CN101457355A - Organic promoting phosphating solution and preparation method and application thereof - Google Patents
Organic promoting phosphating solution and preparation method and application thereof Download PDFInfo
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- CN101457355A CN101457355A CNA2008102207896A CN200810220789A CN101457355A CN 101457355 A CN101457355 A CN 101457355A CN A2008102207896 A CNA2008102207896 A CN A2008102207896A CN 200810220789 A CN200810220789 A CN 200810220789A CN 101457355 A CN101457355 A CN 101457355A
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Abstract
一种有机促进磷化液及其制备方法和应用，所述的磷化液包括基础液和促进剂，所述的基础液与促进剂的重量比是1.5－2.5∶1；所述基础液是铁粉、磷酸、氧化锌、氢氟酸、碳酸盐、氟硅酸、水的混合物；所述促进剂是氟硼酸钠、酒石酸、氯酸钠、烧碱、硝基苯磺酸钠、水的混合物。该磷化液磷化工艺范围宽，可以在5－65℃范围内使用，适用于汽车、家电、家具和机械设备的涂装前处理，其生产及使用方法简单，符合环保要求。An organic accelerated phosphating solution and its preparation method and application, the phosphating solution includes a base liquid and an accelerator, the weight ratio of the base liquid to the accelerator is 1.5-2.5:1; the base liquid is Iron powder, phosphoric acid, zinc oxide, hydrofluoric acid, carbonate, fluosilicic acid, water mixture; the accelerator is sodium fluoborate, tartaric acid, sodium chlorate, caustic soda, sodium nitrobenzenesulfonate, water mixture. The phosphating solution has a wide range of phosphating process and can be used in the range of 5-65°C. It is suitable for the pre-painting treatment of automobiles, household appliances, furniture and mechanical equipment. Its production and use methods are simple and meet environmental protection requirements.
Description
Technical field
The present invention relates to a kind of phosphatization liquid, preparation method and application, relate in particular to a kind of no nickel wide temperature rang phosphating liquid, preparation method and application thereof.
Background technology
Metal generally need carry out pre-treatment in containing phosphatic solution before application, form the metal phosphate chemical conversion film, and this technological process is referred to as phosphatization.The main purpose of phosphatization is to provide the protection of short-term inter process to matrix metal before the application, prevents that to a certain extent metal is corroded, and improves the sticking power and the anti-corrosion capability of paint film layer.Along with the enhancing of people's environmental protection consciousness and the worsening shortages of the energy, novel Coating Pretreatment worker's technology develops towards low temperature, less energy-consumption, low pollution and hypotoxic direction.Though the phosphatization thickness that middle high temperature phosphorization liquid forms, corrosion-resistant, cost height, many, the complex process of slag, particularly energy consumption is big.And the use temperature of normal-temperature phosphorizing liquid is low, does not need the energy, long service life, and tank liquor is safeguarded simple, comprehensive cost is low.But different metal bases has different requirements to the temperature of phosphatization, and common same phosphatization liquid can not use at low temperature and middle high temperature range, and the operation of phosphating process has been brought restriction.And contain nickel salt in the present most widely used phosphatization liquid, and adopt nitrite as promotor, nitrite in the phosphatization working fluid is unstable in acidic solution, need add to the concentration of regulation during each production, the control indexes relative complex, will waste a large amount of shortization agent, the gas of generation also environmental pollution is more serious.
Chinese patent CN1401820 discloses a kind of normal-temperature phosphorizing liquid, form by following substances in percentage by weight, phosphoric acid 2.0-4.0%, zinc oxide 0.4-0.6%, zinc nitrate 0.5-1.5%, nickelous nitrate 3.0-5.0%, manganous nitrate 2.0-4.0%, boron fluoric acid sodium 0.2-1.0%, sodium chlorate 2.0-3.0%, citric acid 0.5-2.0%, surplus is a softening water.No matter this invention nickel salt is produced and also is to use this phosphatization liquid, and all being unfavorable for controlling the phosphatization fluidity can parameter index.
