CN107523818A - A kind of preparation method of low-temperature metal phosphorizing liquid - Google Patents
A kind of preparation method of low-temperature metal phosphorizing liquid Download PDFInfo
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- CN107523818A CN107523818A CN201710843585.7A CN201710843585A CN107523818A CN 107523818 A CN107523818 A CN 107523818A CN 201710843585 A CN201710843585 A CN 201710843585A CN 107523818 A CN107523818 A CN 107523818A
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- temperature metal
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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
- C23C22/07—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 phosphates
- C23C22/08—Orthophosphates
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention provides a kind of preparation method of low-temperature metal phosphorizing liquid, by weight, 150 240 parts of phosphoric acid, 5 11 parts of tartaric acid, 39 parts of potassium chlorate, 0.01 0.1 part three（The benzene trihydroxy of 1,3 hexichol 1,3）(1,10 phenanthrolene), 15 part of four (ethyl-methyl amido) titanium (IV), 16 parts of ammonium citrates, 15 parts of triethanolamines, 18 part of three (8 oxyquinoline) gallium, 3 11 parts of aqueous polyurethanes, 14 parts of m-xylene diamines.
Description
Technical field
The present invention relates to the preparation method of metal phosphorizing liquid, especially a kind of preparation method of low-temperature metal phosphorizing liquid.
Background technology
Metal surface is because the pollution and corrosion of air can deposit various dirts and get rusty.This rust is mostly the oxidation of metal
Thing and hydroxide, they are loose and have hygroscopicity, make metal be more easy to continue to corrode.In addition, metal is processed in manufacture
Cheng Zhong, its surface can also leave the residue of various liquid or solids.Therefore, metallic article and part be before antirust treatment,
It must be surface-treated, make its appearance clean, so as to which complete coating and preferable protecting effect could be obtained.Pickling be
Metal surface occurs for the method for removing these rusts or debris is taken after the things such as rust, and phosphatization is one
Kind chemistry forms the process of phosphate chemical conversion film with electrochemical reaction, and the phosphate conversion film formed is referred to as phosphatization
Film.The purpose of phosphatization mainly provides protection to parent metal, prevents metal to be corroded to a certain extent, for being beaten before painting
Bottom, the adhesive force and anti-corrosion capability of paint film layer are improved, antifriction lubrication use is played in metal cold machining process.
CN200910013346.4, which discloses a kind of metal surface, to be needed to carry out the normal-temperature phosphorizing liquid of pre-treatment, and its technology will
Putting is：It includes a certain amount of nitric acid, zinc oxide or zinc powder, phosphoric acid, manganese carbonate, manganese nitrate or manganese sulfate, HF, NaF or
NH4F, nickel sulfate or nickel nitrate, zinc sulfate or zinc nitrate, it is finished product after fully being dissolved in appropriate water.The present invention's is normal
Warm phosphating solution can be according to the size of processed workpiece, and soaking, spray or wipe can be so that suitably adjustment time, is completed
Phosphorating treatment, and quality complies fully with requirement.The present invention has phosphating solution stability good, film formation time is long, film strength is big,
The advantages that corrosion resistance is strong；The present invention has wide range of applications, it may be said that all steel products, including industry and civilian industry all
It can use, such as：Air-conditioning and radiator and accessory, automobile and accessory, power equipment etc., and because normal temperature phosphating can save
Save time and the energy.
CN201310105719.7 discloses a kind of phosphating solution suitable for metal fastenings, is by following mass percent
Component composition：Phosphoric acid 3.5%, zinc oxide 0.6%, nitric acid 0.25%, nickel nitrate 4.0%, zinc nitrate 1.0%, nickel sulfate 1.5%,
Zinc sulfate 5.5%, manganese carbonate 0.2%, ethylenediamine tetra-acetic acid 0.02%, citric acid 2.0%, tartaric acid 2.8%, sodium perborate 0.7%, carbon
Sour sodium 2.3%, potassium chlorate 1.7%, surplus are water.Application method is：Diluted with 15 times of volume ratios, soak screw surface, during construction
Between be 3~40 minutes, temperature in use be 15~40 DEG C.The phosphating solution suitable for metal fastenings of the present invention, makes at normal temperatures
With not limited, can be soaked according to the size of processed workpiece, spray or wipe can be with by natural conditions；Complete phosphatization
Processing, can be in the excellent fine and close phosphatization crystalline film of metal fastenings surface forming properties, and continuous, uniform, film formation time is short, film forming
Intensity is big, and corrosion resistance is strong, and quality complies fully with requirement.
