CN109267142A - A kind of PH stainless steel room temperature electrolytic pickling method - Google Patents
A kind of PH stainless steel room temperature electrolytic pickling method Download PDFInfo
- Publication number
- CN109267142A CN109267142A CN201811123266.XA CN201811123266A CN109267142A CN 109267142 A CN109267142 A CN 109267142A CN 201811123266 A CN201811123266 A CN 201811123266A CN 109267142 A CN109267142 A CN 109267142A
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- China
- Prior art keywords
- stainless steel
- room temperature
- pickling
- neutral salt
- ultrasonic cavitation
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Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
- C25F1/02—Pickling; Descaling
- C25F1/04—Pickling; Descaling in solution
- C25F1/06—Iron or steel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating
Abstract
A kind of PH stainless steel room temperature electrolytic pickling method.It includes the neutral salt electrolyte for preparing sulfur acid sodium, nitric acid and water；By in PH stainless steel dipped type salt electrolyte, ultrasonic cavitation processing is carried out using ultrasonic cavitation；Using PH stainless steel as anode, platinum electrode carries out neutral salt electrolysis pickling processes as cathode, to PH stainless steel；It is alternately repeated ultrasonic cavitation and cathodic pickling treatment process, until the surface non-scale residual of PH stainless steel and etc..PH stainless steel room temperature electrolytic pickling method provided by the invention can improve the surface quality after PH stainless steel cathodic pickling, improve stainless steel watch surface oxidized skin removal efficiency, production energy consumption and acid consumption is greatly reduced, realizes the efficient electrolysis pickling of stainless steel under room temperature.
Description
Technical field
The invention belongs to stainless steel surface processing technology fields, more particularly to a kind of PH stainless steel room temperature electricity
Solve acid washing method.
Background technique
In practical projects, enterprises of producing stainless steel all kinds of stainless steel products produced are machined such as by multiple tracks
Number vehicle after boring apical pore, often has complicated geometry.And it is being passed through with the PH stainless steel of complex geometric shapes
After crossing the heat treatment such as solid solution, timeliness, the oxide skin that stainless steel product surface generates under corresponding condition can cover securely very much
In product surface, and the defect of stainless steel surface can be covered and cause to be not easy to detect.
From the perspective of stainless steel product, if it is mechanical, blunt that these stainless steels after being heat-treated directly are sent to progress
The production and processings such as change can bring many problems: (1) stainless steel product will cause surface oxidation skin portion in subsequent mechanical processing
It falls off, leads between oxide skin and stainless steel base that there are anode and cathode potential differences, so that the surface quality for influencing stainless steel is special
It is corrosion resistance, or even will cause waste product；(2) oxide skin being crushed in subsequent mechanical processing process can enter lathe, to lead
It causes to be affected with the stainless steel product geometric accuracy of batch, or even will cause equipment damage；(3) when surface passivating treatment
The generation that stainless steel surface passivating film can be greatly influenced if there is oxide skin causes stainless steel product surface different parts blunt
The quality for changing film is different, greatly affected the corrosion resistance of stainless steel product.Therefore, PH stainless steel is being heat-treated
Afterwards, it is necessary to remove the oxide skin of its surface generation.
Existing scale removal mode is broadly divided into 3 kinds: (1) mechanical sandblasting；(2) multistage pickling；(3) cathodic pickling.
About above-mentioned first method: mechanical sandblasting, manufacturing enterprise using sandblasting carry out oxide skin removal when, due to
Some stainless steel products such as bolt often has complicated geometry, and stainless steel product surface often remains a small amount of oxygen
Change skin, the primary battery for forming " big cathode primary anode " with stainless steel base can accelerate the corrosion of stainless steel.
About above-mentioned second method: multistage pickling, the multistage pickling master of existing removal stainless steel watch surface oxidized skin
It will be by the way of sulfuric acid, nitric acid acidwashing and mixed acid pickling continuous operation.By taking patent KR2012-0075344 as an example, at this
In patent document, discloses and impregnate steel plate in the mixed acid containing hydrofluoric acid and the method for pickling, due to using mixed acid,
Therefore risk caused by being revealed there are hydrofluoric acid in mixed acid.Such as on January 27th, 2013, Samsung's chip factory's hydrofluoric acid
Leakage accident causes dead four people of a people injured.Therefore the mode of multistage pickling not only produces great prestige to production safety
The side of body, and the acid consumption of acid cleaning process is higher, substantially increases treatment cost of waste liquor.
