CN105970202A - Hydroxylamine-modified phosphating solution and preparation method thereof - Google Patents
Hydroxylamine-modified phosphating solution and preparation method thereof Download PDFInfo
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- CN105970202A CN105970202A CN201610373108.4A CN201610373108A CN105970202A CN 105970202 A CN105970202 A CN 105970202A CN 201610373108 A CN201610373108 A CN 201610373108A CN 105970202 A CN105970202 A CN 105970202A
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- azanol
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
- C23C22/36—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
- C23C22/367—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing alkaline earth metal cations
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Abstract
The invention discloses a hydroxylamine-modified phosphating solution and a preparation method thereof. The hydroxylamine-modified phosphating solution is prepared from the following components in parts by weight: 22-46 parts of zinc oxide, 13-32 parts of phosphoric acid, 12-25 parts of nitric acid, 14-28 parts of citric acid, 12-25 parts of zinc nitrate, 16-28 parts of calcium carbonate, 14-26 parts of copper nitrate, 18-33 parts of manganese dihydrogen phosphate, 22-42 parts of hydroxylamine, 14-28 parts of fluorozirconate, 12-25 parts of nanometre silver oxide, 13-28 parts of nanometrebarium chloride and 22-45 parts of water. Compared with the prior art, the hydroxylamine-modified phosphating solution disclosed by the invention has the following advantages: (1) the hydroxylamine-modified phosphating solution disclosed by the invention is low in energy consumption, and capable of ensuring the quality of a phosphating film; (2) the hydroxylamine-modified phosphating solution disclosed by the invention is low in toxicity and pollution; and (3) the phosphating solution disclosed by the invention is low in concentration and cost.
Description
Technical field
The present invention relates to steel surface process field, particularly relate to a kind of azanol modification Phosphating Solution and preparation method thereof.
Background technology
The mankind smelt iron with a long history, and people learn to smelt iron and shortly occur in that steel-making in fact.Because the mechanical property of steel is better than ferrum,
Obtain the favor of people soon, be widely used in every profession and trade.Due to technical conditions lagging in development at that time, steel produces
The limitation of amount makes people can not be met the demand of iron and steel.Until after the industrial revolution, plant equipment operating replaces part hands
Work operates, and smelting iron and steel is paid attention to and quickly grown.Since 21st century iron and steel play especially in human lives can not or
The effect lacked, becomes most important metal material, and in engineering, consumption is the most most.
Iron and steel is to add the alloy that the elements such as C, Si, P, S, Mn are smelted in ferrum, is most important in industrial and agricultural production
Structural material.But the shortcoming of steel product maximum is easily corrosion, iron and steel corrosion the economic loss caused is the most surprising, China
The ferrous materials scrapped because of steel corrosion every year accounts for the 1/4 of iron and steel output, and the product line caused because of its corrosion and damage is stopped work, yield
The serious consequences such as minimizing, defect ware increases, environmental pollution increases the weight of, human body health is on the hazard have no way of estimating especially.Therefore,
The effect of China's economy and social development be should not be underestimated by the research of anticorrosion of iron and steel.
Phosphatization refer to metal surface after either physically or chemically cleaning, under the conditions of specific temperature and time etc., use oil removing,
A series of technological process and the brushing such as rust cleaning, table tune, phosphatization, washing, impregnate, spray, spray the methods such as combination, and press
There is chemistry or electrochemical reaction in the Phosphating Solution that certain formula makes, generate one layer of phosphating coat in metal surface.The phosphorus that phosphatization is formed
Changing film and be typically complex salt crystal film, structure is the most more complicated, and the composition that phosphate compounds is in phosphating coat is by several factors
(the reagent composition of Phosphating Solution and proportioning, the attribute of metal phosphate, free phosphoric acid are to the erosive velocity of metal works, phosphatization side
The formula impact on ion diffusion velocity, the temperature etc. of Phosphating Solution) impact.W.machu sums up the phosphate compounds of phosphating coat
There are about kind more than 30, relatively common phosphate compounds has phosphoric acid zinc salt (Zn3 (PO4) 2 4H2O), ferrous phosphate salt
(Fe3 (PO4) 2 8H2O), iron phosphate zinc salt (Zn2Fe (PO4) 2 4H2O), zinc phosphate calcium salt (Zn2Ca (PO4) 2 2H2O)
Deng.
