CN106906460A - A kind of fast bonderizing liquor and preparation method thereof - Google Patents

A kind of fast bonderizing liquor and preparation method thereof Download PDF

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Publication number
CN106906460A
CN106906460A CN201610234164.XA CN201610234164A CN106906460A CN 106906460 A CN106906460 A CN 106906460A CN 201610234164 A CN201610234164 A CN 201610234164A CN 106906460 A CN106906460 A CN 106906460A
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China
Prior art keywords
reactor
water
phosphating
added
citric acid
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CN201610234164.XA
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Chinese (zh)
Inventor
邹明瑞
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Foshan Ruijian Sports Equipment Co Ltd
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Foshan Ruijian Sports Equipment Co Ltd
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Priority to CN201610234164.XA priority Critical patent/CN106906460A/en
Publication of CN106906460A publication Critical patent/CN106906460A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/07Chemical 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

Abstract

The invention provides a kind of fast bonderizing liquor and preparation method thereof, by percentage to the quality, fast bonderizing liquor is made up of following raw material:Phosphatase 11 5 20%, zinc oxide 6 10%, zinc nitrate 20 25%, m-nitrobenzene sodium sulfonate 1 5%, citric acid 0.5 2%, ethylenediamine tetra-acetic acid(EDTA)1 4%, balance of water.The phosphating coat cupric sulphate dropping test time of Phosphating Solution of the present invention was up to 30 seconds, the neutral salt spray test time was up to 4 hours, paint film adhesion is up to 0 grade, phosphating time is short simultaneously, substantially increases operating efficiency, and temperature in use is low, and phosphating dregs are not produced substantially, cleaning cycle is substantially prolongs, fixed-end forces expense is reduced, without consuming the energy.

