that records phosphate coating in the little test piece is 10-12 μ m, against corrosion 3 minutes and 30 seconds, it is qualified to detect, and adds citric acid 1000g then and promptly make described phosphatization liquid in solution.
Embodiment 5:
The lamina wear-resisting phosphorization agent of a kind of 1000l, the moiety of this phosphatization liquid and content thereof are: Mazhev salt 46000g, concentration of volume percent is 84% phosphoric acid 2000ml, nickelous nitrate 3000g, nitrocalcite 3000g, zinc nitrate 500g, iron filings 3000g, citric acid 1000g, in order to adjust the manganous carbonate 800g of free acidity, surplus is a water.
The total acidity of above-mentioned phosphatization liquid is 45, and free acidity is 6.8, and total acidity is 6.6: 1 with the ratio of free acidity.
A kind of compound method of above-mentioned lamina wear-resisting phosphorization agent, this compound method is carried out according to the following steps successively:
The first step: take by weighing Mazhev salt 43000g earlier and put into 70 ℃ 800l water and dissolve, dissolving finishes back restock water to 1000l, then solution is heated to boiling;
Second step: above-mentioned ebullient solution is carried out naturally cooling, add iron filings 3000g when being cooled to 70 ℃, react that to add concentration of volume percent after 32 minutes again be 84% phosphoric acid 2000ml, the total acidity of sampling analysis solution and free acidity subsequently, the total acidity that records solution is 40.1, free acidity is 8.1, add manganous carbonate 1500g again, the total acidity that records solution is 40.1, and free acidity is 6.5, and total acidity is 6.2: 1 with the ratio of free acidity;
The 3rd step: in solution, add nickelous nitrate 3000g, nitrocalcite 3000g, zinc nitrate 500g again, the total acidity of sampling analysis solution and free acidity subsequently, the total acidity that records solution is 42.1, free acidity is 6.5, add Mazhev salt 3000g again, the total acidity that records solution then is 45, free acidity is 6.8, produce as a trial with little test piece subsequently, little test piece was reacted in solution 15 minutes, and the thickness that records phosphate coating in the little test piece is 10-12 μ m, against corrosion 3 minutes and 30 seconds, it is qualified to detect, and adds citric acid 1000g then and promptly make described phosphatization liquid in solution.

Claims (4)

1. lamina wear-resisting phosphorization agent, the moiety and the content thereof that it is characterized in that described phosphatization liquid are: Mazhev salt 45~50g/l, concentration of volume percent is phosphatase 11~2ml/l of 84%, nickelous nitrate 2~4g/l, nitrocalcite 2~10g/l, zinc nitrate 0.5~2g/l, iron filings 3~5g/l, citric acid 1~3g/l, an amount of in order to the manganous carbonate of adjusting free acidity, surplus is a water; The total acidity of described phosphatization liquid is 45~50 points, and free acidity is 6.5~7.5 points, and the ratio of total acidity and free acidity is 6: 1~7: 1.
2. a kind of lamina wear-resisting phosphorization agent according to claim 1, the moiety and the content thereof that it is characterized in that described phosphatization liquid are: Mazhev salt 48g/l, concentration of volume percent is 84% phosphatase 11 .5ml/l, nickelous nitrate 3g/l, nitrocalcite 6g/l, zinc nitrate 1.3g/l, iron filings 4g/l, citric acid 1.2g/l, an amount of in order to the manganous carbonate of adjusting free acidity, surplus is a water; The total acidity of described phosphatization liquid is 45~50 points, and free acidity is 6.5~7.5 points, and the ratio of total acidity and free acidity is 6: 1~7: 1.
3. the compound method of the described lamina wear-resisting phosphorization agent of claim 1 is characterized in that described compound method carries out according to the following steps successively:
The first step: take by weighing Mazhev salt 40~45g/l earlier and put into 70 ℃ water and dissolve, dissolving finishes back restock water to the volume that needs preparation, then solution is heated to boiling;
Second step: above-mentioned ebullient solution is carried out naturally cooling, add iron filings 3~5g/l when being cooled to 70 ℃, react that to add concentration of volume percent after 30~45 minutes again be 84% phosphoric acid, 0.5~2.0ml/l, the total acidity of sampling analysis solution and free acidity subsequently, adding Mazhev salt, water, concentration of volume percent according to the result of sampling analysis then is the acidity that 84% phosphoric acid and manganous carbonate are adjusted solution, total acidity until solution is 40~42 points, and total acidity is 6: 1~7: 1 with the ratio of free acidity;
The 3rd step: add nickelous nitrate 2~4g/l, nitrocalcite 2~10g/l, zinc nitrate 0.5~2g/l, the total acidity of sampling analysis solution and free acidity subsequently, result according to sampling analysis adds Mazhev salt again, water, concentration of volume percent is the acidity that 84% phosphoric acid and manganous carbonate are adjusted solution, total acidity until solution is 45~50 points, free acidity is 6.5~7.5 points, and total acidity is 6: 1~7: 1 with the ratio of free acidity, produce as a trial with little test piece then, and the thickness and the corrosion stability of phosphate coating in the little test piece in back are produced in inspection, after the passed examination, in solution, add citric acid 1~3g/l again and promptly make described phosphatization liquid.
4. the compound method of a kind of lamina wear-resisting phosphorization agent according to claim 3 is characterized in that: described interpolation Mazhev salt, water, concentration of volume percent are that the acidity that 84% phosphoric acid and manganous carbonate are adjusted solution is meant:
When total acidity is high, add water, consumption A=(the M-S)/S of water, wherein M counts for the total acidity of measuring, and S is counting of required total acidity, and A is the water yield that every liter of solution should be added, and unit is for rising;
When total acidity is hanged down, add Mazhev salt, whenever add total acidity 1 point that 1 gram Mazhev salt can improve every liter of solution, can improve free acidity 0.1~0.2 point of every liter of solution simultaneously;
When free acidity is high, add manganous carbonate, whenever add free acidity 1 point that 1 gram manganous carbonate can reduce every liter of solution;
When free acidity is hanged down, add phosphoric acid, whenever add concentration of volume percent and be 0.7 milliliter of 84% phosphoric acid, can improve free acidity 1 point of every liter of solution.
CN2010101223545A 2010-03-08 2010-03-08 Lamina wear-resisting phosphorization agent and preparation method thereof Active CN101787524B (en)

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