CN107513682A - A kind of zincincation of acid circulation - Google Patents
A kind of zincincation of acid circulation Download PDFInfo
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- CN107513682A CN107513682A CN201710730586.0A CN201710730586A CN107513682A CN 107513682 A CN107513682 A CN 107513682A CN 201710730586 A CN201710730586 A CN 201710730586A CN 107513682 A CN107513682 A CN 107513682A
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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
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Abstract
The invention discloses a kind of zincincation of acid circulation, its drip irrigation device is to comprise the technical steps that：（1）Degreasing；（2）Cleaning；（3）Pickling；（4）Oxidation；（5）Iron removaling；（6）Reclaim acid solution；（7）Help plating；（8）It is zinc-plated；（9）Cooling；（10）Chromium-free deactivation and cool down again, after iron removal step, the Tea Saponin aqueous solution is put into pickling tube, the Tea Saponin aqueous solution plays stabilization to aqueous ammonium chloride solution, be advantageous to ammonia radical ion stably in aqueous ammonium chloride solution to exist, purer hydrogen chloride is evaporated so as to be advantageous to hydrochloric acid, so as to improve the cyclic utilization rate of hydrochloric acid.
Description
Technical field
The present invention relates to chemical field, more particularly to a kind of zincincation of acid circulation.
Background technology
In recent years, as high voltage power transmission, traffic, communication career develop rapidly, to steel and iron parts requirement of shelter more and more higher, heat
Zinc-plated demand is also continuously increased.Galvanizing is that zinc ingot metal is melted at high temperature, then adds some auxiliary materials, metal structure
Part is immersed in galvanizing bath, adheres to one layer of galvanized alloy layer in metal component surface.The thickness of usual cold galvanizing layer is 5 ~ 15 μm, and
Hot galvanized layer is typically more than 35 μm, 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.
At present, application publication number is that CN106868438A Chinese patent discloses a kind of steel structure galvanizer in existing patent
Skill, its processing step include：1）Supplied materials pre-processes；2）Washing；3）Pickling；4）Washing；5）Soak plating assistant solvent；6）Drying；7）Steel
Structure is zinc-plated；8）Cooling；9）Medicine；10）Cleaning；11）Polishing；12）Examine；The processing step is simple, efficiently solves unplated piece
The zinc-plated rear surface blackening of steel structure, there is the problem of piebald.
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, contain substantial amounts of iron ion after pickling in remaining acid solution, be not suitable for recycle, the processing of spent acid
Problem is the problem that those skilled in the art urgently captures at this stage.
The content of the invention
It is an object of the invention to provide a kind of zincincation of acid circulation, the zincincation solves the difficulty of spent acid processing
Topic, hydrochloric acid is recycled, significantly reduce the cost of galvanizing process.
The present invention above-mentioned technical purpose technical scheme is that：
A kind of zincincation of acid circulation, is comprised the technical steps that：
（1）Degreasing：Hardware is stacked neatly, hardware is sling and put into service sink successively using driving, is put into
Mass concentration is 5 ~ 10% alkaline degreasing agent, and the oil substances of metal component surface are cleaned, water temperature is maintained at 45 ~
50 DEG C, processing time is 0.5 ~ 1 hour；
（2）Cleaning：Hardware after degreasing is handled is placed in flushing tank, molten using the NaCl that mass concentration is 5 ~ 10%
Liquid is rinsed to the surface of hardware；
（3）Pickling：Hardware after flushing is put into pickling tube, the mass concentration of hydrochloric acid is 23 ~ 25% in pickling tube, leaching
It is 1 ~ 1.5 hour to steep the time；
（4）Oxidation：After Chu Liwan is with the hardware of batch, the H that mass concentration is 28 ~ 32% is passed through into pickling tube2O2Water
Solution, by Fe2+It is oxidized to Fe3+；
（5）Iron removaling：To by step（4）The ammoniacal liquor that mass concentration is 25 ~ 28% is added in pickling tube after processing, is stood so that
Fe（OH）3Precipitation is complete, and excludes to precipitate Fe（OH）3；
（6）Reclaim acid solution：Then by step（5）Remaining acid solution after processing is introduced in evaporator, and add mass concentration for 60 ~
70% Tea Saponin, is heated to reflux, and hydrochloric acid is collected, by hydrochloric acid cycle bleeder to the pickling tube being collected into；
（7）Help plating：By step（3）Hardware after pickling, which is put into, to be helped in coating bath, and quickening liquid uses zinc chloride and ammonium chloride
Solution is mixed to form, in metal component surface forming salt film；
（8）It is zinc-plated：Through step（7）Hardware after processing is put into galvanized bath, and the zinc liquid composition 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
Hold between 450 ~ 510 DEG C, dip time is 1 ~ 5 minute；
（9）Cooling：After zinc-plated, hardware is placed in cold rinse bank, 40 DEG C of softened water cooling and shaping is less than using water temperature；
（10）Chromium-free deactivation and cool down again.
