CN107513682B - A kind of zincincation of acid circulation - Google Patents
A kind of zincincation of acid circulation Download PDFInfo
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- CN107513682B CN107513682B CN201710730586.0A CN201710730586A CN107513682B CN 107513682 B CN107513682 B CN 107513682B CN 201710730586 A CN201710730586 A CN 201710730586A CN 107513682 B CN107513682 B CN 107513682B
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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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
- C23C2/06—Zinc or cadmium or alloys based thereon
Abstract
The invention discloses a kind of zincincations of acid circulation, its key points of the technical solution are that comprising the technical steps that: (1) degreasing；(2) it cleans；(3) pickling；(4) it aoxidizes；(5) iron is removed；(6) acid solution is recycled；(7) plating is helped；(8) zinc-plated；(9) cooling；(10) it chromium-free deactivation and cools down again, after iron removal step, Tea Saponin aqueous solution is put into pickling tube, Tea Saponin aqueous solution plays stabilization to aqueous ammonium chloride solution, be conducive to ammonia radical ion steadily to exist in aqueous ammonium chloride solution, purer hydrogen chloride is evaporated to be conducive to hydrochloric acid, to improve the cyclic utilization rate of hydrochloric acid.
Description
Technical field
The present invention relates to chemical field, in particular to a kind of zincincation of acid circulation.
Background technique
In recent years, as high voltage power transmission, traffic, communication career rapidly develop, heat higher and higher to steel and iron parts requirement of shelter
Zinc-plated demand is also continuously increased.Hot galvanizing is that zinc ingot metal is melted at high temperature, then adds some auxiliary materials, metal structure
Part immerses in galvanizing bath, adheres to one layer of galvanized alloy layer in metal component surface.Usual cold galvanizing layer with a thickness of 5 ~ 15 μm, and
Hot galvanized layer is generally at 35 μm or more, and even as high as 200 μm, hot dip galvanizing process covering power is good, plated layer compact, no organic matter folder
It is miscellaneous, there is excellent corrosion resisting property and service life.
Currently, application publication number is that the Chinese patent of CN106868438A discloses a kind of steel structure galvanizer in existing patent
Skill, processing step include: 1) supplied materials pretreatment；2) it washes；3) pickling；4) it washes；5) plating assistant solvent is soaked；6) it dries；7) steel
Structure is zinc-plated；8) cooling；9) medicine；10) it cleans；11) it polishes；12) it examines；The processing step is simple, efficiently solves unplated piece
The zinc-plated rear surface of steel structure blacks, the problem of piebald occurs.
The process of above-mentioned pickling is to clean up the rusty stain on steel member surface, pickling be for improve coating and matrix it
Between adhesive force, still, after pickling in remaining acid solution contain a large amount of iron ion, be not suitable for be recycled, the processing of spent acid
Problem is the problem that those skilled in the art urgently captures at this stage.
Summary of the invention
The object of the present invention is to provide a kind of zincincation of acid circulation, which solves the difficulty of waste acid treatment
Topic is recycled hydrochloric acid, significantly reduces the cost of galvanizing process.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of zincincation of acid circulation, comprises the technical steps that:
(1) degreasing: metal component being stacked neatly, successively metal component is sling using driving and puts into service sink,
The alkaline degreasing agent that mass concentration is 5 ~ 10% is put into, the oil substances of metal component surface are cleaned, water temperature is maintained at
45 ~ 50 DEG C, the processing time is 0.5 ~ 1 hour；
(2) clean: by degreasing, treated that metal component is placed in flushing tank, is 5 ~ 10% using mass concentration
NaCl solution is rinsed the surface of metal component；
(3) pickling: the metal component after flushing is put into pickling tube, in pickling tube the mass concentration of hydrochloric acid be 23 ~
25%, soaking time is 1 ~ 1.5 hour；
(4) aoxidize: after Chu Liwan is with the metal component of batch, it is 28 ~ 32% that mass concentration is passed through into pickling tube
H2O2Aqueous solution, by Fe2+It is oxidized to Fe3+；
(5) it removes iron: to by the ammonium hydroxide that mass concentration is 25 ~ 28% is added in step (4) treated pickling tube, standing,
So that Fe(OH)3Precipitating completely, and excludes precipitating Fe(OH)3；
(6) acid solution is recycled: and then by step (5), treated that remaining acid solution introduces in evaporator, and mass concentration is added
It for 60 ~ 70% Tea Saponin, is heated to reflux, collects hydrochloric acid, it will be in the hydrochloric acid cycle bleeder to pickling tube that be collected into；
(7) it helps plating: metal component of the step (3) after pickling being put into and is helped in coating bath, quickening liquid uses zinc chloride and chlorine
Change ammonium salt solution to be mixed to form, in metal component surface forming salt film；
(8) zinc-plated: through step (7), treated, and metal component is put into galvanized bath, and the zinc liquid ingredient in galvanized bath is nickel
0.018 ~ 0.03%, aluminium 0.005 ~ 0.008%, rare earth 0.003 ~ 0.005%, tin 0.001%, remaining is zinc, and the temperature of zinc liquid is protected
It holds between 450 ~ 510 DEG C, dip time is 1 ~ 5 minute；
(9) cooling: after zinc-plated, metal component to be placed in cold rinse bank, the softened water using water temperature lower than 40 DEG C is cooling
Sizing；
(10) it chromium-free deactivation and cools down again.