Phosphating coat is the thin layer that a layer thickness is minimum, and its crystallization direction presses the bottom pattern of phosphating coat or by metallic surface structures shape
Becoming multidimensional lattice, overlap extension is on metal base surface, and constitutes firm adhesion therewith.Its effect is mainly manifested in:
(1) phosphating coat has bad electric conductivity, directly as the protecting film of metal, can stop the erosion of workpiece local environment medium；
(2) phosphating coat has porous, by increasing capacitance it is possible to increase the adhesive force of paint, can be as bottom before metal surface coating, and this is that phosphatization is the widest
General purposes, accounts for the 60%～70% of phosphatization application；(3) phosphating coat can also play lubrication, reduces work in producing
The friction produced because inevitably contacting between part.
Summary of the invention
Present invention solves the technical problem that and be: in order to overcome the defect of prior art, it is thus achieved that a kind of low energy consumption, low toxicity, low concentration
And the phosphating coat of low cost, the invention provides a kind of azanol modification Phosphating Solution and preparation method thereof.
Technical scheme: a kind of azanol modification Phosphating Solution, is made up of following components proportioning by weight: zinc oxide 22～46 parts,
Phosphatase 11 3～32 parts, nitric acid 12～25 parts, citric acid 14～28 parts, zinc nitrate 12～25 parts, calcium carbonate 16～28 parts,
Copper nitrate 14～26 parts, phosphate dihydrogen manganese 18～33 parts, azanol 22～42 parts, fluorine zirconic acid 14～28 parts, nano phase ag_2 o
12～25 parts, nanometer barium chloride 13～28 parts, water 22～45 parts.
Preferably, described azanol modification Phosphating Solution is made up of following components proportioning by weight: zinc oxide 38 parts, phosphoric acid 26
Part, 21 parts of nitric acid, citric acid 24 parts, zinc nitrate 22 parts, calcium carbonate 23 parts, copper nitrate 20 parts, phosphate dihydrogen manganese 26
Part, azanol 36 parts, fluorine zirconic acid 22 parts, nano phase ag_2 o 19 parts, nanometer barium chloride 21 parts, 38 parts of water.
The preparation method of a kind of azanol modification Phosphating Solution, comprises the steps of
(1) nano phase ag_2 o, nanometer barium chloride, nitric acid being added to the water, be placed in ultrasonic stirrer, temperature is 40～52 DEG C,
Power is 19.4～21.9kHZ, stirs 7～22 minutes；
(2) in the ultrasonic stirrer described in step (1), phosphate dihydrogen manganese, azanol and fluorine zirconic acid are added, in ultrasonic stirrer
Temperature rises to 55～68 DEG C, and ultrasonic power is 19.5～21.5kHZ, and mixing time is 24～40 minutes, prepares nanometer plating solution；
(3) zinc oxide, phosphoric acid, citric acid, zinc nitrate, calcium carbonate and copper nitrate are mixed with water, add in autoclave,
Being 2.6～4.2MPa at pressure, temperature is reacted 32～50 minutes under the conditions of being 266～450 DEG C, prepares basic bath；
(4) basic bath that step (3) prepares is added in the nanometer plating solution that step (2) obtains, is placed in ultrasonic stirrer,
Being 52～66 DEG C in temperature, power is to react 30～55 minutes under the conditions of 19.7～21.9kHZ, can be prepared by azanol modification Phosphating Solution.
Preferably, nano phase ag_2 o, nanometer barium chloride, nitric acid are added to the water by step (1), are placed in ultrasonic stirrer,
Temperature is 47 DEG C, and power is 20.8kHZ, stirs 16 minutes.
Preferably, step (2) adds in the ultrasonic stirrer described in step (1) phosphate dihydrogen manganese, azanol and fluorine zirconic acid,
In ultrasonic stirrer, temperature rises to 62 DEG C, and ultrasonic power is 20.5kHZ, and mixing time is 34 minutes, prepares nanometer plating solution.