By using above-mentioned technical proposal, zincincation includes degreasing, cleaning, pickling, iron removaling, helps plating, be zinc-plated and cold
But the process, be passivated, cooled down again, after iron removal step, the Tea Saponin aqueous solution, the Tea Saponin aqueous solution pair are put into pickling tube
Aqueous ammonium chloride solution plays stabilization, is advantageous to ammonia radical ion and stably exists in aqueous ammonium chloride solution, so as to be advantageous to
Hydrochloric acid evaporates purer hydrogen chloride, so as to improve the cyclic utilization rate of hydrochloric acid.
The present invention is further arranged to：The alkaline degreasing agent is that mass ratio is 1：10 phosphate dihydrate sodium and metaphosphoric acid
The mixture of sodium.
By using above-mentioned technical proposal, ten phosphate dihydrate sodium are colourless or white crystals, are dissolved in water, and the aqueous solution is in highly basic
Property, insoluble in ethanol, carbon disulfide, play quality-improving in food processing, for example have in meat products and keep holding for meat
Water-based, enhancement is knotted the effect such as power, reduces the loss of nutritional ingredient in meat, keeps the tenderness of meat；Breast is also served as in food
Agent, nutritional supplement, quality improver, it is the raw material 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, easy moisture absorption in atmosphere, it is anti-in alkalescence to be dissolved in water
Should, insoluble in ethanol；By ten phosphate dihydrate sodium and sodium metaphosphate compounding use, the infiltration on metal component surface is enhanced
Property, so as to improve the degreasing ability to metal component surface；Meanwhile also improve the combination of zinc coat and metal component surface
Power.
The present invention is further arranged to：Step（2）The middle flushing speed for limiting NaCl solution is 10 ~ 20L/min.
By using above-mentioned technical proposal, when the flushing speed of NaCl solution is less than 10L/min, to metal component surface
Impulsive 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 impulsive 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
Beneficial to the maintenance to workshop condition.
The present invention is further arranged to：Step（4）Middle hydrochloric acid and H2O2The amount ratio of the material of the aqueous solution is 6 ~ 8：1.
By using above-mentioned technical proposal, H2O2The aqueous solution has stronger oxidisability, by the Fe in pickling tube2+It is oxidized to
Fe3+, 1molH2O2The aqueous solution can aoxidize 2mol Fe2+, 6molHCl can handle 1molFe2O3（Iron rust）, so setting salt
Acid and H2O2The amount ratio of the material of the aqueous solution is 6：1, for the iron rust on metal component surface is removed completely, hydrochloric acid is excessive, but
To save cost, content of hydrochloric acid is not easy excessively, hydrochloric acid and H2O2The amount proportioning of the optimal material of the aqueous solution is 6 ~ 8：1.
The present invention is further arranged to：Step（5）The pH of mixed solution is 3 ~ 3.5 in middle regulation pickling tube.