By using above-mentioned technical proposal, zincincation include degreasing, cleaning, pickling, except iron, help plating, zinc-plated and cold
But, passivation, process cooling again put into Tea Saponin aqueous solution, Tea Saponin aqueous solution pair into pickling tube after iron removal step
Aqueous ammonium chloride solution plays stabilization, is conducive to ammonia radical ion and steadily exists in aqueous ammonium chloride solution, to be conducive to
Hydrochloric acid evaporates purer hydrogen chloride, to improve the cyclic utilization rate of hydrochloric acid.
The present invention is further arranged to: the alkalinity degreasing agent is the ten phosphate dihydrate sodium and metaphosphoric acid that mass ratio is 1:1
The mixture of sodium.
By using above-mentioned technical proposal, ten phosphate dihydrate sodium are colourless or white crystals, are dissolved in water, and aqueous solution is in highly basic
Property, ethyl alcohol, carbon disulfide are not dissolved in, plays quality-improving in food processing, for example has in meat products and keeps holding for meat
It is aqueous, promote the effects of being knotted power, reduces the loss of nutritional ingredient in meat, keep the tenderness of meat；Cream is also served as in food
Agent, nutritional supplement, quality improver are the raw materials for preparing wheaten food buck；Also serve as the washing of food bottle, tank etc.
Agent；Sodium metaphosphate is colourless glass clear crystals, white plates or powder, and easy to moisture absorption in air, being dissolved in water is in that alkalinity is anti-
It answers, does not dissolve in ethyl alcohol；Ten phosphate dihydrate sodium and sodium metaphosphate are used in compounding, the infiltration on metal component surface is enhanced
Property, to improve the degreasing ability to metal component surface；Meanwhile also improving the combination of zinc coat and metal component surface
Power.
The present invention is further arranged to: limiting the flushing speed of NaCl solution as 10 ~ 20L/min in step (2).
By using above-mentioned technical proposal, when the flushing speed of NaCl solution is lower than 10L/min, to metal component surface
Impact force it is smaller, be unfavorable for the cleaning to metal component surface；It is right when the flushing speed of NaCl solution is higher than 20L/min
The impact force of metal component surface is larger, also larger to the recoil strength of NaCl solution according to active force and reaction force principle, no
Conducive to the maintenance to workshop condition.
The present invention is further arranged to: hydrochloric acid and H in step (4)2O2The mass ratio of the material of aqueous solution is 6 ~ 8:1.
By using above-mentioned technical proposal, H2O2Aqueous solution has stronger oxidisability, by the Fe in pickling tube2+It is oxidized to
Fe3+, 1molH2O2Aqueous solution can aoxidize the Fe of 2mol2+, 6molHCl is capable of handling 1molFe2O3(iron rust), so setting salt
Acid and H2O2The mass ratio of the material of aqueous solution is 6:1, and to completely remove the iron rust on metal component surface, hydrochloric acid is excessive, but
To save cost, content of hydrochloric acid is not easy excessively, hydrochloric acid and H2O2The amount proportion of the optimal substance of aqueous solution is 6 ~ 8:1.