Summary of the invention
The technical problem to be solved in the present invention provides that a kind of not contain nitrite and nickel salt and operating procedure simple, easy to maintenance, organic promotive phosphating liquor that can (5-65 ℃) uses in different temperature ranges; Further the present invention also provides the preparation method and the application of this phosphatization liquid.
It is to realize by following technical scheme that the present invention will solve the problems of the technologies described above: a kind of organic promotive phosphating liquor, comprise basal liquid and promotor, and the weight ratio of described basal liquid and promotor is 1.5-2.5: 1; Described basal liquid is the mixture of iron powder, phosphoric acid, zinc oxide, hydrofluoric acid, carbonate, silicofluoric acid, water; Described promotor is the mixture of Sodium tetrafluoroborate, tartrate, sodium chlorate, caustic soda, nitrobenzene sodium sulfonate, water.
Further: in above-mentioned organic promotive phosphating liquor, the weight ratio of described basal liquid and promotor is 2: 1.Described basal liquid prescription is by weight percentage: iron powder 0.064%-0.25%, phosphoric acid 31.1%-40%, zinc oxide 12.7%-15.8%, hydrofluoric acid 0%-0.71%, carbonate 3.2-3.8%, silicofluoric acid 1.3-1.6%, surplus are water.Described promotor is that Sodium tetrafluoroborate 0.01%-0.05%, tartrate 0.5%-1%, sodium chlorate 3%-8%, caustic soda 0.1%-1.0%, nitrobenzene sodium sulfonate 1%-5%, surplus are water by weight percentage.
The present invention also provides the preparation method and the application of this organic promotive phosphating liquor.Among the described preparation method, comprise the preparation of basal liquid and promotor, described basal liquid preparation process is, with load weighted iron powder, phosphoric acid add in the reactor with after the water dissolution, substep adds zinc oxide, hydrofluoric acid, carbonate, silicofluoric acid, when a kind of speciality of every adding, equal dilute with waters and be stirred to material and dissolve fully or mix, at last the clear solution of gained is filtered basal liquid.Described promotor preparation process is, load weighted Sodium tetrafluoroborate, tartrate, sodium chlorate, caustic soda, m-nitrobenzene sodium sulfonate are joined in the reactor, adds water again and stirs and place after 1-2 hour, and restir is to dissolving fully.The described basal liquid percentage of filling a prescription is by weight counted: iron powder 0.064%-0.25%, phosphoric acid 31.1%-40%, zinc oxide 12.7%-15.8%, hydrofluoric acid 0%-0.71%, carbonate 3.2-3.8%, silicofluoric acid 1.3-1.6%, surplus are water.Described promotor percentage is by weight counted, and Sodium tetrafluoroborate 0.01%-0.05%, tartrate 0.5%-1%, sodium chlorate 3%-8%, caustic soda 0.1%-1.0%, nitrobenzene sodium sulfonate 1%-5%, surplus are water.
Accurately pipetting the 10.0ml basal liquid in triangular flask, add deionized water 50ml, add 1-2 and drip methyl orange indicator, is counting of free acid with 0.1000mol/LNaOH standard solution titration to the orange milliliter number that consumes the NaOH standardized solution; The total acidity of Fundamentals of Measurement liquid is not less than 800 points, and free acidity is not less than 145 points, and density is 1.5-1.6 gram/cm
3The density of directly measuring promotor is 1.3-1.4 gram/cm
3
Above-mentioned phosphatization liquid is used for the preceding pretreated application of coated metal.In this purposes, in the phosphatization groove earlier with basal liquid with water dissolution after, add again promotor and water stir working fluid, the weight ratio of described basal liquid and promotor is: 1.5-2.5: 1; With above-mentioned working fluid spray or immersion workpiece, water dries after cleaning again.The weight ratio of base of optimum selection liquid and promotor is: 2: 1, the time of described spray or immersion was 1-10 minute.The wide temperature rang phosphating liquid of organic shortization of the inventive method preparation can form careful uniform phosphatize phosphate coat at workpiece surface, can improve paint film adhesion and erosion resistance, is applicable to the Coating Pretreatment of automobile, household electrical appliances, furniture and mechanical means.