Description

A kind of fast bonderizing liquor and preparation method thereof
Technical field
The present invention relates to Phosphating Solution technical field, in particular, it is related to a kind of fast bonderizing liquor and preparation method thereof.
Background technology
With developing rapidly for metal-processing industry, phosphating process is especially painted in Treatment of Metal Surface(Or spray painting)Before The application of the aspects such as treatment is increasingly extensive.Presently used Phosphating Solution is generally medium and high temperature Phosphating Solution(55 DEG C -95 DEG C of temperature in use), Phosphating coat obtained in this kind of Phosphating Solution, thick with crystallizing, film layer is thicker, and phosphating time is long, and phosphating equipment investment is big, energy consumption The high, unfavorable factor such as acid mist is big, stability of solution is poor, sediment is more, adjustment is cumbersome, environmental protection pressure is big.
Chinese patent CN102605364 discloses a kind of middle overcast slag low emission phosphorization of thick film liquid of temperature and its method for bonderizing, The component of the Phosphating Solution is:Mazhev salt 3~5%, zinc nitrate 9~12%, manganese nitrate 3~5%, ammonium molybdate 0~ 0.01%, sodium chlorate 0~0.02%, citric acid 0.01~0.03%, ethylenediamine tetra-acetic acid 0.01~0.03%, surplus It is water, by weight.Although the patent Phosphating Solution produces few sediment in use, its free acidity is extremely low, The shortcomings of film is difficult, and phosphating time is long is caused in phosphatization.
The content of the invention
An object of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of fast bonderizing liquor, this Phosphating Solution phosphorus The change time is short, substantially increases operating efficiency, and temperature in use is low, reduces energy consumption, and without processing sediment.
The second object of the present invention is the preparation method for providing above-mentioned fast bonderizing liquor.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of fast bonderizing liquor, by percentage to the quality, is made up of following raw material:
Phosphatase 11 5-20%, zinc oxide 6-10%, zinc nitrate 20-25%, m-nitrobenzene sodium sulfonate 1-5%, citric acid 0.5-2%, second two Amine tetraacethyl(EDTA)1-4%, balance of water.
Currently preferred technical scheme is:A kind of fast bonderizing liquor, by percentage to the quality, is made up of following raw material:
Phosphatase 11 5-18%, zinc oxide 7-9%, zinc nitrate 20-22%, m-nitrobenzene sodium sulfonate 1-2%, citric acid 0.5-1%, ethylenediamine Tetraacethyl(EDTA)1-2%, balance of water.
Technical scheme of the invention preferred is:
Phosphatase 11 5%, zinc oxide 9%, zinc nitrate 22%, m-nitrobenzene sodium sulfonate 1%, citric acid 1%, ethylenediamine tetra-acetic acid(EDTA) 1%, water 51%.
A kind of fast bonderizing liquor, by percentage to the quality, is made up of following raw material:
The preparation method of fast bonderizing liquor of the present invention in turn includes the following steps:
(1)Phosphoric acid is added in a kettle., is opened reactor and is stirred;
(2)The water of the total consumption 40%-60% of water needed for being added toward reactor;
(3)Zinc oxide is added toward reactor;
(4)Reaction is completely and after solution clarification toward adding remaining water in reactor;
(5)Zinc nitrate is added toward reactor, stirs and make solution to clarify;
(6)M-nitrobenzene sodium sulfonate is added toward reactor, stirs and make solution to clarify;
(7)Finally toward addition citric acid, EDTA in reactor, stir and solution clarification.
Main operational principle of the invention is as follows:
Steel and iron parts immerse Phosphating Solution(By Zn (H2PO42The acid dilute aqueous solution of composition, pH value is 1-3)In, the generation of phosphating coat Reaction is as follows:
3Zn(H2PO42 =Zn3(PO42↓+4H3PO4
Iron and steel parts are steel and alloy, under phosphatizing, Fe and FeC3Countless galvanic cells are formed, in anode region, iron starts molten It is Fe to solve2+, while ejected electron.
Fe+2H3PO4 =Fe (H2PO42+H2
Fe =Fe2+ +2e-
Fe in solution near surface of steel workpiece2+It is continuously increased, works as Fe2+With HPO4 2-, PO4 3-Concentration is more than phosphatic During solubility product, precipitation is produced, phosphating coat is formed in workpiece surface:
Fe(H2PO42= FeHPO4↓+ H3PO4
Fe+ Fe(H2PO42= 2FeHPO4↓+ H2
3FeHPO4= Fe3(PO42↓+ H3PO4
Fe+ 2FeHPO4 =Fe3(PO42↓+H2
Cathodic region releases substantial amounts of hydrogen:
2H+ +2e- =H2
O2 + 2H20 + 4e- =4OH-
Net reaction:
3Zn(H2PO42= Zn3(PO42↓+4H3PO4
2Fe+3Zn(H2PO42= Zn3(PO42↓+2FeHPO4↓+2H3PO4+ 2H2
Wherein Zn3(PO42、FeHPO4It is the composition of phosphating coat;Formula intermediate nitro benzene sulfonic acid sodium salt adds accelerator in, and additional Accelerator should just use when with groove, and accelerator can shorten the time of phosphating coat formation;Citric acid plays refinement phosphatization in formula Crystallization, the effect for reducing thickness.Ethylenediamine tetra-acetic acid is complexing agent in formula, reduces slagging scorification amount during phosphorating treatment.
The application method of Phosphating Solution of the present invention is(To prepare lm3As a example by):The water of 1/2 volume, plus 50-100 are contained in groove Kilogram Phosphating Solution, adds water to cumulative volume lm3(3-6 kilograms of Phosphating Solution added promoter is just added using preceding)Stir, survey Examination total acidity is between 18-30pt and free acidity 0.6-1.5pt between.