Phosphorating treatment is carried out for steel surface, the phosphating solution temperature in use that tradition uses is high, and power consumption is big, processing time
Long and cost is high, especially for large-scale workpieces such as lathe, automobile chassis and parts, if using high temperature phosphorization, to some
It is really relatively difficult for medium-sized and small enterprises.In recent years, had also been reported for normal-temperature phosphorizing liquid, but in use, during processing
Between it is long, and corrosion of its acidic materials to steel surface is larger, although disadvantages mentioned above can be overcome, this phosphating solution phosphatization
Afterwards, slightly not very, the phosphating coat of formation is thin, corrosion resistance is poor, phosphating time length.
The content of the invention
Present invention aims at solve above-mentioned technical problem present in prior art, there is provided a kind of low-temperature metal phosphorizing liquid
Preparation method, especially phosphorization membrane intensity is big, the formula and system of the short metal phosphorizing liquid of the strong phosphating time of corrosion resistance
Preparation Method, it is characterised in that following steps：
By weight, 150-240 parts phosphoric acid, 5-11 part tartaric acid, 3-9 part potassium chlorate, 0.01-0.1 parts three（1,3- hexichol -1,
3- benzene trihydroxies）(1,10- phenanthrolene), 1-5 parts four (ethyl-methyl amido) titanium (IV), 1-6 part ammonium citrates, 1-5 parts
Triethanolamine, 1-8 parts three (8-hydroxyquinoline)-gallium, 3-11 part aqueous polyurethanes, 1-4 part m-xylene diamines.Mix, add water
100-500 parts, 55-65 DEG C of stirring 40-120min is warming up to, then adds 1-6 parts surfactant, 1-5 part accelerator, stirring
Obtain low-temperature metal passivation phosphating solution.
The surfactant is tannic acid or DTAB.
The accelerator is thiocarbamide.
The product of the present invention has the advantages that：
A kind of preparation method of low-temperature metal phosphorizing liquid of the present invention, has the advantages that：
1st, the operating temperature of Phosphating with High Acidity Bath Solution liquid can be dropped to 0-20 DEG C, it is not necessary to heat, save big energy, simplify work
Sequence, shorten the production cycle.
2nd, ultralow temperature metal passivation phosphating solution is without the harmful substance such as chromate, nitrite, low operating temperatures bubble-free,
Acid mist will not be produced, three wastes are pollution-free, improve working environment.
3rd, there is special superiority to metal surface phosphating when less than 10 DEG C, phosphating solution good film-forming property, adhesive force is good, resistance to
Corrosivity is strong.Indoor rust-proof life can also avoid hydrogen embrittlement more than 1 year, can replace chemical oxidation, be not required to antirust oil of painting and apply
Preserve.
4th, production is easy, and cost is low.
Embodiment
Following instance is only to further illustrate the present invention, is not limitation the scope of protection of the invention.
Embodiment 1
By weight, 200 parts of phosphoric acid, 9 parts of tartaric acid, 6 parts of potassium chlorate, 0.07 part three（1,3- hexichol -1,3- benzene trihydroxies）(1,
10- phenanthrolenes), 4 part of four (ethyl-methyl amido) titanium (IV), 5 parts of ammonium citrates, 4 parts of triethanolamines, 7 part of three (8- hydroxyl
Quinoline)-gallium, 10 parts of aqueous polyurethanes, 1,3.5 parts of m-xylene diamines, mix, add 200 parts of water, be warming up to 60 DEG C of stirring 50min,
Then 5 parts of tannic acid, 4 parts of thiocarbamides are added, stir to obtain low-temperature metal phosphorizing liquid M-1.
Embodiment 2
By weight, 150 parts of phosphoric acid, 5 parts of tartaric acid, 3 parts of potassium chlorate, 0.01 part three（1,3- hexichol -1,3- benzene trihydroxies）(1,
10- phenanthrolenes), 1 part of four (ethyl-methyl amido) titanium (IV), 1 part of ammonium citrate, 1 part of triethanolamine, 1 part of three (8- hydroxyl
Quinoline)-gallium, 3 parts of aqueous polyurethanes, 1 part of m-xylene diamine.Mix, add 100 parts of water, be warming up to 55 DEG C of stirring 40min, then
1 part of DTAB is added, 1 part of thiocarbamide, stirs to obtain low-temperature metal phosphorizing liquid M-2.
Embodiment 3
By weight, 240 parts of phosphoric acid, 11 parts of tartaric acid, 9 parts of potassium chlorate, 0.1 part three（1,3- hexichol -1,3- benzene trihydroxies）(1,
10- phenanthrolenes), 5 part of four (ethyl-methyl amido) titanium (IV), 6 parts of ammonium citrates, 5 parts of triethanolamines, 8 part of three (8- hydroxyl
Quinoline)-gallium, 11 parts of aqueous polyurethanes, 4 parts of m-xylene diamines, mix, add 500 parts of water, be warming up to 65 DEG C of stirring 120min, so
6 parts of DTABs, 5 parts of thiocarbamides are added afterwards, stir to obtain low-temperature metal phosphorizing liquid M-3.
