CN103132122B - Steel wire on-line normal-temperature electrolytic phosphatization method - Google Patents
Steel wire on-line normal-temperature electrolytic phosphatization method Download PDFInfo
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- CN103132122B CN103132122B CN201110371863.6A CN201110371863A CN103132122B CN 103132122 B CN103132122 B CN 103132122B CN 201110371863 A CN201110371863 A CN 201110371863A CN 103132122 B CN103132122 B CN 103132122B
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- steel wire
- electrolytic
- heat treated
- negative electrode
- electric current
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 69
- 239000010959 steel Substances 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 32
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 16
- 239000010452 phosphate Substances 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- 238000001994 activation Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 7
- 150000003016 phosphoric acids Chemical class 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- 238000005868 electrolysis reaction Methods 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 230000010287 polarization Effects 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims 1
- 235000011149 sulphuric acid Nutrition 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000013049 sediment Substances 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 230000004913 activation Effects 0.000 description 12
- 229910052759 nickel Inorganic materials 0.000 description 6
- 238000005554 pickling Methods 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- 239000002184 metal Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 241001347978 Major minor Species 0.000 description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 3
- 229910000978 Pb alloy Inorganic materials 0.000 description 3
- 239000012190 activator Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical group [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 238000005491 wire drawing Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
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- Chemical Treatment Of Metals (AREA)
Abstract
The invention relates to a steel wire on-line normal-temperature electrolytic phosphatization method which comprises the following steps: firstly performing surface cleaning of heat-treated steel wires by an electrolytic acid method, and performing electrolytic phosphatization of the steel wires at normal temperature. The invention provides an energy-saving, low-carbon, green, environment-friendly steel wire on-line normal-temperature electrolytic phosphatization method; when compared with the prior art, the method of the invention has the advantages of less time consumption, high efficiency, no phosphate sediment generation, no heating requirement, realizability at normal temperature, and the like.
Description
Technical field
The present invention relates to metal products deep-draw processing technique field, be specifically related to the online normal-temperature electrolytic phosphatization of steel wire.
Background technology
In metal products deep-draw processing industry, in order to the steel wire of certain specification and intensity rank will be obtained, need through multiple tracks treatment process.Wherein, in wire rod cogging technics link, traditional method adopts:
A, carry out acidifying, namely remove panel surface zone of oxidation;
B, water rinse;
C, middle temperature soak phosphatization, and wherein temperature is not less than 70 DEG C, and soak time is 5-10 minute;
D, water rinse;
E, saponification;
F, steel wire drawing;
G, same temperature hardening heat treatment;
H, A-B-C-D-E-F step is repeated to the process wire after thermal treatment, carry out deep-draw processing further.
Visible, traditional steel wire middle temperature phosphating method not only consuming time but also effort, its phosphating time needed generally more than 60 seconds, and requires that the temperature to soaking phosphatization controls more than 70 DEG C, can produce the objectionable impuritiess such as a large amount of phosphoric acid salt sediments, the discharge of objectionable impurities can cause severe contamination to environment.
Summary of the invention
The object of the present invention is to provide the online normal-temperature electrolytic phosphatization of a kind of steel wire, without the need to heating in immersion parkerizing process, can realize under normal temperature, and phosphoric acid salt sediment can not be produced.Compare compared with the parkerizing process of traditional method, phosphating time shortens by the present invention greatly, only needs 10 seconds.
In order to realize foregoing invention object, the online normal-temperature electrolytic phosphatization of steel wire provided by the invention adopts following technical characteristic:
A, carry out surface cleaning process to through heat treated steel wire, by the zone of oxidation of electrolysis acid system eccysis Steel Wire Surface, the acid solution water of Steel Wire Surface remnants is rinsed well;
B, surface activation process is carried out to steel wire, by through surface cleaning Treatment of Washing except the steel wire base of surface oxide layer is fully exposed, with the oxalic acid aqueous solution effect of 8%-12% lower concentration, produce polarization surface energy;
C, electrolytic phosphating process is carried out to steel wire, steel wire through surface active is imported cathode electrolytic cell reposefully by cathode wire opinion, polarized by the effect generation negative electrode phosphoric acid salt of pulse direct current electric current, make insoluble phosphoric acid salt be deposited on Steel Wire Surface securely.
In step C, the thickness of phosphorous layer needed for Steel Wire Drawing Process, implements the control to steel wire cathode current density, guarantees that phosphorous layer at least can reach 8g/m within 10 seconds
2above.
