CN102965667A - Method for regenerating and recycling waste etching solution in stainless steel etching production line - Google Patents
Method for regenerating and recycling waste etching solution in stainless steel etching production line Download PDFInfo
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- CN102965667A CN102965667A CN2012105259920A CN201210525992A CN102965667A CN 102965667 A CN102965667 A CN 102965667A CN 2012105259920 A CN2012105259920 A CN 2012105259920A CN 201210525992 A CN201210525992 A CN 201210525992A CN 102965667 A CN102965667 A CN 102965667A
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- etching
- stainless steel
- etching waste
- waste liquor
- solution
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- 238000005530 etching Methods 0.000 title claims abstract description 123
- 239000002699 waste material Substances 0.000 title claims abstract description 72
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 35
- 239000010935 stainless steel Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000004064 recycling Methods 0.000 title abstract description 7
- 230000001172 regenerating effect Effects 0.000 title abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000011069 regeneration method Methods 0.000 claims abstract description 39
- 230000008929 regeneration Effects 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 20
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 12
- 239000012286 potassium permanganate Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 6
- 238000012423 maintenance Methods 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract description 6
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 239000007800 oxidant agent Substances 0.000 abstract 2
- 230000007774 longterm Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000009418 renovation Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
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Abstract
The invention provides a method for regenerating and recycling waste etching solution in a stainless steel etching production line. The method comprises the following steps in sequence: adding 1 to 15% of oxidant based on the weight of the waste solution to the waste etching solution or the circular flowing waste etching solution; adding 5 to 25% of technical hydrochloric acid based on the weight of the waste solution; and keeping the waste etching solution in stirring or circular flowing for some time, thus accomplishing the regeneration of the waste solution. According to the method, the oxidant is especially added at two to six times. The method is simple and easy for regenerating and recycling the waste etching stainless steel column. By adopting the method, the etching efficiency of the waste etching stainless steel solution can be recovered into a new liquid level, and the purposes of regenerating and recycling are realized; ferric trichloride is not added in the method; a cylinder is not needed to be replaced; and the method is high in regeneration speed, simple in operation and low in cost, and can realize the long-term recycling of the waste etching stainless steel solution.
Description
Technical field
The present invention relates to the method for stainless steel etching waste liquid regeneration, particularly the simple and easy method of the regeneration of acid ferric trichloride etching waste liquor in the stainless steel etched plate production process.
Background technology
The stainless steel etching technique is extensive application in stainless steel stamp, engraving.Acid iron trichloride etching solution is inexpensive because of it, corrosion stabilised efficiency and do not produce harmful and inflammable gas, is the first-selection in the stainless steel etched decorative plate production process for a long time always.In the solution of acid iron trichloride, the iron reaction in ferric iron and the stainless steel generates ferrous iron.Along with the carrying out of reaction, the ferric iron concentration in the etching solution constantly reduces, and ferrous iron concentration constantly raises, and redox potential constantly decays, the reduction of corrosion efficient.When potential decay to a certain degree, the etching solution corrosive effect can not satisfy the requirements such as stamp and engraving, just must shut down all waste liquids in the etching machine fluid cylinder are extracted out this moment, the etching solution that more renews can be proceeded to produce.Not only production efficiency is low for this batch production mode, and factory also needs to arrange a large amount of places to stack etching solution and etching waste liquor, and potential safety hazard is large.Stainless steel finishing material enterprise generally is by privately discharging or processed by modes such as the free recovery of production firm, causing environmental pollution and the wasting of resources to etching waste liquor.And existing renovation process (referring to patent CN02116014.7, CN200310120087.8, CN200810065306.X) complex process and cost height for etching solution are difficult to realize online updating, regeneration and recycle in industrial production.
The present invention is based on ferrous oxidizing reaction in the etching solution, adopting hydrogen peroxide, potassium permanganate and sodium chlorate is oxygenant, has realized the rapid regeneration of etching waste liquor.This method is simple and cost is low, is particularly suitable for using at stainless steel etching production line.
Summary of the invention
The object of the invention is to, providing a kind of can directly use on stainless steel etching production line, realizes the method for acid ferric trichloride etching waste liquor regeneration and recycle.