By using above-mentioned technical proposal, after adding the ammoniacal liquor that mass concentration is 25 ~ 28%, the Fe in pickling tube3+It can occur
Precipitation, when pH is between 3 ~ 3.5, Fe can be promoted3+Precipitation, be advantageous in hydrochloric acid quickly discharge Fe3+。
The present invention is further arranged to：Step（6）Middle heating-up temperature is to 100 ~ 110 DEG C so that the chlorination in remaining acid solution
Hydrogen volatilizees completely.
By using above-mentioned technical proposal, control heating-up temperature is at 100 ~ 110 DEG C, and the hydrogen chloride gas in hydrochloric acid is in the temperature
It can be volatilized away as much as possible within degree scope, so as to improve the organic efficiency to hydrochloric acid.
The present invention is further arranged to：Step（7）Quickening liquid in the material of zinc chloride and ammonium chloride amount ratio be 1：2~
3。
By using above-mentioned technical proposal, ammonium chloride helps plating positive effect, but decomposition temperature is relatively low, and mistake is easily decomposed when heated
Effect, therefore the drying temperature of hardware quickening liquid is no more than 140 DEG C；In addition, the ammonium chloride that metal component surface is helped in plating salt film
Larger flue dust can also be caused；Zinc chloride easily makes moist, but better heat stability, and generation flue dust is less when soaking zinc, by zinc chloride
Generation synergy is mixed with ammonium chloride, is advantageous to improve and plating effect is helped to metal component surface.
The present invention is further arranged to：Step（8）The off speed of middle hardware is 1 ~ 1.5 meter/min.
By using above-mentioned technical proposal, after zinc-plated process, limit the off speed of hardware as 1 ~ 1.5 meter/
Min, it is in slow removal galvanized bath after zinc-plated to show hardware, reduces the shadow to metal component surface zinc coat compactness
Ring.
In summary, the invention has the advantages that：
1st, after iron removaling embroidery art's sequence, the Tea Saponin that mass concentration is 60 ~ 70%, Tea Saponin enhancing are added into remaining acid solution
The stability of ammonium chloride, during being heated to reflux, reduces the thermal decomposition of ammonium chloride, improves to hydrogen chloride in acid solution
Organic efficiency；
2nd, after the processing of parlkaline degreasing agent degreasing, the surface of hardware is rinsed using NaCl solution, is advantageous to
Improve the compactness of metal component surface；
3rd, alkaline degreasing agent is mixed using ten phosphate dihydrate sodium and sodium metaphosphate, improves the infiltration on metal component surface
Property, so as to improve the degreasing ability to metal component surface, meanwhile, also improve the combination of zinc coat and metal component surface
Power；
4th, in Fe3+In precipitation process, regulation pH is 3 ~ 3.5, is advantageous to quickly discharge Fe in hydrochloric acid3+。
Embodiment
The present invention is described in further detail with reference to embodiments.
Embodiment one：
A kind of zincincation of acid circulation, is comprised the technical steps that：
（1）Degreasing：Hardware is stacked neatly, hardware is sling and put into service sink successively using driving, is put into
Mass concentration is 5% ten phosphate dihydrate sodium and the aqueous solution of sodium metaphosphate, wherein the material of ten phosphate dihydrate sodium and sodium metaphosphate
Amount ratio be 1：1, stir, water temperature is maintained at 45 DEG C, and processing time is 1 hour；
（2）Cleaning：Hardware after degreasing is handled is placed in flushing tank, utilizes the NaCl solution pair that mass concentration is 8%
The surface of hardware is rinsed, and flushing speed is 10L/min；
（3）Pickling：Hardware after flushing is put into pickling tube, the mass concentration of hydrochloric acid is 23% in pickling tube, during immersion
Between be 1 hour；
（4）Iron removaling：After Chu Liwan is with the hardware of batch, the H that mass concentration is 28% is passed through into pickling tube2O2It is water-soluble
Liquid, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The amount ratio of the material of the aqueous solution is 7：1；
（5）To by step（4）The ammoniacal liquor that mass concentration is 25% is added in pickling tube after processing, is mixed in regulation pickling tube
The pH of solution is 3.5, is stood so that Fe（OH）3Precipitation is complete, and excludes to precipitate Fe（OH）3；
（6）Reclaim acid solution：Then by step（5）Remaining acid solution after processing is introduced in evaporator, and adds mass concentration as 60%
The Tea Saponin aqueous solution, be heated to reflux, collect hydrochloric acid, by hydrochloric acid cycle bleeder to the pickling tube being collected into；
（7）Help plating：By step（3）Hardware after pickling, which is put into, to be helped in coating bath, and quickening liquid uses zinc chloride and ammonium chloride
It is 1 by the amount ratio of material：2 are mixed to form, in metal component surface forming salt film；
（8）It is zinc-plated：Through step（7）Hardware after processing is put into galvanized bath, and the zinc liquid composition in galvanized bath is nickel
0.018%th, 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, during dipping
Between be 3 minutes, the off speed of hardware is 1 meter/min；
（9）Cooling：After zinc-plated, hardware is placed in cold rinse bank, 40 DEG C of softened water cooling and shaping is less than using water temperature；
（10）Chromium-free deactivation and cool down again.