Preferably, zinc oxide, phosphoric acid, citric acid, zinc nitrate, calcium carbonate and copper nitrate are mixed in (3) by step with water, add
Entering in autoclave, be 3.7MPa at pressure, temperature is reacted 43 minutes under the conditions of being 413 DEG C, prepares basic bath.
Preferably, the basic bath that step (3) prepares is added in the nanometer plating solution that step (2) obtains by step (4), puts
In ultrasonic stirrer, being 62 DEG C in temperature, power is to react 48 minutes under the conditions of 21.2kHZ, can be prepared by azanol modified
Phosphating Solution.
Beneficial effect: the power consumption of (1) azanol of the present invention modification Phosphating Solution is few, and can guarantee that the quality of phosphating coat；(2) this
Bright described azanol modification Phosphating Solution low toxicity low stain；(3) Phosphating Solution concentration of the present invention is low and cost is relatively low.
Detailed description of the invention
Embodiment 1
A kind of azanol modification Phosphating Solution, is made up of following components proportioning by weight: zinc oxide 22 parts, phosphatase 11 3 parts, nitre
Acid 12 parts, citric acid 14 parts, zinc nitrate 12 parts, calcium carbonate 16 parts, copper nitrate 14 parts, phosphate dihydrogen manganese 18 parts, hydroxyl
Amine 22 parts, fluorine zirconic acid 14 parts, nano phase ag_2 o 12 parts, nanometer barium chloride 13 parts, 22 parts of water.
The preparation method of a kind of azanol modification Phosphating Solution, comprises the steps of
(1) nano phase ag_2 o, nanometer barium chloride, nitric acid being added to the water, be placed in ultrasonic stirrer, temperature is 40 DEG C,
Power is 19.4kHZ, stirs 7 minutes；
(2) in the ultrasonic stirrer described in step (1), phosphate dihydrogen manganese, azanol and fluorine zirconic acid are added, in ultrasonic stirrer
Temperature rises to 55 DEG C, and ultrasonic power is 19.5kHZ, and mixing time is 24 minutes, prepares nanometer plating solution；
(3) zinc oxide, phosphoric acid, citric acid, zinc nitrate, calcium carbonate and copper nitrate are mixed with water, add in autoclave,
Being 2.6MPa at pressure, temperature is reacted 32 minutes under the conditions of being 266 DEG C, prepares basic bath；
(4) basic bath that step (3) prepares is added in the nanometer plating solution that step (2) obtains, is placed in ultrasonic stirrer,
Being 52 DEG C in temperature, power is to react 30 minutes under the conditions of 19.7kHZ, can be prepared by azanol modification Phosphating Solution.
Embodiment 2
A kind of azanol modification Phosphating Solution, is made up of following components proportioning by weight: zinc oxide 38 parts, phosphoric acid 26 parts, nitre
Acid 21 parts, citric acid 24 parts, zinc nitrate 22 parts, calcium carbonate 23 parts, copper nitrate 20 parts, phosphate dihydrogen manganese 26 parts, hydroxyl
Amine 36 parts, fluorine zirconic acid 22 parts, nano phase ag_2 o 19 parts, nanometer barium chloride 21 parts, 38 parts of water.
The preparation method of a kind of azanol modification Phosphating Solution, comprises the steps of
(1) nano phase ag_2 o, nanometer barium chloride, nitric acid being added to the water, be placed in ultrasonic stirrer, temperature is 47 DEG C,
Power is 20.8kHZ, stirs 16 minutes；
(2) in the ultrasonic stirrer described in step (1), phosphate dihydrogen manganese, azanol and fluorine zirconic acid are added, in ultrasonic stirrer
Temperature rises to 62 DEG C, and ultrasonic power is 20.5kHZ, and mixing time is 34 minutes, prepares nanometer plating solution；
(3) zinc oxide, phosphoric acid, citric acid, zinc nitrate, calcium carbonate and copper nitrate are mixed with water, add in autoclave,
Being 3.7MPa at pressure, temperature is reacted 43 minutes under the conditions of being 413 DEG C, prepares basic bath；
(4) basic bath that step (3) prepares is added in the nanometer plating solution that step (2) obtains, is placed in ultrasonic stirrer,
Being 62 DEG C in temperature, power is to react 48 minutes under the conditions of 21.2kHZ, can be prepared by azanol modification Phosphating Solution.