The present invention adopts iron powder, phosphoric acid, zinc oxide, hydrofluoric acid, manganous carbonate, silicofluoric acid and water to prepare the phosphatization basal liquid, adopt Sodium tetrafluoroborate, tartrate, sodium chlorate, caustic soda, m-nitrobenzene sodium sulfonate and water to prepare Phosphating Accelerant, be mixed with working fluid operation and maintenance management in different operating liquid scope with prepared basal liquid, promotor, soda ash solution and water then.The beneficial effect that the present invention is compared with prior art produced is as follows:
(1) phosphatization liquid does not use nickel salt and nitrite, helps environment protection;
(2) phosphating process wide ranges can be used in 5-65 ℃ of scope, can adopt spray and soaking technology;
(3) phosphatization liquid is safeguarded simply, does not need to measure the promotor index;
(4) use of saving material, promotor does not contain nitrite, does not have the waste of toxic gas generation and promotor.
Embodiment
Purport of the present invention is to improve the prescription of phosphatization liquid, and operating procedure is simple, and is easy to maintenance, and the technological temperature wide ranges can be used in 5-65 ℃ of scope.Workpiece is careful evenly through the phosphatize phosphate coat that bonderizing forms, and improves paint film adhesion and erosion resistance, is applicable to automobile, household electrical appliances, furniture and mechanical means Coating Pretreatment.Below in conjunction with embodiment content of the present invention is described in further detail, mentioned content is not a limitation of the invention in the embodiment, and the selection of parameter can be suited measures to local conditions and the result be there is no substantial effect among the preparation method.
At first sketch general planning of the present invention: a kind of organic promotive phosphating liquor, comprise basal liquid and promotor, the weight ratio of described basal liquid and promotor is 1.5-2.5: 1; Described basal liquid is the mixture of iron powder, phosphoric acid, zinc oxide, hydrofluoric acid, carbonate, silicofluoric acid, water; Described promotor is the mixture of Sodium tetrafluoroborate, tartrate, sodium chlorate, caustic soda, nitrobenzene sodium sulfonate, water.
Embodiment 1
(1) preparation of phosphatization liquid
The preparation of i, basal liquid
To dissolve in 0.9 gram iron powder, 10 gram water and the 30 gram phosphoric acid adding reactors, in reactor, add 200 gram zinc oxide again, add 120 gram water and stir 5 minutes to pasty state, slowly adding 600 gram phosphoric acid and 12 gram hydrofluoric acid again stirs and to be transparent to solution in 20 minutes, slowly add 60 gram manganous carbonates, stir and be transparent to solution in 10 minutes, add 500 gram water again, slowly adding 25 gram silicofluoric acid when solution temperature is cooled to 30 ℃, to be stirred to solution transparent and filter; The total acidity of Fundamentals of Measurement liquid is not less than 800 points, and free acidity is not less than 145 points, and density is 1.5-1.6 gram/cm
3
The preparation of ii, promotor
0.4 gram Sodium tetrafluoroborate, 6 gram tartrate, 70 gram sodium chlorate, 5 gram caustic soda, 15 gram m-nitrobenzene sodium sulfonates are joined in the reactor, add water again and be stirred to 1 liter of volume, placed 1 hour, restir dissolves fully, and the density of promotor is 1.3-1.4 gram/cm
3
(2) use of phosphatization liquid
The first step is the configuration of working fluid, in 1 liter of phosphatization groove, contain 2/3 volume water, add basal liquid component 40 grams, add soda ash (using water dissolution before using) 1.5 grams then and stir well dissolving, add promotor component 20 grams again, stirring and water is added to volume is 1 liter, chemical examination total acidity 18-22 point, free acidity is transferred to temperature in the 20-25 ℃ of scope at the 0.8-1.0 point;
Second step was the phosphatization of workpiece, and workpiece is cleaned, shows to transfer by oil removing, water, and spray is 2 minutes in the phosphatization working fluid of above-mentioned steps preparation, dries after water cleans;
The 3rd step be the maintenance of phosphatization liquid, controlled the total acidity of phosphatization liquid and free acidity in process of production in the scope of the first step requirement; When total acidity higher, thin up or allow it reduce naturally, every 1.0 points on the low side of total acidity add 2 kilograms of basal liquid components at every cubic metre of tank liquor, add 1 kilogram of promotor simultaneously; When higher 1.0 points of free acidity, in every cubic metre of tank liquor, add 0.6 kilogram of soda ash, free acidity is on the low side 1.0 points add 8 kilograms of basal liquid components at every cubic metre of tank liquor, add 4 kilograms of promotor simultaneously.