The present invention is further arranged to: the pH that mixed solution in pickling tube is adjusted in step (5) is 3 ~ 3.5.
By using above-mentioned technical proposal, after the ammonium hydroxide that mass concentration is 25 ~ 28% is added, the Fe in pickling tube3+It can occur
Precipitating can promote Fe when pH is between 3 ~ 3.53+Precipitating, be conducive to that Fe is quickly discharged in hydrochloric acid3+。
The present invention is further arranged to: heating temperature is to 100 ~ 110 DEG C in step (6), so that the chlorination in remaining acid solution
Hydrogen volatilizees completely.
By using above-mentioned technical proposal, heating temperature is controlled at 100 ~ 110 DEG C, the hydrogen chloride gas in hydrochloric acid is in the temperature
It can volatilize away as much as possible within degree range, to improve the recovery efficiency to hydrochloric acid.
The present invention is further arranged to: in the quickening liquid of step (7) the mass ratio of the material of zinc chloride and ammonium chloride be 1:2 ~
3。
By using above-mentioned technical proposal, ammonium chloride helps plating effect obvious, but decomposition temperature is lower, easily decomposes mistake when heated
Effect, therefore the drying temperature of metal component quickening liquid is no more than 140 DEG C；In addition, metal component surface helps the ammonium chloride in plating salt film
Biggish flue dust can also be caused；Zinc chloride is easy dampness, but better heat stability, and generation flue dust is less when soaking zinc, by zinc chloride
Generation synergistic effect is mixed with ammonium chloride, is conducive to improve and plating effect is helped to metal component surface.
The present invention is further arranged to: the off speed of metal component is 1 ~ 1.5 meter/min in step (8).
By using above-mentioned technical proposal, after zinc-plated process, limit the off speed of metal component as 1 ~ 1.5 meter/
Min shows that metal component is to reduce the shadow to metal component surface zinc coat compactness in slow removal galvanized bath after zinc-plated
It rings.
In conclusion the invention has the following advantages:
1, after except iron embroidery art sequence, the Tea Saponin that mass concentration is 60 ~ 70%, Tea Saponin are added into remaining acid solution
The stability of ammonium chloride in acid solution is enhanced, during being heated to reflux, the thermal decomposition of ammonium chloride is reduced, improves to chlorination
The recovery efficiency of hydrogen；
2, it after the processing of parlkaline degreasing agent degreasing, is rinsed, is had using surface of the NaCl solution to metal component
Conducive to the compactness for improving metal component surface；
3, alkaline degreasing agent is mixed using ten phosphate dihydrate sodium and sodium metaphosphate, improves the infiltration on metal component surface
Permeability, so that the degreasing ability to metal component surface is improved, meanwhile, also improve the combination of zinc coat and metal component surface
Power；
4, in Fe3+In precipitation process, adjusting pH is 3 ~ 3.5, is conducive to that Fe is quickly discharged in hydrochloric acid3+。
Specific embodiment
Invention is further described in detail with reference to embodiments.
Embodiment one:
A kind of zincincation of acid circulation, comprises the technical steps that:
(1) degreasing: metal component being stacked neatly, successively metal component is sling using driving and puts into service sink,
The aqueous solution for the ten phosphate dihydrate sodium and sodium metaphosphate that mass concentration is 5% is put into, wherein ten phosphate dihydrate sodium and sodium metaphosphate
The mass ratio of the material is 1:1, is stirred evenly, and water temperature is maintained at 45 DEG C, and the processing time is 1 hour；
(2) clean: by degreasing, treated that metal component is placed in flushing tank, and the NaCl for being 8% using mass concentration is molten
Liquid is rinsed the surface of metal component, and flushing speed is 10L/min；
(3) pickling: the metal component after flushing is put into pickling tube, and the mass concentration of hydrochloric acid is 23% in pickling tube, leaching
Steeping the time is 1 hour；
(4) it removes iron: after Chu Liwan is with the metal component of batch, the H that mass concentration is 28% is passed through into pickling tube2O2Water
Solution, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The mass ratio of the material of aqueous solution is 7:1；
(5) it to by the ammonium hydroxide that mass concentration is 25% is added in step (4) treated pickling tube, adjusts in pickling tube
The pH of mixed solution is 3.5, is stood, so that Fe(OH)3Precipitating completely, and excludes precipitating Fe(OH)3；
(6) acid solution is recycled: and then by step (5), treated that remaining acid solution introduces in evaporator, and mass concentration is added
It for 60% Tea Saponin aqueous solution, is heated to reflux, collects hydrochloric acid, it will be in the hydrochloric acid cycle bleeder to pickling tube that be collected into；
(7) it helps plating: metal component of the step (3) after pickling being put into and is helped in coating bath, quickening liquid uses zinc chloride and chlorine
Change ammonium to be mixed to form by the mass ratio of the material for 1:2, in metal component surface forming salt film；
(8) zinc-plated: through step (7), treated, and metal component is put into galvanized bath, and the zinc liquid ingredient in galvanized bath is nickel
0.018%, aluminium 0.005%, rare earth 0.003%, tin 0.001%, remaining is zinc, and the temperature of zinc liquid is maintained at 450 DEG C, when dipping
Between be 3 minutes, the off speed of metal component is 1 meter/min；
(9) cooling: after zinc-plated, metal component to be placed in cold rinse bank, the softened water using water temperature lower than 40 DEG C is cooling
Sizing；
(10) it chromium-free deactivation and cools down again.