Embodiment two：
A kind of zincincation of acid circulation, is comprised the technical steps that：
（1）Degreasing：Hardware is stacked neatly, hardware is sling and put into service sink successively using driving, is put into
Mass concentration is 8% ten phosphate dihydrate sodium and the aqueous solution of sodium metaphosphate, wherein the material of ten phosphate dihydrate sodium and sodium metaphosphate
Amount ratio be 1：1, stir, water temperature is maintained at 45 DEG C, and processing time is 1 hour；
（2）Cleaning：Hardware after degreasing is handled is placed in flushing tank, utilizes the NaCl solution that mass concentration is 10%
The surface of hardware is rinsed, flushing speed is 15L/min；
（3）Pickling：Hardware after flushing is put into pickling tube, the mass concentration of hydrochloric acid is 25% in pickling tube, during immersion
Between be 1 hour；
（4）Iron removaling：After Chu Liwan is with the hardware of batch, the H that mass concentration is 30% is passed through into pickling tube2O2It is water-soluble
Liquid, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The amount ratio of the material of the aqueous solution is 7：1；
（5）To by step（4）The ammoniacal liquor that mass concentration is 25% is added in pickling tube after processing, is mixed in regulation pickling tube
The pH of solution is 3.2, is stood so that Fe（OH）3Precipitation is complete, and excludes to precipitate Fe（OH）3；
（6）Reclaim acid solution：Then by step（5）Remaining acid solution after processing is introduced in evaporator, and adds mass concentration as 65%
The Tea Saponin aqueous solution, be heated to reflux, collect hydrochloric acid, by hydrochloric acid cycle bleeder to the pickling tube being collected into；
（7）Help plating：By step（3）Hardware after pickling, which is put into, to be helped in coating bath, and quickening liquid uses zinc chloride and ammonium chloride
It is 1 by the amount ratio of material：3 are mixed to form, in metal component surface forming salt film；
（8）It is zinc-plated：Through step（7）Hardware after processing is put into galvanized bath, and the zinc liquid composition in galvanized bath is nickel
0.018%th, 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, during dipping
Between be 3 minutes, the off speed of hardware is 1 meter/min；
（9）Cooling：After zinc-plated, hardware is placed in cold rinse bank, 40 DEG C of softened water cooling and shaping is less than using water temperature；
（10）Chromium-free deactivation and cool down again.