The invention provides the online normal-temperature electrolytic phosphatization of steel wire of a kind of energy-conservation, low-carbon (LC), environmental protection, compared with conventional phosphatizing method, the present invention have consuming time short, efficiency is high, do not produce phosphoric acid salt sediment, the progressive such as can to realize without the need to heating normal temperature, refers to following table.
Accompanying drawing explanation
Fig. 1 is the online normal-temperature electrolytic phosphatization schematic diagram of a kind of steel wire provided by the invention.
Fig. 2 is the online normal-temperature electrolytic phosphatization schema of a kind of steel wire provided by the invention.
Identifier declaration:
1-cathode wire is taken turns; The major-minor negative electrode of 2-; 3-electrolyzer; 4-Lower tank; 5-impulse commutation system; 6-current control system; 7-overflow control device; 8-liquid pump.
Specific implementation method
Below in conjunction with drawings and Examples, description clear, complete is further done to technical scheme of the present invention, so that novelty, creativeness and practicality that the present invention meets patent law completely and requires to be described.It should be noted that and can not be used for just a part of embodiment of the present invention that embodiment describes limiting the scope of the invention.
Embodiment 1
The invention provides a kind of normal-temperature electrolytic phosphatization of steel wire, the steps include:
Steps A: carry out surface treatment to through heat treated steel wire.Remove surface scale of steel wire by electrolytic pickling, this method removes descaling more thoroughly totally than mechanical, and plays the effect of activation Steel Wire Surface, increase activation energy.Electrolytic pickling liquid adopts concentration to be the sulfuric acid of 10%, and how much judges according to surface scale of steel wire the size applying electric current, is rinsed by the sour water of Steel Wire Surface remnants dry clear, then carries out Steel Wire Surface activation treatment.
Step B: surface activation process is the critical process of steel wire normal temperature electrolytic phosphating, present invention employs concentration be the oxalic acid solution of 8% as activator, impel Steel Wire Surface within 5 seconds, form the activation nucleus of the tiny densification of multinuclear.
Step C: the steel wire through surface active imports in electrolytic phosphating groove, applies certain electric current under normal temperature condition by anticathode, just can obtain within 10 seconds that the whole Steel Wire Surface of covering is complete, firmly phosphatize phosphate coat.If desired 8g/m is obtained
2the phosphatize phosphate coat of above thickness, can regulate according to heat treated linear velocity the size applying electric current.
Such as, in step C, if implement to steel wire diameter be
carry out normal temperature electrolytic phosphating, and heat treated linear velocity is 12m/min, phosphatize phosphate coat thickness need be obtained and reach 8g/m
2above, then the electric current being applied to steel wire (negative electrode) is 150mA.
As shown in Figure 1, the normal temperature electrolytic phosphating of implementation step C, bottom nickel in its electrolyzer 3, lead alloy and impulse commutation system 5, the anode of current control system 6 is connected, wherein, main electrode is nickel metal, auxiliary electrode is lead metal, under the startup of liquid pump 8, normal temperature electrolytic phosphating liquid injects rapidly electrolytic phosphating groove 3, guarantee that the steel wire be imported into all is immersed in from below liquid level 2cm, regulating overflow to control 6 makes Phosphating Solution overflow in Lower tank 4, then steel wire is entered electrolyzer 3 by cathode wire wheel 1, open impulse commutation system 5 and apply pulsed current by major-minor negative electrode 2 pairs of steel wires, current control system 6 is regulated to obtain 8g/m according to heat treated linear velocity
2the phosphatize phosphate coat of above thickness.
Embodiment 2
The invention provides a kind of normal-temperature electrolytic phosphatization of steel wire, the steps include:
Steps A: carry out surface treatment to through heat treated steel wire.Remove surface scale of steel wire by electrolytic pickling, this method removes descaling more thoroughly totally than mechanical, and plays the effect of activation Steel Wire Surface, increase activation energy.Electrolytic pickling liquid adopts concentration to be the sulfuric acid of 10%, and how much judges according to surface scale of steel wire the size applying electric current, is rinsed by the sour water of Steel Wire Surface remnants dry clear, then carries out Steel Wire Surface activation treatment.
Step B: surface activation process is the critical process of steel wire normal temperature electrolytic phosphating, present invention employs concentration be the oxalic acid solution of 10% as activator, impel Steel Wire Surface within 5 seconds, form the activation nucleus of the tiny densification of multinuclear.
Step C: the steel wire through surface active imports in electrolytic phosphating groove, applies certain electric current under normal temperature condition by anticathode, just can obtain within 10 seconds that the whole Steel Wire Surface of covering is complete, firmly phosphatize phosphate coat.If desired 8g/m is obtained
2the phosphatize phosphate coat of above thickness, can regulate according to heat treated linear velocity the size applying electric current.