Embodiment 3
A kind of azanol modification Phosphating Solution, is made up of following components proportioning by weight: zinc oxide 46 parts, phosphoric acid 32 parts, nitre
Acid 25 parts, citric acid 28 parts, zinc nitrate 25 parts, calcium carbonate 28 parts, copper nitrate 26 parts, phosphate dihydrogen manganese 33 parts, hydroxyl
Amine 42 parts, fluorine zirconic acid 28 parts, nano phase ag_2 o 25 parts, nanometer barium chloride 28 parts, 45 parts of water.
The preparation method of a kind of azanol modification Phosphating Solution, comprises the steps of
(1) nano phase ag_2 o, nanometer barium chloride, nitric acid being added to the water, be placed in ultrasonic stirrer, temperature is 52 DEG C,
Power is 21.9kHZ, stirs 22 minutes；
(2) in the ultrasonic stirrer described in step (1), phosphate dihydrogen manganese, azanol and fluorine zirconic acid are added, in ultrasonic stirrer
Temperature rises to 68 DEG C, and ultrasonic power is 21.5kHZ, and mixing time is 40 minutes, prepares nanometer plating solution；
(3) zinc oxide, phosphoric acid, citric acid, zinc nitrate, calcium carbonate and copper nitrate are mixed with water, add in autoclave,
Being 4.2MPa at pressure, temperature is reacted 50 minutes under the conditions of being 450 DEG C, prepares basic bath；
(4) basic bath that step (3) prepares is added in the nanometer plating solution that step (2) obtains, is placed in ultrasonic stirrer,
Being 66 DEG C in temperature, power is to react 55 minutes under the conditions of 21.9kHZ, can be prepared by azanol modification Phosphating Solution.
The azanol modification Phosphating Solution preparing embodiment 1～3 carries out performance detection, and result is as shown in the table:
Claims (7)
1. an azanol modification Phosphating Solution, it is characterised in that be made up of following components proportioning by weight: zinc oxide 22～46 parts,
Phosphatase 11 3～32 parts, nitric acid 12～25 parts, citric acid 14～28 parts, zinc nitrate 12～25 parts, calcium carbonate 16～28
Part, copper nitrate 14～26 parts, phosphate dihydrogen manganese 18～33 parts, azanol 22～42 parts, fluorine zirconic acid 14～28 parts, nanometer
Silver oxide 12～25 parts, nanometer barium chloride 13～28 parts, water 22～45 parts.
A kind of azanol modification Phosphating Solution the most according to claim 1, it is characterised in that by following components proportioning system by weight
Become: zinc oxide 38 parts, phosphoric acid 26 parts, 21 parts of nitric acid, citric acid 24 parts, zinc nitrate 22 parts, calcium carbonate 23 parts,
Copper nitrate 20 parts, phosphate dihydrogen manganese 26 parts, azanol 36 parts, fluorine zirconic acid 22 parts, nano phase ag_2 o 19 parts, nanometer chlorine
Change barium 21 parts, 38 parts of water.
3. the preparation method of a kind of azanol modification Phosphating Solution described in claim 1, it is characterised in that comprise the steps of
(1) nano phase ag_2 o, nanometer barium chloride, nitric acid being added to the water, be placed in ultrasonic stirrer, temperature is 40～52 DEG C,
Power is 19.4～21.9kHZ, stirs 7～22 minutes；
(2) in the ultrasonic stirrer described in step (1), phosphate dihydrogen manganese, azanol and fluorine zirconic acid are added, in ultrasonic stirrer
Temperature rises to 55～68 DEG C, and ultrasonic power is 19.5～21.5kHZ, and mixing time is 24～40 minutes, prepares nanometer plating solution；
(3) zinc oxide, phosphoric acid, citric acid, zinc nitrate, calcium carbonate and copper nitrate are mixed with water, add in autoclave,
Being 2.6～4.2MPa at pressure, temperature is reacted 32～50 minutes under the conditions of being 266～450 DEG C, prepares basic bath；
(4) basic bath that step (3) prepares is added in the nanometer plating solution that step (2) obtains, is placed in ultrasonic stirrer,
Being 52～66 DEG C in temperature, power is to react 30～55 minutes under the conditions of 19.7～21.9kHZ, can be prepared by azanol modification Phosphating Solution.