Embodiment two:
A kind of zincincation of acid circulation, comprises the technical steps that:
(1) degreasing: metal component being stacked neatly, successively metal component is sling using driving and puts into service sink,
The aqueous solution for the ten phosphate dihydrate sodium and sodium metaphosphate that mass concentration is 8% is put into, wherein ten phosphate dihydrate sodium and sodium metaphosphate
The mass ratio of the material is 1:1, is stirred evenly, and water temperature is maintained at 45 DEG C, and the processing time is 1 hour；
(2) clean: by degreasing, treated that metal component is placed in flushing tank, the NaCl for being 10% using mass concentration
Solution is rinsed the surface of metal component, and flushing speed is 15L/min；
(3) pickling: the metal component after flushing is put into pickling tube, and the mass concentration of hydrochloric acid is 25% in pickling tube, leaching
Steeping the time is 1 hour；
(4) it removes iron: after Chu Liwan is with the metal component of batch, the H that mass concentration is 30% is passed through into pickling tube2O2Water
Solution, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The mass ratio of the material of aqueous solution is 7:1；
(5) it to by the ammonium hydroxide that mass concentration is 25% is added in step (4) treated pickling tube, adjusts in pickling tube
The pH of mixed solution is 3.2, is stood, so that Fe(OH)3Precipitating completely, and excludes precipitating Fe(OH)3；
(6) acid solution is recycled: and then by step (5), treated that remaining acid solution introduces in evaporator, and mass concentration is added
It for 65% Tea Saponin aqueous solution, is heated to reflux, collects hydrochloric acid, it will be in the hydrochloric acid cycle bleeder to pickling tube that be collected into；
(7) it helps plating: metal component of the step (3) after pickling being put into and is helped in coating bath, quickening liquid uses zinc chloride and chlorine
Change ammonium to be mixed to form by the mass ratio of the material for 1:3, in metal component surface forming salt film；
(8) zinc-plated: through step (7), treated, and metal component is put into galvanized bath, and the zinc liquid ingredient in galvanized bath is nickel
0.018%, aluminium 0.005%, rare earth 0.003%, tin 0.001%, remaining is zinc, and the temperature of zinc liquid is maintained at 470 DEG C, when dipping
Between be 3 minutes, the off speed of metal component is 1 meter/min；
(9) cooling: after zinc-plated, metal component to be placed in cold rinse bank, the softened water using water temperature lower than 40 DEG C is cooling
Sizing；
(10) it chromium-free deactivation and cools down again.