In step C, if implement to steel wire diameter be
carry out normal temperature electrolytic phosphating, and heat treated linear velocity is 15m/min, phosphatize phosphate coat thickness need be obtained and reach 8g/m
2above, then the electric current being applied to steel wire (negative electrode) is 120mA.
As shown in Figure 1, the normal temperature electrolytic phosphating of implementation step C, bottom nickel in its electrolyzer 3, lead alloy and impulse commutation system 5, the anode of current control system 6 is connected, wherein, main electrode is nickel metal, auxiliary electrode is lead metal, under the startup of liquid pump 8, normal temperature electrolytic phosphating liquid injects rapidly electrolytic phosphating groove 3, guarantee that the steel wire be imported into all is immersed in from below liquid level 2cm, regulating overflow to control 6 makes Phosphating Solution overflow in Lower tank 4, then steel wire is entered electrolyzer 3 by cathode wire wheel 1, open impulse commutation system 5 and apply pulsed current by major-minor negative electrode 2 pairs of steel wires, current control system 6 is regulated to obtain 8g/m according to heat treated linear velocity
2the phosphatize phosphate coat of above thickness.
Embodiment 3
The invention provides a kind of normal-temperature electrolytic phosphatization of steel wire, the steps include:
Steps A: carry out surface treatment to by through heat treated steel wire.Remove surface scale of steel wire by electrolytic pickling, this method removes descaling more thoroughly totally than mechanical, and plays the effect of activation Steel Wire Surface, increase activation energy.Electrolytic pickling liquid adopts concentration to be the sulfuric acid of 12%, and how much judges according to surface scale of steel wire the size applying electric current, is rinsed by the sour water of Steel Wire Surface remnants dry clear, then carries out Steel Wire Surface activation treatment.
Step B: surface activation process is the critical process of steel wire normal temperature electrolytic phosphating, present invention employs concentration be the oxalic acid solution of 12% as activator, impel Steel Wire Surface within 5 seconds, form the activation nucleus of the tiny densification of multinuclear.
Step C: the steel wire through surface active imports in electrolytic phosphating groove, applies certain electric current under normal temperature condition by anticathode, just can obtain within 10 seconds that the whole Steel Wire Surface of covering is complete, firmly phosphatize phosphate coat.If desired 8g/m is obtained
2the phosphatize phosphate coat of above thickness, can regulate according to heat treated linear velocity the size applying electric current.
In step C, if implement to steel wire diameter be
carry out normal temperature electrolytic phosphating, and heat treated linear velocity is 20m/min, phosphatize phosphate coat thickness need be obtained and reach 8g/m
2above, then the electric current being applied to steel wire (negative electrode) is 100mA.
As shown in Figure 1, the normal temperature electrolytic phosphating of implementation step C, bottom nickel in its electrolyzer 3, lead alloy and impulse commutation system 5, the anode of current control system 6 is connected, wherein, main electrode is nickel metal, auxiliary electrode is lead metal, under the startup of liquid pump 8, normal temperature electrolytic phosphating liquid injects rapidly electrolytic phosphating groove 3, guarantee that the steel wire be imported into all is immersed in from below liquid level 2cm, regulating overflow to control 6 makes Phosphating Solution overflow in Lower tank 4, thereafter steel wire is entered electrolyzer 3 by cathode wire wheel 1, open impulse commutation system 5 and apply pulsed current by major-minor negative electrode 2 pairs of steel wires, current control system 6 is regulated to obtain 8g/m according to heat treated linear velocity
2the phosphatize phosphate coat of above thickness.
Claims (7)
1. the online normal-temperature electrolytic phosphatization of steel wire, is characterized in that:
A, carry out surface cleaning process to through heat treated steel wire, by the zone of oxidation of electrolysis acid system eccysis Steel Wire Surface, the acid solution water of Steel Wire Surface remnants is rinsed well;
B, surface activation process is carried out to steel wire, by through surface cleaning Treatment of Washing except the steel wire base of surface oxide layer is fully exposed, be the oxalic acid aqueous solution effect of 8%-12% with concentration range, within 5 seconds, produce polarization surface energy;
C, electrolytic phosphating process is carried out to steel wire, under normal temperature condition more than 0 DEG C, steel wire through surface active is imported cathode electrolytic cell by guide roller, is polarized by the effect generation negative electrode phosphoric acid salt of pulse direct current, make insoluble phosphoric acid salt be deposited on Steel Wire Surface securely.