Embodiment 2
(1) preparation of phosphatization liquid
With embodiment 1;
(2) use of phosphatization liquid
The first step is the configuration of working fluid, in 1 liter of phosphatization groove, contain 2/3 volume water, add basal liquid component 60 grams, add soda ash (using water dissolution before using) 2.5 grams then and stir well dissolving, add promotor component 30 grams again, stirring and water is added to volume is 1 liter, chemical examination total acidity 32-36 point, free acidity is transferred to temperature in the 10-20 ℃ of scope at the 1.6-2.0 point;
Second step was the phosphatization of workpiece, and workpiece is cleaned, neutralizes, shows to transfer by oil removing, rust cleaning, water, soaked 10 minutes in the phosphatization working fluid of above-mentioned steps preparation, dried after the water cleaning;
The 3rd step is with embodiment 1.
Embodiment 3
(1) preparation of phosphatization liquid
The preparation of i, basal liquid
To dissolve in 1.2 gram iron powders, 10 gram water and the 30 gram phosphoric acid adding reactors, in reactor, add 150 gram zinc oxide again, add 130 gram water and stir 5 minutes to pasty state, slowly adding 550 gram phosphoric acid and 14 gram hydrofluoric acid again stirs and to be transparent to solution in 20 minutes, slowly add 50 gram manganous carbonates, stir and be transparent to solution in 10 minutes, add 400 gram water again, slowly adding 20 gram silicofluoric acid when solution temperature is cooled to 30 ℃, to be stirred to solution transparent and filter; The total acidity of Fundamentals of Measurement liquid is not less than 800 points, and free acidity is not less than 145 points, and density is 1.5-1.6 gram/cm
3
The preparation of ii, promotor
6 gram Sodium tetrafluoroborates, 4 gram tartrate, 60 gram sodium chlorate, 7 gram caustic soda, 18 gram m-nitrobenzene sodium sulfonates are joined in the reactor, add water again and be stirred to 1 liter of volume, placed 1 hour, restir dissolves fully, and the density of promotor is 1.3-1.4 gram/cm
3
(2) use of phosphatization liquid
The first step is the configuration of working fluid, in 1 liter of phosphatization groove, contain 2/3 volume water, add basal liquid component 24 grams, add soda ash (using water dissolution before using) 1 gram then and stir well dissolving, add promotor component 12 grams again, stirring and water is added to volume is 1 liter, chemical examination total acidity 11-15 point, free acidity is transferred to temperature in the 40-50 ℃ of scope at the 0.6-0.8 point;
Second step was the phosphatization of workpiece, and workpiece is cleaned, shows to transfer by oil removing, water, and spray is 2 minutes in the phosphatization working fluid of above-mentioned steps preparation, dries after water cleans;
The 3rd step is with embodiment 1.