Embodiment three：
A kind of zincincation of acid circulation, is comprised the technical steps that：
（1）Degreasing：Hardware is stacked neatly, hardware is sling and put into service sink successively using driving, is put into
Mass concentration is 10% ten phosphate dihydrate sodium and the aqueous solution of sodium metaphosphate, wherein the thing of ten phosphate dihydrate sodium and sodium metaphosphate
The amount ratio of matter is 1：1, stir, water temperature is maintained at 45 DEG C, and processing time is 1 hour；
（2）Cleaning：Hardware after degreasing is handled is placed in flushing tank, utilizes the NaCl solution that mass concentration is 10%
The surface of hardware is rinsed, flushing speed is 20L/min；
（3）Pickling：Hardware after flushing is put into pickling tube, the mass concentration of hydrochloric acid is 25% in pickling tube, during immersion
Between be 1 hour；
（4）Iron removaling：After Chu Liwan is with the hardware of batch, the H that mass concentration is 30% is passed through into pickling tube2O2It is water-soluble
Liquid, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The amount ratio of the material of the aqueous solution is 8：1；
（5）To by step（4）The ammoniacal liquor that mass concentration is 25% is added in pickling tube after processing, is mixed in regulation pickling tube
The pH of solution is 3.5, is stood so that Fe（OH）3Precipitation is complete, and excludes to precipitate Fe（OH）3；
（6）Reclaim acid solution：Then by step（5）Remaining acid solution after processing is introduced in evaporator, and adds mass concentration as 70%
The Tea Saponin aqueous solution, be heated to reflux, collect hydrochloric acid, by hydrochloric acid cycle bleeder to the pickling tube being collected into；
（7）Help plating：By step（3）Hardware after pickling, which is put into, to be helped in coating bath, and quickening liquid uses zinc chloride and ammonium chloride
It is 1 by the amount ratio of material：3 are mixed to form, in metal component surface forming salt film；
（8）It is zinc-plated：Through step（7）Hardware after processing is put into galvanized bath, and the zinc liquid composition in galvanized bath is nickel
0.018%th, 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, during dipping
Between be 3 minutes, the off speed of hardware is 1 meter/min；
（9）Cooling：After zinc-plated, hardware is placed in cold rinse bank, 40 DEG C of softened water cooling and shaping is less than using water temperature；
（10）Chromium-free deactivation and cool down again.
Comparative example one：
A kind of zincincation of acid circulation, is comprised the technical steps that：
（1）Degreasing：Hardware is stacked neatly, hardware is sling and put into service sink successively using driving, is put into
Mass concentration is 5% ten phosphate dihydrate sodium and the aqueous solution of sodium metaphosphate, wherein the material of ten phosphate dihydrate sodium and sodium metaphosphate
Amount ratio be 1：1, stir, water temperature is maintained at 45 DEG C, and processing time is 1 hour；
（2）Cleaning：Hardware after degreasing is handled is placed in flushing tank, utilizes the NaCl solution pair that mass concentration is 8%
The surface of hardware is rinsed, and flushing speed is 10L/min；
（3）Pickling：Hardware after flushing is put into pickling tube, the mass concentration of hydrochloric acid is 23% in pickling tube, during immersion
Between be 1 hour；
（4）Iron removaling：After Chu Liwan is with the hardware of batch, the H that mass concentration is 28% is passed through into pickling tube2O2It is water-soluble
Liquid, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The amount ratio of the material of the aqueous solution is 7：1；
（5）To by step（4）The ammoniacal liquor that mass concentration is 25% is added in pickling tube after processing, is mixed in regulation pickling tube
The pH of solution is 3, is stood so that Fe（OH）3Precipitation is complete, and excludes to precipitate Fe（OH）3；
（6）Reclaim acid solution：Then by step（5）Remaining acid solution after processing is introduced in evaporator, is heated to reflux, and collects hydrochloric acid,
By in hydrochloric acid cycle bleeder to the pickling tube being collected into；
（7）Help plating：By step（3）Hardware after pickling, which is put into, to be helped in coating bath, and quickening liquid uses zinc chloride and ammonium chloride
It is 1 by the amount ratio of material：2 are mixed to form, in the surface forming salt film of hardware；
（8）It is zinc-plated：Through step（7）Hardware after processing is put into galvanized bath, and the zinc liquid composition in galvanized bath is nickel
0.018%th, 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, during dipping
Between be 3 minutes, the off speed of hardware is 1 meter/min；
（9）Cooling：After zinc-plated, hardware is placed in cold rinse bank, 40 DEG C of softened water cooling and shaping is less than using water temperature；
（10）Chromium-free deactivation and cool down again.