2. method according to claim 1, is characterized in that, the electrolysis acid solution that steps A adopts to be concentration be 10% sulphuric acid soln.
3. method according to claim 1, is characterized in that, in step B, the action time of steel wire and oxalic acid solution was 5 seconds.
4. method according to claim 1, is characterized in that, when the normal temperature electrolytic phosphating of step C, steel wire is imported in electrolytic phosphating groove, and steel wire all should be immersed in the degree of depth of distance below liquid level 2cm.
5. method according to claim 1, is characterized in that, in step C, if that steel wire is directly Φ 3.60mm, heat treated linear velocity is 12m/min, need obtain phosphatize phosphate coat thickness and reach 8g/m
2above, then the electric current being applied to steel wire negative electrode is 150mA.
6. method according to claim 1, is characterized in that, in step C, if steel wire diameter is Φ 2.80mm, heat treated linear velocity is 15m/min, need obtain phosphatize phosphate coat thickness and reach 8g/m
2above, then the electric current being applied to steel wire negative electrode is 120mA.
7. method according to claim 1, is characterized in that, in step C, if steel wire diameter is Φ 1.60mm, heat treated linear velocity is 20m/min, need obtain phosphatize phosphate coat thickness and reach 8g/m
2above, then the electric current being applied to steel wire negative electrode is 100mA.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110371863.6A CN103132122B (en) | 2011-11-22 | 2011-11-22 | Steel wire on-line normal-temperature electrolytic phosphatization method |
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|---|---|---|---|
| CN201110371863.6A CN103132122B (en) | 2011-11-22 | 2011-11-22 | Steel wire on-line normal-temperature electrolytic phosphatization method |
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| CN103132122B true CN103132122B (en) | 2015-07-22 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103741195B (en) * | 2013-12-23 | 2016-06-15 | 南通恒新金属工艺科技有限公司 | Electrolytic phosphating of steel wires processes device |
| CN105951155B (en) * | 2016-06-01 | 2017-12-29 | 中钢集团郑州金属制品研究院有限公司 | A kind of steel wire double method for bonderizing and its continuous producing apparatus online |
| CN109056034A (en) * | 2018-08-03 | 2018-12-21 | 南京派诺金属表面处理技术有限公司 | Room temperature electrolytic phosphating process and phosphating solution |
| CN111197163A (en) * | 2018-11-20 | 2020-05-26 | 天津市银丰钢绞线股份有限公司 | Pretreatment process of steel strand |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0340530A1 (en) * | 1988-04-28 | 1989-11-08 | Henkel Kommanditgesellschaft auf Aktien | Titanium-free activating agents, process for preparing them and their use in activating a metal surface before zinc phosphating |
| WO2003042426A2 (en) * | 2001-11-14 | 2003-05-22 | Henkel Kommanditgesellschaft Auf Aktien | Regulation of the accelerator concentration in phosphating baths |
| CN1891865A (en) * | 2005-04-28 | 2007-01-10 | 株式会社电装 | Electrolytic phosphating process |
| CN102061503A (en) * | 2010-11-19 | 2011-05-18 | 江苏巨力钢绳有限公司 | Electrolytic phosphating method for steel wires |
-
2011
- 2011-11-22 CN CN201110371863.6A patent/CN103132122B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0340530A1 (en) * | 1988-04-28 | 1989-11-08 | Henkel Kommanditgesellschaft auf Aktien | Titanium-free activating agents, process for preparing them and their use in activating a metal surface before zinc phosphating |
| US5039362A (en) * | 1988-04-28 | 1991-08-13 | Henkel Kommanditgesellschaft Auf Aktien | Titanium free composition and process for activating metal surfaces prior to zinc phosphating |
| WO2003042426A2 (en) * | 2001-11-14 | 2003-05-22 | Henkel Kommanditgesellschaft Auf Aktien | Regulation of the accelerator concentration in phosphating baths |
| CN1891865A (en) * | 2005-04-28 | 2007-01-10 | 株式会社电装 | Electrolytic phosphating process |
| CN102061503A (en) * | 2010-11-19 | 2011-05-18 | 江苏巨力钢绳有限公司 | Electrolytic phosphating method for steel wires |
Non-Patent Citations (2)
| Title |
|---|
| Acceleration of ambient temperature phosphating by an electrochemical pulse technique;P. Bala Srinivasan等;《Surface and Coatings Technology》;19941231;第64卷;第161—165页 * |
| 钢丝磷化质量差异原因浅析;陈健民;《金属制品》;20001231;第26卷(第5期);第21-24页 * |
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