Embodiment 4
(1) preparation of phosphatization liquid
With embodiment 3;
(2) use of phosphatization liquid
The first step is the configuration of working fluid, in 1 liter of phosphatization groove, contain 2/3 volume water, add basal liquid component 50 grams, add soda ash (using water dissolution before using) 0.3 gram then and stir well dissolving, add promotor component 25 grams again, stirring and water is added to volume is 1 liter, chemical examination total acidity 25-30 point, free acidity is transferred to temperature in the 50-60 ℃ of scope at the 3-5 point;
Second step was the phosphatization of workpiece, and workpiece is cleaned, shows to transfer by oil removing, water, and spray is 1.5 minutes in the phosphatization working fluid of above-mentioned steps preparation, dries after water cleans;
The 3rd step is with embodiment 1.
Embodiment 5
(1) preparation of phosphatization liquid
With embodiment 3;
(2) use of phosphatization liquid
The first step is the configuration of working fluid, in 1 liter of phosphatization groove, contain 2/3 volume water, add basal liquid component 50 grams, add soda ash (using water dissolution before using) 1.5 grams then and stir well dissolving, add promotor component 25 grams again, stirring and water is added to volume is 1 liter, chemical examination total acidity 28-34 point, free acidity is transferred to temperature in the 30-40 ℃ of scope at the 1.6-2.0 point;
Workpiece is cleaned, neutralizes, shows to transfer by oil removing, rust cleaning, water, in the phosphatization working fluid of above-mentioned steps preparation, soaked 5 minutes, after the water cleaning, dry;
The 3rd step is with embodiment 1.
Claims (7)
1, a kind of organic promotive phosphating liquor comprises basal liquid and promotor, it is characterized in that:
The weight ratio of described basal liquid and promotor is 1.5-2.5:1;
Described basal liquid is the mixture of iron powder, phosphoric acid, zinc oxide, hydrofluoric acid, carbonate, silicofluoric acid, water;
Described promotor is the mixture of Sodium tetrafluoroborate, tartrate, sodium chlorate, caustic soda, nitrobenzene sodium sulfonate, water.
2, organic promotive phosphating liquor according to claim 1 is characterized in that: the weight ratio of described basal liquid and promotor is 2:1.
3, organic promotive phosphating liquor according to claim 2 is characterized in that:
Described basal liquid by weight percentage, iron powder 0.064-0.25%, phosphoric acid 31.1-40%, zinc oxide 12.7-15.8%, hydrofluoric acid 0-0.71%, carbonate 3.2-3.8%, silicofluoric acid 1.3-1.6%, surplus are water;
Described promotor by weight percentage, Sodium tetrafluoroborate 0.01-0.05%, tartrate 0.5-1%, sodium chlorate 3-8%, caustic soda 0.1-1.0%, nitrobenzene sodium sulfonate 1-5%, surplus are water.
4, a kind of method for preparing each described organic promotive phosphating liquor among the claim 1-3, comprise the preparation of basal liquid and promotor, it is characterized in that: described basal liquid preparation process is, with load weighted iron powder, phosphoric acid add in the reactor with after the water dissolution, substep adds zinc oxide, hydrofluoric acid, carbonate, silicofluoric acid, whenever add a kind of material, equal dilute with waters and be stirred to substance dissolves or mix, at last the clear solution of gained is filtered basal liquid;
Described promotor preparation process is, load weighted Sodium tetrafluoroborate, tartrate, sodium chlorate, caustic soda, m-nitrobenzene sodium sulfonate are joined in the reactor, adds water and is stirred to and mixes, place 1-2 hour again after, be stirred to dissolving fully at last.
5, each described organic promotive phosphating liquor is used for the preceding pretreated application of coating metal surfaces among a kind of claim 1-3.
6, organic promotive phosphating liquor purposes according to claim 5 is characterized in that:
In the phosphatization groove earlier with basal liquid with water dissolution after, add again promotor and water stir working fluid, the weight ratio of described basal liquid and promotor is 1.5-2.5:1;
With above-mentioned working fluid spray or immersion metalwork, water dries after cleaning again.