Comparative example two：
A kind of zincincation of acid circulation, is comprised the technical steps that：
（1）Degreasing：Hardware is stacked neatly, hardware is sling and put into service sink successively using driving, is put into
Mass concentration is 5% ten phosphate dihydrate sodium and the aqueous solution of sodium metaphosphate, wherein the material of ten phosphate dihydrate sodium and sodium metaphosphate
Amount ratio be 1：1, stir, water temperature is maintained at 45 DEG C, and processing time is 1 hour；
（2）Cleaning：Hardware after degreasing is handled is placed in flushing tank, utilizes the NaCl solution pair that mass concentration is 5%
The surface of hardware is rinsed, and flushing speed is 20L/min；
（3）Pickling：Hardware after flushing is put into pickling tube, the mass concentration of hydrochloric acid is 25% in pickling tube, during immersion
Between be 1 hour；
（4）Iron removaling：After Chu Liwan is with the hardware of batch, the H that mass concentration is 28% is passed through into pickling tube2O2It is water-soluble
Liquid, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The amount ratio of the material of the aqueous solution is 8：1；
（5）To by step（4）The ammoniacal liquor that mass concentration is 25% is added in pickling tube after processing, is mixed in regulation pickling tube
The pH of solution is 3.5, is stood so that Fe（OH）3Precipitation is complete, and excludes to precipitate Fe（OH）3；
（6）Reclaim acid solution：Then by step（5）Remaining acid solution after processing is introduced in evaporator, is heated to reflux, and collects hydrochloric acid,
By in hydrochloric acid cycle bleeder to the pickling tube being collected into；
（7）Help plating：By step（3）Hardware after pickling, which is put into, to be helped in coating bath, and quickening liquid uses zinc chloride and ammonium chloride
It is 1 by the amount ratio of material：2 are mixed to form, in the surface forming salt film of hardware；
（8）It is zinc-plated：Through step（7）Hardware after processing is put into galvanized bath, and the zinc liquid composition in galvanized bath is nickel
0.018%th, 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, during dipping
Between be 3 minutes, the off speed of hardware is 1 meter/min；
（9）Cooling：After zinc-plated, hardware is placed in cold rinse bank, 40 DEG C of softened water cooling and shaping is less than using water temperature；
（10）Chromium-free deactivation and cool down again.
Comparative example three：
A kind of zincincation of acid circulation, is comprised the technical steps that：
（1）Degreasing：Hardware is stacked neatly, hardware is sling and put into service sink successively using driving, is put into
Mass concentration is 5% ten phosphate dihydrate sodium, is stirred, and water temperature is maintained at 45 DEG C, and processing time is 1 hour；
（2）Cleaning：Hardware after degreasing is handled is placed in flushing tank, utilizes the NaCl solution pair that mass concentration is 8%
The surface of hardware is rinsed, and flushing speed is 10L/min；
（3）Pickling：Hardware after flushing is put into pickling tube, the mass concentration of hydrochloric acid is 23% in pickling tube, during immersion
Between be 1 hour；
（4）Iron removaling：After Chu Liwan is with the hardware of batch, the H that mass concentration is 30% is passed through into pickling tube2O2It is water-soluble
Liquid, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The amount ratio of the material of the aqueous solution is 6：1；
（5）To by step（4）The ammoniacal liquor that mass concentration is 25% is added in pickling tube after processing, is mixed in regulation pickling tube
The pH of solution is 3.5, is stood so that Fe（OH）3Precipitation is complete, and excludes to precipitate Fe（OH）3；
（6）Reclaim acid solution：Then by step（5）Remaining acid solution after processing is introduced in evaporator, and adds mass concentration as 50%
The Tea Saponin aqueous solution, be heated to reflux, collect hydrochloric acid, by hydrochloric acid cycle bleeder to the pickling tube being collected into；
（7）Help plating：By step（3）Hardware after pickling, which is put into, to be helped in coating bath, and quickening liquid uses zinc chloride and ammonium chloride
It is 1 by the amount ratio of material：2 are mixed to form, in metal component surface forming salt film；
（8）It is zinc-plated：Through step（7）Hardware after processing is put into galvanized bath, and the zinc liquid composition in galvanized bath is nickel
0.018%th, 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, during dipping
Between be 3 minutes, the off speed of hardware is 1.8 meters/min；
（9）Cooling：After zinc-plated, hardware is placed in cold rinse bank, 40 DEG C of softened water cooling and shaping is less than using water temperature；
（10）Chromium-free deactivation and cool down again.