The preparation method of a kind of azanol modification Phosphating Solution the most according to claim 3, it is characterised in that will receive in step (1)
Rice silver oxide, nanometer barium chloride, nitric acid are added to the water, and are placed in ultrasonic stirrer, and temperature is 47 DEG C, and power is 20.8kHZ,
Stir 16 minutes.
The preparation method of a kind of azanol modification Phosphating Solution the most according to claim 3, it is characterised in that to step in step (2)
Suddenly adding phosphate dihydrogen manganese, azanol and fluorine zirconic acid in the ultrasonic stirrer described in (1), in ultrasonic stirrer, temperature rises to 62 DEG C,
Ultrasonic power is 20.5kHZ, and mixing time is 34 minutes, prepares nanometer plating solution.
The preparation method of a kind of azanol modification Phosphating Solution the most according to claim 3, it is characterised in that by oxygen in step (3)
Change zinc, phosphoric acid, citric acid, zinc nitrate, calcium carbonate and copper nitrate to mix with water, add in autoclave, at pressure be
3.7MPa, temperature is reacted 43 minutes under the conditions of being 413 DEG C, is prepared basic bath.
The preparation method of a kind of azanol modification Phosphating Solution the most according to claim 3, it is characterised in that will step in step (4)
Suddenly the basic bath that (3) prepare adds in the nanometer plating solution that step (2) obtains, and is placed in ultrasonic stirrer, in temperature is
62 DEG C, power is to react 48 minutes under the conditions of 21.2kHZ, can be prepared by azanol modification Phosphating Solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109531065A (en) * | 2018-12-05 | 2019-03-29 | 东莞市鼎通精密五金股份有限公司 | A kind of communications connectors outer conductor processing method |
| CN111455431A (en) * | 2020-05-15 | 2020-07-28 | 东莞市颖兴金属表面处理材料有限公司 | Preparation method of electrolytic phosphating solution |
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|---|---|---|---|---|
| CN102703889A (en) * | 2012-05-28 | 2012-10-03 | 武汉永正科技发展有限公司 | Low-temperature single-component zinc series phosphating solution and preparation method thereof |
| CN103422082A (en) * | 2012-05-17 | 2013-12-04 | 中化化工科学技术研究总院 | Neodymium-iron-boron magnetic material zinc-series phosphatization liquid and application method thereof |
| JP2015134957A (en) * | 2013-12-18 | 2015-07-27 | 日本パーカライジング株式会社 | Aqueous metal surface treatment agent, metal surface treatment film and metal material having metal surface treatment film |
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2016
- 2016-05-31 CN CN201610373108.4A patent/CN105970202B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103422082A (en) * | 2012-05-17 | 2013-12-04 | 中化化工科学技术研究总院 | Neodymium-iron-boron magnetic material zinc-series phosphatization liquid and application method thereof |
| CN102703889A (en) * | 2012-05-28 | 2012-10-03 | 武汉永正科技发展有限公司 | Low-temperature single-component zinc series phosphating solution and preparation method thereof |
| JP2015134957A (en) * | 2013-12-18 | 2015-07-27 | 日本パーカライジング株式会社 | Aqueous metal surface treatment agent, metal surface treatment film and metal material having metal surface treatment film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109531065A (en) * | 2018-12-05 | 2019-03-29 | 东莞市鼎通精密五金股份有限公司 | A kind of communications connectors outer conductor processing method |
| CN111455431A (en) * | 2020-05-15 | 2020-07-28 | 东莞市颖兴金属表面处理材料有限公司 | Preparation method of electrolytic phosphating solution |
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