In view of the foregoing invention purpose, the present invention has adopted following technical scheme: the method for stainless steel etching production line etching waste liquid regeneration and recycle, the oxygenant that adds first waste liquid weight 1-15% in etching waste liquor or the etching waste liquor that circulates, the technical hydrochloric acid of rear adding waste liquid weight 5-25%, maintenance etching waste liquor stir or circulate for some time and namely finish the whole regenerative process of waste liquid.Especially add oxygenant by a small amount of mode repeatedly, add whole oxygenants in 2-6 time mode, each dosage can be roughly the same.
In this technical scheme, the regeneration temperature of stainless steel etching waste liquor is room temperature-50 ℃, and especially constant is 35-50 ℃; Preferably 40-50 ℃.Stainless steel etching waste liquor chief component is acid liquor ferri trichloridi, and degree Beaume is 40-44; The technical hydrochloric acid mass percent concentration is 30-37%.
Oxygenant is a kind of in hydrogen peroxide, potassium permanganate, the sodium chlorate; When using hydrogen peroxide as oxygenant, employed hydrogen peroxide be technical grade or chemical pure etc. all can, mass percent concentration is 30%, consumption is the 5-15% of etching waste liquor weight, the technical hydrochloric acid consumption is the 15-25% of etching waste liquor weight; When using potassium permanganate as oxygenant, employed potassium permanganate be technical grade or chemical pure etc. all can, consumption is the 1-5% of etching waste liquor weight, the technical hydrochloric acid consumption is the 5-25% of etching waste liquor weight; When using sodium chlorate as oxygenant, employed sodium chlorate be technical grade or chemical pure etc. all can, consumption is the 1-5% of etching waste liquor weight; The technical hydrochloric acid consumption especially is the 5-20% of etching waste liquor weight; After oxygenant and technical hydrochloric acid all add or add fashionablely, etching waste liquor stirs or time of keeping circulating is 5-15 minute.The addition of oxygenant of the present invention and technical hydrochloric acid mainly determines according to the mass loss situation of model after the redox potential of etching solution and the etching.When etch consumption is many, addition will be more.
The invention has the beneficial effects as follows: compared with prior art, the advantage of stainless steel etching waste liquid regeneration method of the present invention is:
1. technique is simple, can add online, can realize continuous production.Only need in the stainless steel etching waste liquor, add desired raw material, just can realize regenerating and recycling, avoid frequently changing cylinder, shorten the etched plate production cycle, improve production efficiency.
2. with low cost, cost performance is high.Regenerate 200 yuan of the cost less thaies of etching waste liquor per ton of the technology of the present invention, cost performance is high.
3. etch effect and the stoste of regeneration etching solution are suitable, and life cycle is prolonged.Under the same conditions, regeneration etching solution and the stoste of utilizing respectively embodiment of the invention 1-3 to obtain are carried out etching to 304 stainless steel plates with batch 900mm * 900mm, etching period 3min, 40 ℃ of etch temperature utilize weighting method and redox potential analytical method (ORP meter) to analyze the etch effect of different etching solutions after etching repeatedly.Can be found by Fig. 1, Fig. 2, the redox potential of regeneration etching solution surpasses stoste, repeatedly the mass loss of model still is higher than stoste after the etching, above result proves absolutely that the etch effect of the regeneration etching solution that utilizes method acquisition provided by the invention reaches the stoste level, and life cycle is longer than stoste.The present invention is the simple and easy method that the stainless steel etching waste liquid regeneration utilizes.Make the etching efficiency of stainless steel etching waste liquor return to new liquid level, reach the purpose of regeneration and recycle.Present method need not be added iron trichloride and need not be changed cylinder, and reproduction speed is fast, simple to operate, cost is low, can realize recycling for a long time of stainless steel etching solution.
Description of drawings
Fig. 1 is that mass loss is with the variation diagram of etching number of times.
Fig. 2 is that redox-potential is with the variation diagram of etching number of times.
Embodiment
Mode below by specific embodiment describes about the stainless steel etching solution regeneration method the present invention, but the present invention is not limited to these embodiment.
Under 40 ℃ of constant temperature, adding first the 100kg mass percent concentration in the 1000kg etching waste liquor that circulates by a small amount of mode repeatedly is 30% hydrogen peroxide, and then to add the 180kg mass percent concentration be the technical hydrochloric acid of 30-37%, keeps etching solution to circulate 10 minutes and can finish etching solution regeneration.