Embodiment three:
A kind of zincincation of acid circulation, comprises the technical steps that:
(1) degreasing: metal component being stacked neatly, successively metal component is sling using driving and puts into service sink,
The aqueous solution for putting into the ten phosphate dihydrate sodium and sodium metaphosphate that mass concentration is 10%, wherein ten phosphate dihydrate sodium and sodium metaphosphate
The mass ratio of the material be 1:1, stir evenly, water temperature is maintained at 45 DEG C, and the processing time is 1 hour；
(2) clean: by degreasing, treated that metal component is placed in flushing tank, the NaCl for being 10% using mass concentration
Solution is rinsed the surface of metal component, and flushing speed is 20L/min；
(3) pickling: the metal component after flushing is put into pickling tube, and the mass concentration of hydrochloric acid is 25% in pickling tube, leaching
Steeping the time is 1 hour；
(4) it removes iron: after Chu Liwan is with the metal component of batch, the H that mass concentration is 30% is passed through into pickling tube2O2Water
Solution, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The mass ratio of the material of aqueous solution is 8:1；
(5) it to by the ammonium hydroxide that mass concentration is 25% is added in step (4) treated pickling tube, adjusts in pickling tube
The pH of mixed solution is 3.5, is stood, so that Fe(OH)3Precipitating completely, and excludes precipitating Fe(OH)3；
(6) acid solution is recycled: and then by step (5), treated that remaining acid solution introduces in evaporator, and mass concentration is added
It for 70% Tea Saponin aqueous solution, is heated to reflux, collects hydrochloric acid, it will be in the hydrochloric acid cycle bleeder to pickling tube that be collected into；
(7) it helps plating: metal component of the step (3) after pickling being put into and is helped in coating bath, quickening liquid uses zinc chloride and chlorine
Change ammonium to be mixed to form by the mass ratio of the material for 1:3, in metal component surface forming salt film；
(8) zinc-plated: through step (7), treated, and metal component is put into galvanized bath, and the zinc liquid ingredient in galvanized bath is nickel
0.018%, aluminium 0.005%, rare earth 0.003%, tin 0.001%, remaining is zinc, and the temperature of zinc liquid is maintained at 470 DEG C, when dipping
Between be 3 minutes, the off speed of metal component is 1 meter/min；
(9) cooling: after zinc-plated, metal component to be placed in cold rinse bank, the softened water using water temperature lower than 40 DEG C is cooling
Sizing；
(10) it chromium-free deactivation and cools down again.
Comparative example one:
A kind of zincincation of acid circulation, comprises the technical steps that:
(1) degreasing: metal component being stacked neatly, successively metal component is sling using driving and puts into service sink,
The aqueous solution for the ten phosphate dihydrate sodium and sodium metaphosphate that mass concentration is 5% is put into, wherein ten phosphate dihydrate sodium and sodium metaphosphate
The mass ratio of the material is 1:1, is stirred evenly, and water temperature is maintained at 45 DEG C, and the processing time is 1 hour；
(2) clean: by degreasing, treated that metal component is placed in flushing tank, and the NaCl for being 8% using mass concentration is molten
Liquid is rinsed the surface of metal component, and flushing speed is 10L/min；
(3) pickling: the metal component after flushing is put into pickling tube, and the mass concentration of hydrochloric acid is 23% in pickling tube, leaching
Steeping the time is 1 hour；
(4) it removes iron: after Chu Liwan is with the metal component of batch, the H that mass concentration is 28% is passed through into pickling tube2O2Water
Solution, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The mass ratio of the material of aqueous solution is 7:1；
(5) it to by the ammonium hydroxide that mass concentration is 25% is added in step (4) treated pickling tube, adjusts in pickling tube
The pH of mixed solution is 3, is stood, so that Fe(OH)3Precipitating completely, and excludes precipitating Fe(OH)3；
(6) acid solution is recycled: and then by step (5), treated that remaining acid solution introduces in evaporator, is heated to reflux, collects salt
Acid, will be in the hydrochloric acid cycle bleeder to pickling tube that be collected into；
(7) it helps plating: metal component of the step (3) after pickling being put into and is helped in coating bath, quickening liquid uses zinc chloride and chlorine
Change ammonium to be mixed to form by the mass ratio of the material for 1:2, on the surface of the metal member forming salt film；
(8) zinc-plated: through step (7), treated, and metal component is put into galvanized bath, and the zinc liquid ingredient in galvanized bath is nickel
0.018%, aluminium 0.005%, rare earth 0.003%, tin 0.001%, remaining is zinc, and the temperature of zinc liquid is maintained at 450 DEG C, when dipping
Between be 3 minutes, the off speed of metal component is 1 meter/min；
(9) cooling: after zinc-plated, metal component to be placed in cold rinse bank, the softened water using water temperature lower than 40 DEG C is cooling
Sizing；
(10) it chromium-free deactivation and cools down again.