Bath maintenance:In processing procedure, total acidity is less than at 18 points to workpiece, and free acidity should add one when being less than at 0.6 Quantitative Phosphating Solution, per m340kg General Acidity in Phosphating Solution is added to improve 2 points or so in tank liquor, free acidity improves 0.2 point or so, Pay special attention to, added promoter is decomposed reaction in use, according to the situation of phosphating coat, should be continuously added dropwise additional Accelerator, it is ensured that tank liquor is steady in a long-term.
The phosphating coat cupric sulphate dropping test time of Phosphating Solution of the present invention up to 30 seconds, the neutral salt spray test time up to 4 hours, Paint film adhesion meets country and professional standard up to 0 grade;Phosphating time of the present invention is short simultaneously, substantially increases operating efficiency, makes It is low with temperature.And phosphating dregs are not produced substantially, cleaning cycle is substantially prolongs, and fixed-end forces expense are reduced, without disappearing Power consumption source.
Specific embodiment
Embodiment 1
Per 1000Kg ordinary-temp fast bonderizing liquors, it is made up of following raw material:
Phosphatase 11 50Kg, the Kg of zinc oxide 90, the Kg of zinc nitrate 220, the Kg of m-nitrobenzene sodium sulfonate 10, citric acid 10 Kg, EDTA10 Kg, the Kg of water 510.
Its preparation method in turn includes the following steps:
(1)Phosphoric acid is added in a kettle., is opened reactor and is stirred;
(2)The water of the total consumption 50% of water needed for being added toward reactor;
(3)Zinc oxide is added toward reactor, question response is completely and solution is clarified(4 hours or so);
(4)Remaining water is added toward reactor;
(5)Zinc nitrate, uniform and solution clarification to be mixed are added toward reactor(2 hours or so);
(6)M-nitrobenzene sodium sulfonate, uniform and solution clarification to be mixed are added toward reactor(1 hour or so);
(7)Citric acid, uniform and solution clarification to be mixed are added toward reactor(1 hour or so);
(8)Product is carried out into physical and chemical index detection, packaging and storage.
Embodiment 2
Per 1000Kg ordinary-temp fast bonderizing liquors, it is made up of following raw material:
Phosphatase 11 80Kg, zinc oxide 70Kg, zinc nitrate 200Kg, m-nitrobenzene sodium sulfonate 15Kg, citric acid 5Kg, EDTA20 Kg, Water 510Kg.
Preparation method is with embodiment 1.
Embodiment 3
Per 1000Kg ordinary-temp fast bonderizing liquors, it is made up of following raw material:
Phosphatase 11 70Kg, the Kg of zinc oxide 80, the Kg of zinc nitrate 210, the Kg of m-nitrobenzene sodium sulfonate 20, the Kg of citric acid 10, EDTA10 Kg, the Kg of water 500.
Preparation method is with embodiment 1.
Embodiment 4
Per 1000Kg ordinary-temp fast bonderizing liquors, it is made up of following raw material:
Phosphatase 11 60Kg, the Kg of zinc oxide 70, the Kg of zinc nitrate 200, the Kg of m-nitrobenzene sodium sulfonate 10, citric acid 5 Kg, EDTA20 Kg, the Kg of water 535.
Preparation method is with embodiment 1.
Embodiment 5
Per 1000Kg ordinary-temp fast bonderizing liquors, it is made up of following raw material:
The Kg of phosphatase 11 70, the Kg of zinc oxide 90, the Kg of zinc nitrate 210, the Kg of m-nitrobenzene sodium sulfonate 20, the Kg of citric acid 10, EDTA10 Kg, the Kg of water 490.
Preparation method is with embodiment 1.
Embodiment 6
Per 1000Kg ordinary-temp fast bonderizing liquors, it is made up of following raw material:
Phosphatase 11 00Kg, the Kg of zinc oxide 100, the Kg of zinc nitrate 250, the Kg of m-nitrobenzene sodium sulfonate 10, the Kg of citric acid 20, EDTA30 Kg, the Kg of water 490.
Preparation method is with embodiment 1.
Embodiment 7
Per 1000Kg ordinary-temp fast bonderizing liquors, it is made up of following raw material:
Phosphoric acid 200Kg, the Kg of zinc oxide 60, the Kg of zinc nitrate 200, the Kg of m-nitrobenzene sodium sulfonate 50, citric acid 5 Kg, EDTA20 Kg, the Kg of water 465.
Preparation method is with embodiment 1.
The Phosphating Solution application method of embodiment of the present invention 1-7 is as follows:(To prepare lm3As a example by)1/2 volume is contained in groove Water, plus 50 kilograms of Phosphating Solutions add water to cumulative volume lm3(It is additional using preceding 6 kilograms of just addition Phosphating Solution added promoter Promotion agent prescription is 40% natrium nitrosum, 60% water(Mass fraction))Stir, total acidity is between 18-30pt and swims for test Between acidity 0.6-1.5pt.
The formula of embodiment of the present invention 1-7 is shown in Table 1(Calculated with 1000Kg Phosphating Solutions).
The formula of the embodiment 1-7 of table 1
The using effect of embodiment of the present invention 1-7 is shown in Table 2, table 3.
The using effect of the embodiment 1-7 of table 2
Phosphating Solution phosphating time of the present invention is short as can be seen from Table 2, substantially increases operating efficiency, and temperature in use is low.And base This does not produce phosphating dregs, substantially prolongs cleaning cycle, fixed-end forces expense is reduced, without consuming the energy.Embodiment 1 Effect is best.
Above content describes general principle of the invention and principal character, and the present invention is not limited to the above embodiments, Merely illustrating the principles of the invention described in above-described embodiment and specification, is not departing from the premise of spirit and scope of the invention Under, various changes and modifications of the present invention are possible, and these changes and improvements all fall within the protetion scope of the claimed invention.This hair Bright claimed scope is by appending claims and its equivalent thereof.