Under 35 ℃ of constant temperature, in the 1000kg etching waste liquor that circulates, add first 35kg potassium permanganate to all dissolvings by a small amount of mode repeatedly, and then to add the 170kg mass percent concentration be the technical hydrochloric acid of 30-37%, keeps etching solution to circulate 10 minutes and can finish etching solution regeneration.Chemical pure hydrochloric acid is certainly better.
Under 40 ℃ of constant temperature, in the 1000kg etching waste liquor, add first the 20kg sodium chlorate to all dissolvings by a small amount of mode repeatedly, and then to add the 120kg mass percent concentration be the technical hydrochloric acid of 30-37%, keeps etching solution to stir and can finish etching solution regeneration in 10 minutes.
Under 45 ℃ of constant temperature, adding first the 150kg mass percent concentration in the 1000kg etching waste liquor that circulates by a small amount of mode repeatedly is 30% hydrogen peroxide, and then to add the 230kg mass percent concentration be the technical hydrochloric acid of 30-37%, keeps etching solution to circulate 10 minutes and can finish etching solution regeneration.
Under 50 ℃ of constant temperature, in the 1000kg etching waste liquor that circulates, add first 15kg potassium permanganate to all dissolvings by a small amount of mode repeatedly, and then to add the 90kg mass percent concentration be the technical hydrochloric acid of 30-37%, keeps etching solution to circulate 5 minutes and can finish etching solution regeneration.
Under 45 ℃ of constant temperature, in the 1000kg etching waste liquor that circulates, add first the 40kg sodium chlorate to all dissolvings by a small amount of mode repeatedly, and then to add the 180kg mass percent concentration be the technical hydrochloric acid of 30-37%, keeps etching solution to circulate 15 minutes and can finish etching solution regeneration.
Under 50 ℃ of constant temperature, adding first the 75kg mass percent concentration in the 1000kg etching waste liquor that circulates by a small amount of mode repeatedly is 30% hydrogen peroxide, and then to add the 230kg mass percent concentration be the technical hydrochloric acid of 30-37%, keeps etching solution to circulate 5 minutes and can finish etching solution regeneration.
Under 45 ℃ of constant temperature, in the 1000kg etching waste liquor that circulates, add first 45kg potassium permanganate to all dissolvings by a small amount of mode repeatedly, and then to add the 240kg mass percent concentration be the technical hydrochloric acid of 30-37%, keeps etching solution to circulate 15 minutes and can finish etching solution regeneration.
Under 50 ℃ of constant temperature, in the 1000kg etching waste liquor that circulates, add first the 10kg sodium chlorate to all dissolvings by a small amount of mode repeatedly, and then to add the 70kg mass percent concentration be the technical hydrochloric acid of 30-37%, keeps etching solution to circulate 5 minutes and can finish etching solution regeneration.
Embodiment 10
Under 40 ℃ of conditions, to adding first the 15kg sodium chlorate in the 1000kg etching waste liquor, be stirred to whole dissolvings, and then adding 65kg mass percent concentration is the technical hydrochloric acid of 30-37%, keep to stir and to finish etching solution regeneration in 5 minutes, get final product reuse after leaving standstill filtration.When etch consumption was many, adding 50kg sodium chlorate and 250kg mass percent concentration was the technical hydrochloric acid of 30-37%.
Claims (9)
1. the method for a stainless steel etching production line etching waste liquid regeneration and recycle, it is characterized in that: the oxygenant that adds first waste liquid weight 1-15% in etching waste liquor or the etching waste liquor that circulates, the technical hydrochloric acid of rear adding waste liquid weight 5-25%, maintenance etching waste liquor stir or circulate for some time and namely finish spent solution regeneration.
2. the method for stainless steel etching production line etching waste liquid regeneration according to claim 1 and recycle, it is characterized in that: the mode by 2-6 time adds oxygenant.
3. the method for stainless steel etching production line etching waste liquid regeneration according to claim 1 and recycle, it is characterized in that: described stainless steel etching waste liquor major ingredient is acid liquor ferri trichloridi, and degree Beaume is 40-44.