Comparative example two:
A kind of zincincation of acid circulation, comprises the technical steps that:
(1) degreasing: metal component being stacked neatly, successively metal component is sling using driving and puts into service sink,
The aqueous solution for the ten phosphate dihydrate sodium and sodium metaphosphate that mass concentration is 5% is put into, wherein ten phosphate dihydrate sodium and sodium metaphosphate
The mass ratio of the material is 1:1, is stirred evenly, and water temperature is maintained at 45 DEG C, and the processing time is 1 hour；
(2) clean: by degreasing, treated that metal component is placed in flushing tank, and the NaCl for being 5% using mass concentration is molten
Liquid is rinsed the surface of metal component, and flushing speed is 20L/min；
(3) pickling: the metal component after flushing is put into pickling tube, and the mass concentration of hydrochloric acid is 25% in pickling tube, leaching
Steeping the time is 1 hour；
(4) it removes iron: after Chu Liwan is with the metal component of batch, the H that mass concentration is 28% is passed through into pickling tube2O2Water
Solution, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The mass ratio of the material of aqueous solution is 8:1；
(5) it to by the ammonium hydroxide that mass concentration is 25% is added in step (4) treated pickling tube, adjusts in pickling tube
The pH of mixed solution is 3.5, is stood, so that Fe(OH)3Precipitating completely, and excludes precipitating Fe(OH)3；
(6) acid solution is recycled: and then by step (5), treated that remaining acid solution introduces in evaporator, is heated to reflux, collects salt
Acid, will be in the hydrochloric acid cycle bleeder to pickling tube that be collected into；
(7) it helps plating: metal component of the step (3) after pickling being put into and is helped in coating bath, quickening liquid uses zinc chloride and chlorine
Change ammonium to be mixed to form by the mass ratio of the material for 1:2, on the surface of the metal member forming salt film；
(8) zinc-plated: through step (7), treated, and metal component is put into galvanized bath, and the zinc liquid ingredient in galvanized bath is nickel
0.018%, aluminium 0.005%, rare earth 0.003%, tin 0.001%, remaining is zinc, and the temperature of zinc liquid is maintained at 450 DEG C, when dipping
Between be 3 minutes, the off speed of metal component is 1 meter/min；
(9) cooling: after zinc-plated, metal component to be placed in cold rinse bank, the softened water using water temperature lower than 40 DEG C is cooling
Sizing；
(10) it chromium-free deactivation and cools down again.
Comparative example three:
A kind of zincincation of acid circulation, comprises the technical steps that:
(1) degreasing: metal component being stacked neatly, successively metal component is sling using driving and puts into service sink,
The ten phosphate dihydrate sodium that mass concentration is 5% are put into, are stirred evenly, water temperature is maintained at 45 DEG C, and the processing time is 1 hour；
(2) clean: by degreasing, treated that metal component is placed in flushing tank, and the NaCl for being 8% using mass concentration is molten
Liquid is rinsed the surface of metal component, and flushing speed is 10L/min；
(3) pickling: the metal component after flushing is put into pickling tube, and the mass concentration of hydrochloric acid is 23% in pickling tube, leaching
Steeping the time is 1 hour；
(4) it removes iron: after Chu Liwan is with the metal component of batch, the H that mass concentration is 30% is passed through into pickling tube2O2Water
Solution, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The mass ratio of the material of aqueous solution is 6:1；
(5) it to by the ammonium hydroxide that mass concentration is 25% is added in step (4) treated pickling tube, adjusts in pickling tube
The pH of mixed solution is 3.5, is stood, so that Fe(OH)3Precipitating completely, and excludes precipitating Fe(OH)3；
(6) acid solution is recycled: and then by step (5), treated that remaining acid solution introduces in evaporator, and mass concentration is added
It for 50% Tea Saponin aqueous solution, is heated to reflux, collects hydrochloric acid, it will be in the hydrochloric acid cycle bleeder to pickling tube that be collected into；
(7) it helps plating: metal component of the step (3) after pickling being put into and is helped in coating bath, quickening liquid uses zinc chloride and chlorine
Change ammonium to be mixed to form by the mass ratio of the material for 1:2, in metal component surface forming salt film；
(8) zinc-plated: through step (7), treated, and metal component is put into galvanized bath, and the zinc liquid ingredient in galvanized bath is nickel
0.018%, aluminium 0.005%, rare earth 0.003%, tin 0.001%, remaining is zinc, and the temperature of zinc liquid is maintained at 450 DEG C, when dipping
Between be 3 minutes, the off speed of metal component is 1.8 meters/min；
(9) cooling: after zinc-plated, metal component to be placed in cold rinse bank, the softened water using water temperature lower than 40 DEG C is cooling
Sizing；
(10) it chromium-free deactivation and cools down again.