Claims (5)

1. a kind of fast bonderizing liquor, it is characterised in that by percentage to the quality, be made up of following raw material:
Phosphatase 11 5-20%, zinc oxide 6-10%, zinc nitrate 20-25%, m-nitrobenzene sodium sulfonate 1-5%, citric acid 0.5-2%, second two Amine tetraacethyl(EDTA)1-4%, balance of water.
2. fast bonderizing liquor according to claim 1, it is characterised in that by percentage to the quality, be made up of following raw material:
Phosphatase 11 5-18%, zinc oxide 7-9%, zinc nitrate 20-22%, m-nitrobenzene sodium sulfonate 1-2%, citric acid 0.5-1%, ethylenediamine Tetraacethyl(EDTA)1-2%, balance of water.
3. fast bonderizing liquor according to claim 1, it is characterised in that by percentage to the quality, be made up of following raw material:
Phosphatase 11 5%, zinc oxide 9%, zinc nitrate 22%, m-nitrobenzene sodium sulfonate 1%, citric acid 1%, EDTA1%, water 51%.
4. the preparation method of fast bonderizing liquor according to claim 1, it is characterised in that in turn include the following steps:
(1)Phosphoric acid is added in a kettle., is opened reactor and is stirred;
(2)The water of the total consumption 40%-60% of water needed for being added toward reactor;
(3)Zinc oxide is added toward reactor;
(4)Reaction is completely and after solution clarification toward adding remaining water in reactor;
(5)Zinc nitrate is added toward reactor, stirs and make solution to clarify;
(6)M-nitrobenzene sodium sulfonate is added toward reactor, stirs and make solution to clarify;
(7)Finally toward addition citric acid, EDTA in reactor, stir and solution clarification.
5. the preparation method of fast bonderizing liquor according to claim 3, it is characterised in that in turn include the following steps:
(1)Phosphoric acid is added in a kettle., is opened reactor and is stirred;
(2)The water of the total consumption 50% of water needed for being added toward reactor;
(3)Zinc oxide is added toward reactor, is reacted after 4 hours completely and solution is clarified;
(4)Remaining water is added toward reactor;
(5)Zinc nitrate is added toward reactor, is stirred, solution clarification;
(6)M-nitrobenzene sodium sulfonate is added toward reactor, is stirred, solution clarification;
(7)Citric acid is added toward reactor, is stirred, solution clarification after 1 hour;
(8)Product is carried out into physical and chemical index detection, packaging and storage.
CN201610234164.XA 2016-04-17 2016-04-17 A kind of fast bonderizing liquor and preparation method thereof Pending CN106906460A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108220938A (en) * 2018-01-17 2018-06-29 安徽工业大学 A kind of low slag phosphating solution of ultra-thin membranous type room temperature and its synthetic method
CN113215557A (en) * 2021-04-13 2021-08-06 东莞市颖兴金属表面处理材料有限公司 Phosphating solution capable of automatically precipitating ferrous ions and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103668149A (en) * 2013-12-19 2014-03-26 湖南金裕化工有限公司 Normal-temperature rapid phosphating solution and preparing method thereof
CN103695881A (en) * 2013-12-19 2014-04-02 湖南金裕化工有限公司 Normal-temperature sludgeless fast phosphating liquid and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103668149A (en) * 2013-12-19 2014-03-26 湖南金裕化工有限公司 Normal-temperature rapid phosphating solution and preparing method thereof
CN103695881A (en) * 2013-12-19 2014-04-02 湖南金裕化工有限公司 Normal-temperature sludgeless fast phosphating liquid and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108220938A (en) * 2018-01-17 2018-06-29 安徽工业大学 A kind of low slag phosphating solution of ultra-thin membranous type room temperature and its synthetic method
CN113215557A (en) * 2021-04-13 2021-08-06 东莞市颖兴金属表面处理材料有限公司 Phosphating solution capable of automatically precipitating ferrous ions and preparation method thereof

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Application publication date: 20170630