7, organic promotive phosphating liquor purposes according to claim 6 is characterized in that, the weight ratio of described basal liquid and promotor is 2:1, and the time of described spray or immersion is 1-10 minute.
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Cited By (8)
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| CN101838804A (en) * | 2010-05-10 | 2010-09-22 | 长沙祁胜新材料科技有限公司 | Laminated phosphating liquid and preparation method thereof |
| CN102304709A (en) * | 2011-04-25 | 2012-01-04 | 大连三达奥克化学股份有限公司 | Black phosphating agent for automotive special tools and preparation method thereof |
| CN102321883A (en) * | 2011-09-29 | 2012-01-18 | 石敏 | Normal-temperature phosphating solution |
| CN102899650A (en) * | 2012-10-23 | 2013-01-30 | 自贡勃生表面技术推广有限公司 | Steel normal-temperature blackening solution composite film-forming accelerator, steel normal-temperature blackening solution and preparation method of steel normal-temperature blackening solution |
| CN105256296A (en) * | 2015-11-12 | 2016-01-20 | 山东大学 | Normal/low-temperature chemical conversion solution for 35CrMnSi steel and preparing method thereof |
| CN105431568A (en) * | 2013-03-06 | 2016-03-23 | 奎克化学公司 | High temperature conversion coating on ferriferous substrates |
| CN106148931A (en) * | 2015-04-01 | 2016-11-23 | 四川亨通兴达科技有限公司 | A kind of shiny black type dicoration bonderite and preparation method thereof |
| CN108149234A (en) * | 2017-11-24 | 2018-06-12 | 安徽江南泵阀有限公司 | A kind of pump housing fastener surface parkerizing method |
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- 2008-12-29 CN CN2008102207896A patent/CN101457355B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838804A (en) * | 2010-05-10 | 2010-09-22 | 长沙祁胜新材料科技有限公司 | Laminated phosphating liquid and preparation method thereof |
| CN101838804B (en) * | 2010-05-10 | 2013-06-19 | 长沙祁胜新材料科技有限公司 | Laminated phosphating liquid and preparation method thereof |
| CN102304709A (en) * | 2011-04-25 | 2012-01-04 | 大连三达奥克化学股份有限公司 | Black phosphating agent for automotive special tools and preparation method thereof |
| CN102304709B (en) * | 2011-04-25 | 2013-10-30 | 大连三达奥克化学股份有限公司 | Black phosphating agent for automotive special tools and preparation method thereof |
| CN102321883A (en) * | 2011-09-29 | 2012-01-18 | 石敏 | Normal-temperature phosphating solution |
| CN102899650A (en) * | 2012-10-23 | 2013-01-30 | 自贡勃生表面技术推广有限公司 | Steel normal-temperature blackening solution composite film-forming accelerator, steel normal-temperature blackening solution and preparation method of steel normal-temperature blackening solution |
| CN105431568A (en) * | 2013-03-06 | 2016-03-23 | 奎克化学公司 | High temperature conversion coating on ferriferous substrates |
| US9926628B2 (en) | 2013-03-06 | 2018-03-27 | Quaker Chemical Corporation | High temperature conversion coating on steel and iron substrates |
| CN106148931A (en) * | 2015-04-01 | 2016-11-23 | 四川亨通兴达科技有限公司 | A kind of shiny black type dicoration bonderite and preparation method thereof |
| CN105256296A (en) * | 2015-11-12 | 2016-01-20 | 山东大学 | Normal/low-temperature chemical conversion solution for 35CrMnSi steel and preparing method thereof |
| CN105256296B (en) * | 2015-11-12 | 2017-12-05 | 山东大学 | A kind of 35CrMnSi steel normal cryochemistry conversion fluid and preparation method thereof |
| CN108149234A (en) * | 2017-11-24 | 2018-06-12 | 安徽江南泵阀有限公司 | A kind of pump housing fastener surface parkerizing method |
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