CN104630867A - High-efficiency electrolytic phosphating solution - Google Patents
High-efficiency electrolytic phosphating solution Download PDFInfo
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- CN104630867A CN104630867A CN201510085709.0A CN201510085709A CN104630867A CN 104630867 A CN104630867 A CN 104630867A CN 201510085709 A CN201510085709 A CN 201510085709A CN 104630867 A CN104630867 A CN 104630867A
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- acid
- additive
- deionized water
- phosphating solution
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/36—Phosphatising
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- Engineering & Computer Science (AREA)
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- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention relates to a high-efficiency electrolytic phosphating solution which is composed of 100-150 g/L phosphoric acid, 71-75 g/L zinc oxide, 60-80 g/L nitric acid, 180-220 g/L calcium carbonate, 8-40 g/L additive and the balance of deionized water. The additive is citric acid or tartaric acid or sodium nitrate or nickel nitrate or copper sulfate or fluosilicic acid, or a mixture of any combination. The preparation method comprises the following steps: injecting the deionized water into a container, adding the phosphoric acid and nitric acid, heating while stirring, slowly adding the zinc oxide while stirring when the temperature reaches 80 DEG C, and stopping heating when the zinc oxide is completely dissolved; continuing stirring for half an hour, adding the calcium carbonate, and continuing stirring for half an hour; and cooling the obtained solution to room temperature, adding the additive, continuing stirring until the additive is completely dissolved, and adding the deionized water to the specified volume, thereby obtaining the electrolytic phosphating solution. The phosphating solution has the characteristic of no toxicity, can be used at normal temperature, and avoids physical damage to the operators and the waste of resources.
Description
Technical field
The present invention relates to metal cold processing pretreating reagent, specifically a kind of electrolytic phosphating liquid forming the protective membrane with raising solidity to corrosion and processibility on metal material surface.
Background technology
In metal cold plasticity deformation process, causing the damage of mould in order to avoid directly contacting between processing mold with machined material, often surface treatment being carried out to machined material.In current tradition, high temperature phosphorization process has been a kind of technology of comparative maturity in the cold plasticity processing treatment of ferrous materials, and in order to meet the requirement of resources conservation and environmental protection, phosphorization technology develops to low temperature phosphor aspect, but low temperature phosphor process at present all needs the longer reaction times, and all need to add nitrite or the promotor such as oxymuriate and Organic nitro class oxyammonia compounds, these promotor are not only expensive, and can toxic substance be decomposed in chemical reaction process when bonderizing, very large to operator's actual bodily harm.
Summary of the invention
The object of the present invention is to provide a kind of efficient electrolysis Phosphating Solution, nontoxic by this efficient electrolysis Phosphating Solution, and can use at normal temperatures, carry out drying again after the method attachment of this efficient electrolysis Phosphating Solution by electrolytic phosphating and just can form phosphating protective film.
To achieve these goals, a kind of efficient electrolysis Phosphating Solution provided by the invention, its raw material consists of: phosphatase 11 00-150g/l, zinc oxide 71-75g/l, nitric acid 60-80g/l, calcium carbonate 180 ~ 220g/l, additive 8-40 g/l, and surplus is deionized water; Described additive is citric acid or tartrate or SODIUMNITRATE or nickelous nitrate or copper sulfate or silicofluoric acid, or the mixture of their arbitrary combination.
Present invention also offers the preparation method of above-mentioned efficient electrolysis Phosphating Solution, comprise the following steps: the deionized water 1) being first injected to the electrolytic phosphating liquid cumulative volume 1/5-1/4 of required preparation in a container, add phosphoric acid and nitric acid again, heat while stirring, when temperature arrives 80 DEG C, slowly add zinc oxide while stirring, after zinc to be oxidized dissolves completely, stop heating; 2) add calcium carbonate again after continuing to stir half an hour, then continue to stir half an hour; 3) above-mentioned 2) step complete after after the solution of acquisition is down to room temperature, add additive, and continue to be stirred to and dissolve completely, and then add deionized water constant volume, namely obtain electrolytic phosphating liquid.
Efficient electrolysis Phosphating Solution provided by the invention contains one or more additives, and it has following beneficial effect:
1), in formula without the heavy metal ion of environmental pollution, be a kind of environment-friendly type metal surface finishing agent.
2), this electrolytic phosphating liquid adopts cathodic deposition in the use processed metal, because anode uses the noble electrode not participating in reacting, whole process does not have metallic matrix to participate in reaction, therefore belong to without sediment shaped metal process of surface treatment, without the need to falling groove, reduce waste of human resource phenomenon.
3), this electrolytic phosphating liquid just can carry out at normal temperatures in the use processed metal, and the treatment time is all shorter than common high, medium and low temperature phosphatization, can increase production line speed to a certain extent.
4), after this electrolytic phosphating liquid carries out electrolytic phosphating process to metal, metallic surface due to overlay film even, the corrosion resistance of metal is significantly increased.