Comparative example four：
A kind of zincincation of acid circulation, is comprised the technical steps that：
（1）Degreasing：Hardware is stacked neatly, hardware is sling and put into service sink successively using driving, is put into
Mass concentration is the aqueous solution of 5% sodium metaphosphate, is stirred, and water temperature is maintained at 45 DEG C, and processing time is 1 hour；
（2）Cleaning：Hardware after degreasing is handled is placed in flushing tank, utilizes the NaCl solution pair that mass concentration is 8%
The surface of hardware is rinsed, and flushing speed is 10L/min；
（3）Pickling：Hardware after flushing is put into pickling tube, the mass concentration of hydrochloric acid is 23% in pickling tube, during immersion
Between be 1 hour；
（4）Iron removaling：After Chu Liwan is with the hardware of batch, the H that mass concentration is 28% is passed through into pickling tube2O2It is water-soluble
Liquid, by Fe2+It is oxidized to Fe3+, wherein hydrochloric acid and H2O2The amount ratio of the material of the aqueous solution is 7：1；
（5）To by step（4）The ammoniacal liquor that mass concentration is 25% is added in pickling tube after processing, is mixed in regulation pickling tube
The pH of solution is 3.5, is stood so that Fe（OH）3Precipitation is complete, and excludes to precipitate Fe（OH）3；
（6）Reclaim acid solution：Then by step（5）Remaining acid solution after processing is introduced in evaporator, and adds mass concentration as 70%
The Tea Saponin aqueous solution, be heated to reflux, collect hydrochloric acid, by hydrochloric acid cycle bleeder to the pickling tube being collected into；
（7）Help plating：By step（3）Hardware after pickling, which is put into, to be helped in coating bath, and quickening liquid uses zinc chloride and ammonium chloride
It is 1 by the amount ratio of material：3 are mixed to form, in metal component surface forming salt film；
（8）It is zinc-plated：Through step（7）Hardware after processing is put into galvanized bath, and the zinc liquid composition in galvanized bath is nickel
0.018%th, 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, during dipping
Between be 3 minutes, the off speed of hardware is 1 meter/min；
（9）Cooling：After zinc-plated, hardware is placed in cold rinse bank, 40 DEG C of softened water cooling and shaping is less than using water temperature；
（10）Chromium-free deactivation and cool down again.
Detection means：
1st, ammonia radical ion overflows in evaporation process：Screen pack is placed in evaporator, is twined on screen pack using litmus red test paper
Around the discoloration of observation screen pack litmus paper.
2nd, the adhesive force of zinc coat：With flat-nose pliers by 90 degree of tests of product bending, 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, blueness |
| Comparative example two | Red, blueness |
By upper table, the step of comparative example one, comparative example two（6）In do not add the Tea Saponin aqueous solution, compared to embodiment
For, occur blueness on litmus paper, show that acid solution produces ammonia in evaporation process, so the Tea Saponin aqueous solution rises to acid solution
To stabilization, have the function that suppress ammonium chloride thermally decomposes in thermal histories.
The testing result of adhesive force is as shown in the table：
| Sample | Dropping situations |
| Embodiment one | Coating is without coming off |
| Embodiment two | Coating is without coming off |
| Embodiment three | Coating is without coming off |
| Comparative example one | Coating comes off |
| Comparative example two | Coating comes off |
By upper table, coating is without coming off in the sample of embodiment, and 12 water are used alone in comparative example one, comparative example two
The aqueous solution of sodium phosphate or sodium metaphosphate occurs coating obscission, shows to use 12 water phosphorus as alkaline degreasing agent
The mixed solution of sour sodium and sodium metaphosphate, be advantageous to strengthen the adhesion between zinc coat and hardware.