Comparative example four:
A kind of zincincation of acid circulation, comprises the technical steps that:
(1) degreasing: metal component being stacked neatly, successively metal component is sling using driving and puts into service sink,
The aqueous solution for putting into the sodium metaphosphate that mass concentration is 5%, stirs evenly, and water temperature is maintained at 45 DEG C, and the processing time is 1 hour；
(2) clean: by degreasing, treated that metal component is placed in flushing tank, and the NaCl for being 8% using mass concentration is molten
Liquid is rinsed the surface of metal component, and flushing speed is 10L/min；
(3) pickling: the metal component after flushing is put into pickling tube, and the mass concentration of hydrochloric acid is 23% in pickling tube, leaching
Steeping the time is 1 hour；
(4) it removes iron: after Chu Liwan is with the metal component of batch, the H that mass concentration is 28% is passed through into pickling tube2O2Water
Solution, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The mass ratio of the material of aqueous solution is 7:1；
(5) it to by the ammonium hydroxide that mass concentration is 25% is added in step (4) treated pickling tube, adjusts in pickling tube
The pH of mixed solution is 3.5, is stood, so that Fe(OH)3Precipitating completely, and excludes precipitating Fe(OH)3；
(6) acid solution is recycled: and then by step (5), treated that remaining acid solution introduces in evaporator, and mass concentration is added
It for 70% Tea Saponin aqueous solution, is heated to reflux, collects hydrochloric acid, it will be in the hydrochloric acid cycle bleeder to pickling tube that be collected into；
(7) it helps plating: metal component of the step (3) after pickling being put into and is helped in coating bath, quickening liquid uses zinc chloride and chlorine
Change ammonium to be mixed to form by the mass ratio of the material for 1:3, in metal component surface forming salt film；
(8) zinc-plated: through step (7), treated, and metal component is put into galvanized bath, and the zinc liquid ingredient in galvanized bath is nickel
0.018%, aluminium 0.005%, rare earth 0.003%, tin 0.001%, remaining is zinc, and the temperature of zinc liquid is maintained at 450 DEG C, when dipping
Between be 3 minutes, the off speed of metal component is 1 meter/min；
(9) cooling: after zinc-plated, metal component to be placed in cold rinse bank, the softened water using water temperature lower than 40 DEG C is cooling
Sizing；
(10) it chromium-free deactivation and cools down again.
Detection means:
1, ammonia radical ion overflows in evaporation process: placing filter screen in evaporator, is tried on filter screen using red reindeer moss
Paper winding, observes the discoloration of filter screen litmus paper.
2, the adhesive force of zinc coat: being tested 90 degree of product bending with flat-nose pliers, sample visual inspection folding after observation test
Coating dropping situations inside and outside curved.
The discoloration testing result of litmus paper is as shown in the table:
| Sample | Discoloration |
| Embodiment one | It is red |
| Embodiment two | It is red |
| Embodiment three | It is red |
| Comparative example one | Red, blue |
| Comparative example two | Red, blue |
By upper table it is found that Tea Saponin aqueous solution is not added in (6) the step of comparative example one, comparative example two, compared to reality
For applying example, occurs blue on litmus paper, show that acid solution generates ammonia in evaporation process, so Tea Saponin aqueous solution is to acid
Liquid plays the role of stabilization, has and ammonium chloride is inhibited to thermally decompose in thermal histories.