4. the method for described stainless steel etching production line etching waste liquid regeneration and recycle one of according to claim 1-3 is characterized in that: described oxygenant is a kind of in hydrogen peroxide, potassium permanganate, the sodium chlorate.
5. the method for stainless steel etching production line etching waste liquid regeneration according to claim 4 and recycle, it is characterized in that: described hydrogen peroxide mass percent concentration is 30%, consumption is the 5-15% of etching waste liquor weight; Described potassium permanganate consumption is the 1-5% of etching waste liquor weight; Described sodium chlorate consumption is the 1-5% of etching waste liquor weight.
6. the method for stainless steel etching production line etching waste liquid regeneration according to claim 1 and recycle, it is characterized in that: described technical hydrochloric acid mass percent concentration is 30-37%; When using hydrogen peroxide as oxygenant, the hydrochloric acid consumption is the 15-25% of etching waste liquor weight; When using potassium permanganate as oxygenant, the hydrochloric acid consumption is the 5-25% of etching waste liquor weight; When using sodium chlorate as oxygenant, the hydrochloric acid consumption is the 5-20% of etching waste liquor weight.
7. the simple and easy method of stainless steel etching waste liquid regeneration according to claim 1 is characterized in that: after oxygenant and technical hydrochloric acid all added, the time that etching solution keeps circulating was 5-15 minute.
8. the simple and easy method of stainless steel etching waste liquid regeneration according to claim 1 is characterized in that: the treatment temp of etching solution is room temperature-50 ℃.
9. the simple and easy method of stainless steel etching waste liquid regeneration according to claim 8, it is characterized in that: the treatment temp of etching solution is 40-50 ℃; Described stainless steel etching waste liquor circulate online when regeneration homo(io)thermism at 40-50 ℃.
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| CN201210525992.0A CN102965667B (en) | 2012-12-10 | 2012-12-10 | Method for regenerating and recycling waste etching solution in stainless steel etching production line |
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| CN102965667B CN102965667B (en) | 2015-06-17 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710706A (en) * | 2013-12-24 | 2014-04-09 | 沈阳师范大学 | Purification and regeneration method of iron trichloride etching waste liquid |
| CN104087941A (en) * | 2014-07-17 | 2014-10-08 | 深圳市卓力达电子有限公司 | Etching method and equipment of etching stainless steel by ferric chloride |
| CN105018732A (en) * | 2015-07-01 | 2015-11-04 | 夏栋 | Novel method for comprehensive recovery of etching waste liquid and waste residues |
| CN110528006A (en) * | 2019-09-11 | 2019-12-03 | 上海八菱环保科技有限公司 | Automatic adding device, etching production line, adding method, control system, control method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462803A (en) * | 2009-01-04 | 2009-06-24 | 健鼎（无锡）电子有限公司 | Method for recovering etching waste liquor containing copper chloride and ferric trichloride |
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2012
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462803A (en) * | 2009-01-04 | 2009-06-24 | 健鼎（无锡）电子有限公司 | Method for recovering etching waste liquor containing copper chloride and ferric trichloride |
Non-Patent Citations (2)
| Title |
|---|
| 李维钢，等: "FeCl3腐蚀溶液再生应用的研究", 《天津化工》, no. 3, 30 June 1999 (1999-06-30), pages 31 - 32 * |
| 顾江楠，等: "三氯化铁溶液蚀刻不锈钢的研究", 《电镀与精饰》, vol. 10, no. 4, 31 August 1988 (1988-08-31), pages 6 - 9 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710706A (en) * | 2013-12-24 | 2014-04-09 | 沈阳师范大学 | Purification and regeneration method of iron trichloride etching waste liquid |
| CN103710706B (en) * | 2013-12-24 | 2015-12-02 | 沈阳师范大学 | The electrolysis method method of iron trichloride etching waste liquid |
| CN104087941A (en) * | 2014-07-17 | 2014-10-08 | 深圳市卓力达电子有限公司 | Etching method and equipment of etching stainless steel by ferric chloride |
| CN105018732A (en) * | 2015-07-01 | 2015-11-04 | 夏栋 | Novel method for comprehensive recovery of etching waste liquid and waste residues |
| CN110528006A (en) * | 2019-09-11 | 2019-12-03 | 上海八菱环保科技有限公司 | Automatic adding device, etching production line, adding method, control system, control method |
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