5), after this electrolytic phosphating liquid carries out electrolytic phosphating process to metal, the rete dense uniform of acquisition, Film color is that grey arrives light/dark balance, and polarized current density is less.
The present invention fills a prescription simple, easy to prepare, in use, on the basis not increasing the electrolytic phosphating time, can obtain compactness very good, and the very strong and uniform phosphatize phosphate coat of sticking power is a kind of well metal conditioner.The maximum feature of the present invention is exactly that Phosphating Solution is nontoxic and can carry out at normal temperatures, avoids operator's actual bodily harm and the wasting of resources in production application.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
General description is carried out to the material used in the present invention's experiment and preparation method in this part.Although for realizing many materials that the object of the invention uses and working method is well known in the art, the present invention describes in detail as far as possible at this.It will be apparent to those skilled in the art that hereinafter, if not specified, material therefor of the present invention, equipment and working method are well known in the art.
Embodiment 1
Efficient electrolysis Phosphating Solution, its raw material consists of:
Phosphoric acid (85%) 120g/l
Zinc oxide (99%) 73g/l
Nitric acid (68%) 70g/l
Calcium carbonate 200g/l
Citric acid 20g/l
Tartrate 4g/l
SODIUMNITRATE 4g/l
Nickelous nitrate 4g/l
Silicofluoric acid 4g/l
Copper sulfate 2g/l
Oxalic acid 2g/l
Deionized water surplus
Wherein, citric acid, tartrate, SODIUMNITRATE, nickelous nitrate, silicofluoric acid, copper sulfate, oxalic acid are additive.
Above-mentioned efficient electrolysis Phosphating Solution is prepared by following steps:
1) in a container, the deionized water of the electrolytic phosphating liquid cumulative volume 1/5-1/4 of required preparation, is first injected to (such as, the electrolytic phosphating liquid cumulative volume of required preparation is 1 liter, the deionized water first injected is then 0.2-0.25 liter, by that analogy), add phosphoric acid and nitric acid again, heat while stirring, when temperature arrives 80 DEG C, slowly add zinc oxide while stirring, after zinc to be oxidized dissolves completely, stop heating;
2), continue to stir after half an hour and add calcium carbonate again, then continue to stir half an hour;
3), above-mentioned 2) step complete after after the solution of acquisition is down to room temperature, add additive, and continue to be stirred to and dissolve completely, and then add deionized water constant volume, namely obtain electrolytic phosphating liquid.
Embodiment 2
Efficient electrolysis Phosphating Solution, its raw material consists of:
Phosphoric acid (85%) 130g/l
Zinc oxide (99%) 70g/l
Nitric acid (68%) 75g/l
Calcium carbonate 190g/l
Citric acid 18g/l
Tartrate 3g/l
SODIUMNITRATE 3g/l
Nickelous nitrate 3g/l
Silicofluoric acid 3g/l
Copper sulfate 2g/l
Oxalic acid 2g/l
Deionized water surplus
Wherein, citric acid, tartrate, SODIUMNITRATE, nickelous nitrate, silicofluoric acid, copper sulfate, oxalic acid are additive.
The preparation process of above-mentioned efficient electrolysis Phosphating Solution is identical with embodiment 1.
Embodiment 3
Efficient electrolysis Phosphating Solution, its raw material consists of:
Phosphoric acid (85%) 140g/l
Zinc oxide (99%) 68g/l
Nitric acid (68%) 65g/l
Calcium carbonate 210g/l
Citric acid 6g/l
Copper sulfate 2g/l
Oxalic acid 2g/l
Deionized water surplus
Wherein, citric acid, copper sulfate, oxalic acid are additive.
The preparation process of above-mentioned efficient electrolysis Phosphating Solution is identical with embodiment 1.
Efficient electrolysis Phosphating Solution of the present invention and existing Phosphating Solution bonderizing simultaneous test:
The ratio weight average of the electrolytic phosphating liquid obtained in the various embodiments described above is at 1.2 ~ 1.4kg/l.In addition, adopt the invention provides to electrolytic phosphating liquid process metal time, electrolytic phosphating under normal temperature can be realized by following steps: acid pickling and rust removing, first time washing, second time washing, electrochemical treatment, wash for the third time, dry up solidification.
Be to be understood that example as herein described and embodiment only in order to illustrate, those skilled in the art can make various amendment or change according to it, all belong to protection scope of the present invention.
Claims (2)
1. an efficient electrolysis Phosphating Solution, its raw material consists of: phosphatase 11 00-150g/l, zinc oxide 71-75g/l, nitric acid 60-80g/l, calcium carbonate 180 ~ 220g/l, additive 8-40 g/l, and surplus is deionized water; Described additive is citric acid or tartrate or SODIUMNITRATE or nickelous nitrate or copper sulfate or silicofluoric acid, or the mixture of their arbitrary combination.