Comparative example 1
Step 1 is added without three (8-hydroxyquinoline)-galliums, and other conditions are the same as embodiment 1.Production code member M-4.
Comparative example 2
Step 1 is added without three（1,3- hexichol -1,3- benzene trihydroxies）(1,10- phenanthrolene), other conditions are the same as embodiment 1.
Production code member M-5.
Comparative example 3
Step 1 is added without four (ethyl-methyl amido) titaniums, and other conditions are the same as embodiment 1.Production code member M-6.
Comparative example 4
Step 1 is added without aqueous polyurethane, and other conditions are the same as embodiment 1.Production code member M-7.
Embodiment 4
The low-temperature metal phosphorizing liquid that embodiment 1-3 and comparative example 1-4 are produced, carries out the anti-corrosion time（h）, 5 DEG C of film forming when
Between (min), adhesive force detection（%）, concrete outcome is shown in Table 1.
Table 1：The low-temperature metal passivation phosphating solution anti-corrosion time that different process is produced（h）, it is 5 DEG C of film formation times (min), attached
Put forth effort to detect（%）Testing result.
Claims (4)
1. a kind of preparation method of low-temperature metal phosphorizing liquid, it is characterised in that comprise the following steps：
By weight, 150-240 parts phosphoric acid, 5-11 part tartaric acid, 3-9 part potassium chlorate, 0.01-0.1 parts three（1,3- hexichol -1,
3- benzene trihydroxies）(1,10- phenanthrolene), 1-5 parts four (ethyl-methyl amido) titanium (IV), 1-6 part ammonium citrates, 1-5 parts
Triethanolamine, 1-8 parts three (8-hydroxyquinoline)-gallium, 3-11 part aqueous polyurethanes, 1-4 part m-xylene diamines.
2. mixing, add water 100-500 parts, be warming up to 55-65 DEG C of stirring 40-120min, then add 1-6 parts surfactants,
1-5 part accelerator, stir to obtain low-temperature metal passivation phosphating solution.
3. the preparation method of a kind of low-temperature metal phosphorizing liquid described in claim 1, it is characterised in that the surfactant is
Tannic acid or DTAB.
4. the preparation method of a kind of low-temperature metal phosphorizing liquid described in claim 1, it is characterised in that the accelerator is thiocarbamide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710843585.7A CN107523818A (en) | 2017-09-19 | 2017-09-19 | A kind of preparation method of low-temperature metal phosphorizing liquid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710843585.7A CN107523818A (en) | 2017-09-19 | 2017-09-19 | A kind of preparation method of low-temperature metal phosphorizing liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113881934A (en) * | 2021-11-04 | 2022-01-04 | 湖南金化科技集团有限公司 | Zinc-based phosphating solution with less slag and ash |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5468734A (en) * | 1977-11-11 | 1979-06-02 | Nippon Packaging Kk | Surface treatment of tin plated steel plate and can |
| CN101974745A (en) * | 2010-10-27 | 2011-02-16 | 大连三达奥克化学股份有限公司 | Normal temperature bonderite for renovating flow string and manufacture method |
| CN105951084A (en) * | 2016-06-27 | 2016-09-21 | 无锡伊佩克科技有限公司 | Ultralow-temperature metal passivation phosphorizing liquid and preparation method thereof |
| CN105951082A (en) * | 2016-06-27 | 2016-09-21 | 无锡伊佩克科技有限公司 | Chromate-free passivant for tin-plated steel plate, and preparation method thereof |
-
2017
- 2017-09-19 CN CN201710843585.7A patent/CN107523818A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5468734A (en) * | 1977-11-11 | 1979-06-02 | Nippon Packaging Kk | Surface treatment of tin plated steel plate and can |
| CN101974745A (en) * | 2010-10-27 | 2011-02-16 | 大连三达奥克化学股份有限公司 | Normal temperature bonderite for renovating flow string and manufacture method |
| CN105951084A (en) * | 2016-06-27 | 2016-09-21 | 无锡伊佩克科技有限公司 | Ultralow-temperature metal passivation phosphorizing liquid and preparation method thereof |
| CN105951082A (en) * | 2016-06-27 | 2016-09-21 | 无锡伊佩克科技有限公司 | Chromate-free passivant for tin-plated steel plate, and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113881934A (en) * | 2021-11-04 | 2022-01-04 | 湖南金化科技集团有限公司 | Zinc-based phosphating solution with less slag and ash |
| CN113881934B (en) * | 2021-11-04 | 2023-04-21 | 湖南金化科技集团有限公司 | Zinc phosphating solution with less slag and ash |
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