The testing result of adhesive force is as shown in the table:
| Sample | Dropping situations |
| Embodiment one | Coating is without falling off |
| Embodiment two | Coating is without falling off |
| Embodiment three | Coating is without falling off |
| Comparative example one | Coating falls off |
| Comparative example two | Coating falls off |
By upper table it is found that coating and is used alone ten in comparative example one, comparative example two without falling off in the sample of embodiment
The aqueous solution of phosphate dihydrate sodium or sodium metaphosphate shows as alkaline degreasing agent, generation coating obscission using 12
The mixed solution of water sodium phosphate and sodium metaphosphate is conducive to enhance the binding force between zinc coat and metal component.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art
Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this
All by the protection of Patent Law in the scope of the claims of invention.
Claims (6)
1. a kind of zincincation of acid circulation, it is characterised in that comprise the technical steps that:
(1) degreasing: metal component is stacked neatly, successively metal component is sling using driving and is put into service sink, is put into
The alkaline degreasing agent that mass concentration is 5~10%, cleans the oil substances of metal component surface, water temperature is maintained at 45
~50 DEG C, the processing time is 0.5~1 hour, and the alkalinity degreasing agent is the ten phosphate dihydrate sodium and metaphosphoric acid that mass ratio is 1:1
The mixture of sodium；
(2) clean: by degreasing, treated that metal component is placed in flushing tank, the NaCl for being 5~10% using mass concentration
Solution is rinsed the surface of metal component；
(3) pickling: the metal component after flushing is put into pickling tube, and the mass concentration of hydrochloric acid is 23~25% in pickling tube,
Soaking time is 1~1.5 hour；
(4) it aoxidizes: after Chu Liwan is with the metal component of batch, the H that mass concentration is 28~32% is passed through into pickling tube2O2
Aqueous solution, by Fe2+It is oxidized to Fe3+；
(5) it removes iron: to by the ammonium hydroxide that mass concentration is 25~28% is added in step (4) treated pickling tube, standing, make
It obtains Fe (OH)3Precipitating completely, and excludes precipitating Fe (OH)3；
(6) acid solution is recycled: and then by step (5), treated that remaining acid solution introduces in evaporator, and it is 60 that mass concentration, which is added,
~70% Tea Saponin, is heated to reflux, and heating temperature is to 100~110 DEG C, so that the hydrogen chloride in remaining acid solution volatilizees completely,
Hydrochloric acid is collected, it will be in the hydrochloric acid cycle bleeder to pickling tube that be collected into；
(7) it helps plating: metal component of the step (3) after pickling being put into and is helped in coating bath, quickening liquid uses zinc chloride and ammonium chloride
Solution is mixed to form, in metal component surface forming salt film；
(8) zinc-plated: through step (7), treated, and metal component is put into galvanized bath, and the zinc liquid ingredient in galvanized bath is nickel 0.018
~0.03%, aluminium 0.005~0.008%, rare earth 0.003~0.005%, tin 0.001%, remaining is zinc, and the temperature of zinc liquid is protected
It holds between 450~510 DEG C, dip time is 1~5 minute；
(9) cooling: after zinc-plated, metal component being placed in cold rinse bank, 40 DEG C of softened water cooling and shaping is lower than using water temperature；
(10) it chromium-free deactivation and cools down again.
2. a kind of zincincation of acid circulation according to claim 1, it is characterised in that: it is molten to limit NaCl in step (2)
The flushing speed of liquid is 10~20L/min.
3. a kind of zincincation of acid circulation according to claim 1, it is characterised in that: hydrochloric acid and H in step (4)2O2Water
The mass ratio of the material of solution is 6~8:1.
4. a kind of zincincation of acid circulation according to claim 1, it is characterised in that: adjust pickling tube in step (5)
The pH of interior mixed solution is 3~3.5.
5. a kind of zincincation of acid circulation according to claim 1, it is characterised in that: chlorine in the quickening liquid of step (7)
The mass ratio of the material for changing zinc and ammonium chloride is 1:2~3.
6. a kind of zincincation of acid circulation according to claim 1, it is characterised in that: metal component in step (8)
Off speed is 1~1.5 meter/min.
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| CN108950445A (en) * | 2018-06-29 | 2018-12-07 | 柳州市横阳机械有限公司 | A kind of wire galvanization method |
| CN115247248A (en) * | 2021-12-10 | 2022-10-28 | 徐州瑞马智能技术有限公司 | Hot galvanizing automatic treatment process based on online detection system |
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