2. the preparation method of efficient electrolysis Phosphating Solution described in claim 1, comprise the following steps: the deionized water 1) being first injected to the electrolytic phosphating liquid cumulative volume 1/5-1/4 of required preparation in a container, add phosphoric acid and nitric acid again, heat while stirring, when temperature arrives 80 DEG C, slowly add zinc oxide while stirring, after zinc to be oxidized dissolves completely, stop heating; 2) add calcium carbonate again after continuing to stir half an hour, then continue to stir half an hour; 3) above-mentioned 2) step complete after after the solution of acquisition is down to room temperature, add additive, and continue to be stirred to and dissolve completely, and then add deionized water constant volume, namely obtain electrolytic phosphating liquid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510085709.0A CN104630867A (en) | 2015-02-17 | 2015-02-17 | High-efficiency electrolytic phosphating solution |
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| CN201510085709.0A CN104630867A (en) | 2015-02-17 | 2015-02-17 | High-efficiency electrolytic phosphating solution |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757280A (en) * | 2016-12-13 | 2017-05-31 | 河南恒星钢缆股份有限公司 | A kind of low temperature On-line electrolytic dissolution Phosphating Solution |
| CN107723696A (en) * | 2017-10-10 | 2018-02-23 | 宁波德豪模架有限公司 | A kind of mould bases and its processing technology |
| CN109056035A (en) * | 2018-08-13 | 2018-12-21 | 济源金五联金属制品有限公司 | A kind of very fast electrolytic phosphating process |
| CN109778166A (en) * | 2019-03-25 | 2019-05-21 | 四川亨通兴达科技有限公司 | The phosphorization treatment process of phosphating solution, the preparation method of phosphating solution and metal wire rod |
| CN109853023A (en) * | 2019-03-26 | 2019-06-07 | 华南理工大学 | A kind of zinc system anti-corrosion electrolytic phosphating liquid and preparation method thereof |
| CN113481565A (en) * | 2021-07-07 | 2021-10-08 | 安徽长江紧固件有限责任公司 | Electrolytic phosphating solution for large-specification fasteners |
| CN115573015A (en) * | 2022-09-01 | 2023-01-06 | 东莞市颖兴金属表面处理材料有限公司 | Electrolytic phosphating solution and preparation method thereof |
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| RU2090650C1 (en) * | 1995-03-07 | 1997-09-20 | Акционерное общество закрытого типа "ФК" | Solution for phosphating the metallic surface |
| US20020009622A1 (en) * | 1999-08-03 | 2002-01-24 | Goodson David M. | Sprayable phosphate cementitious coatings and a method and apparatus for the production thereof |
| KR20020089214A (en) * | 2002-08-14 | 2002-11-29 | 송길웅 | Zinc-calcium based coloring composition, preparation thereof and parkerizing process using the same |
| CN102719872A (en) * | 2012-06-08 | 2012-10-10 | 南京派诺金属表面处理技术有限公司 | Slag-free low-temperature rapid electrolytic phosphorizing liquid and phosphorizing process thereof |
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| CN103938201A (en) * | 2014-04-30 | 2014-07-23 | 安徽启明表面技术有限公司 | Black phosphorizing method with high corrosion resistance |
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2015
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| US20020009622A1 (en) * | 1999-08-03 | 2002-01-24 | Goodson David M. | Sprayable phosphate cementitious coatings and a method and apparatus for the production thereof |
| KR20020089214A (en) * | 2002-08-14 | 2002-11-29 | 송길웅 | Zinc-calcium based coloring composition, preparation thereof and parkerizing process using the same |
| CN102719872A (en) * | 2012-06-08 | 2012-10-10 | 南京派诺金属表面处理技术有限公司 | Slag-free low-temperature rapid electrolytic phosphorizing liquid and phosphorizing process thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757280A (en) * | 2016-12-13 | 2017-05-31 | 河南恒星钢缆股份有限公司 | A kind of low temperature On-line electrolytic dissolution Phosphating Solution |
| CN107723696A (en) * | 2017-10-10 | 2018-02-23 | 宁波德豪模架有限公司 | A kind of mould bases and its processing technology |
| CN109056035A (en) * | 2018-08-13 | 2018-12-21 | 济源金五联金属制品有限公司 | A kind of very fast electrolytic phosphating process |
| CN109778166A (en) * | 2019-03-25 | 2019-05-21 | 四川亨通兴达科技有限公司 | The phosphorization treatment process of phosphating solution, the preparation method of phosphating solution and metal wire rod |
| CN109853023A (en) * | 2019-03-26 | 2019-06-07 | 华南理工大学 | A kind of zinc system anti-corrosion electrolytic phosphating liquid and preparation method thereof |
| CN113481565A (en) * | 2021-07-07 | 2021-10-08 | 安徽长江紧固件有限责任公司 | Electrolytic phosphating solution for large-specification fasteners |
| CN113481565B (en) * | 2021-07-07 | 2022-05-10 | 安徽长江紧固件有限责任公司 | Electrolytic phosphating method for large-size fasteners |
| CN115573015A (en) * | 2022-09-01 | 2023-01-06 | 东莞市颖兴金属表面处理材料有限公司 | Electrolytic phosphating solution and preparation method thereof |
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Application publication date: 20150520 |