This specific embodiment is only explanation of the invention, and it is not limitation of the present invention, people in the art
Member can make the modification of no creative contribution to the present embodiment as needed after this specification is read, but as long as at this
All protected in the right of invention by Patent Law.
Claims (8)
1. a kind of zincincation of acid circulation, it is characterised in that comprise the technical steps that：
（1）Degreasing：Hardware is stacked neatly, hardware is sling and put into service sink successively using driving, is put into
Mass concentration is 5 ~ 10% alkaline degreasing agent, and the oil substances of metal component surface are cleaned, water temperature is maintained at 45 ~
50 DEG C, processing time is 0.5 ~ 1 hour；
（2）Cleaning：Hardware after degreasing is handled is placed in flushing tank, molten using the NaCl that mass concentration is 5 ~ 10%
Liquid is rinsed to the surface of hardware；
（3）Pickling：Hardware after flushing is put into pickling tube, the mass concentration of hydrochloric acid is 23 ~ 25% in pickling tube, leaching
It is 1 ~ 1.5 hour to steep the time；
（4）Oxidation：After Chu Liwan is with the hardware of batch, the H that mass concentration is 28 ~ 32% is passed through into pickling tube2O2Water
Solution, by Fe2+It is oxidized to Fe3+；
（5）Iron removaling：To by step（4）The ammoniacal liquor that mass concentration is 25 ~ 28% is added in pickling tube after processing, is stood so that
Fe（OH）3Precipitation is complete, and excludes to precipitate Fe（OH）3；
（6）Reclaim acid solution：Then by step（5）Remaining acid solution after processing is introduced in evaporator, and add mass concentration for 60 ~
70% Tea Saponin, is heated to reflux, and hydrochloric acid is collected, by hydrochloric acid cycle bleeder to the pickling tube being collected into；
（7）Help plating：By step（3）Hardware after pickling, which is put into, to be helped in coating bath, and quickening liquid uses zinc chloride and ammonium chloride
Solution is mixed to form, in metal component surface forming salt film；
（8）It is zinc-plated：Through step（7）Hardware after processing is put into galvanized bath, and the zinc liquid composition 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
Hold between 450 ~ 510 DEG C, dip time is 1 ~ 5 minute；
（9）Cooling：After zinc-plated, hardware is placed in cold rinse bank, 40 DEG C of softened water cooling and shaping is less than using water temperature；
（10）Chromium-free deactivation and cool down again.
A kind of 2. zincincation of acid circulation according to claim 1, it is characterised in that：The alkaline degreasing agent is quality
Than for 1：10 phosphate dihydrate sodium and the mixture of sodium metaphosphate.
A kind of 3. zincincation of acid circulation according to claim 1, it is characterised in that：Step（2）Middle restriction NaCl is molten
The flushing speed of liquid is 10 ~ 20L/min.
A kind of 4. zincincation of acid circulation according to claim 1, it is characterised in that：Step（4）Middle hydrochloric acid and H2O2Water
The amount ratio of the material of solution is 6 ~ 8：1.
A kind of 5. zincincation of acid circulation according to claim 1, it is characterised in that：Step（5）Middle regulation pickling tube
The pH of interior mixed solution is 3 ~ 3.5.
A kind of 6. zincincation of acid circulation according to claim 1, it is characterised in that：Step（6）Middle heating-up temperature is extremely
100 ~ 110 DEG C so that the hydrogen chloride in remaining acid solution volatilizees completely.
A kind of 7. zincincation of acid circulation according to claim 1, it is characterised in that：Step（7）Quickening liquid in chlorine
The amount ratio for changing the material of zinc and ammonium chloride is 1：2~3.
A kind of 8. zincincation of acid circulation according to claim 1, it is characterised in that：Step（8）Middle hardware
Off speed is 1 ~ 1.5 meter/min.
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| 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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