About the third above-mentioned method: cathodic pickling, existing cathodic pickling is mostly in the higher situation of electrolyte temperature
Lower progress.For example a kind of high quality cold-rolling steel strip pickling work is disclosed in the Chinese patent literature of Publication No. CN106757296A
Skill, but when feeding cathodic pickling solution enters electrolysis, selected electrolysis temperature is 75 DEG C -80 DEG C.This cathodic pickling
Mode substantially increases production energy consumption cost, and the stability of production equipment at relatively high temperatures also have it is a degree of under
Drop.
Summary of the invention
To solve the above-mentioned problems, the purpose of the present invention is to provide a kind of PH stainless steel room temperature cathodic picklings
Method.
In order to achieve the above object, PH stainless steel room temperature electrolytic pickling method provided by the invention includes by suitable
The following steps that sequence carries out:
1) it prepares in a cell containing the neutral salt electricity that 100-150g/L sodium sulphate, 30-50g/L nitric acid and surplus are water
Solve medium of the liquid as ultrasonic cavitation and neutral salt electrolysis pickling；
2) PH stainless steel of surface to be processed with oxide skin is immersed in above-mentioned neutral salt electrolyte, so
Supersonic generator is opened afterwards and generates ultrasonic wave, and PH stainless steel is carried out at ultrasonic cavitation using ultrasonic cavitation
Reason；
3) supersonic generator is closed, using PH stainless steel as anode, platinum electrode is hard to precipitating as cathode
Change type stainless steel carries out neutral salt electrolysis pickling processes；
4) step 2)-step 3) is repeated, until the surface non-scale of PH stainless steel remains.
In step 2) and step 3), the temperature range of the neutral salt electrolyte is 25-35 DEG C.
In step 2), supersonic frequency used by the supersonic generator is 40kHz.
In step 3), whens described neutral salt electrolysis pickling processes, used current density was 6-10A/dm2。
In step 2) and step 3), the ultrasonic cavitation processing and neutral salt electrolysis pickling processes time are 2-
3min。
PH stainless steel room temperature electrolytic pickling method provided by the invention can improve PH stainless steel
Surface quality after cathodic pickling improves stainless steel watch surface oxidized skin removal efficiency, and production energy consumption and acid consumption is greatly reduced, realizes
The efficient electrolysis pickling of stainless steel under room temperature.
Specific embodiment
PH stainless steel room temperature electrolytic pickling method provided by the invention can not only remove precipitating at normal temperature
Oxide skin existing for hardened stainless steel surface, and can be avoided the disadvantage that traditional approach is at high cost, removal effect is undesirable.
The present invention selects sodium sulphate to carry out neutral salt electrolysis pickling as the neutral salt electrolyte of electrolyte.In above-mentioned
Property salt electrolyte in, sodium sulphate as in solution carry out charge transfer medium, concentration can be 100-150g/L.If its is dense
Degree is lower than 100g/L, then electric conductivity is low, therefore therefore pickling efficiency can reduce.When concentration is higher than 150g/L, electrolytic efficiency phase
Together, but it is limited to the raising of sodium sulphate solubility in water and production cost.Therefore the concentration of sodium sulphate is due to electric conductivity
And economy is restricted to the range of 100-150g/L.
In above-mentioned neutral salt electrolyte, nitric acid 30-50g/L need to be added.The reason is that can be generated in dissolution electrolytic process
Iron hydroxide flocculent deposit, these flocculent deposits can be attached to electrode surface, therefore can reduce the cathodic pickling efficiency of oxide skin.
When concentration is lower than 30g/L, then the dissolved efficiency of flocculent deposit is too low, and then influences the cathodic pickling efficiency of oxide skin.Work as nitre
When the concentration of acid is higher than 50g/L, the rate of dissolution of iron hydroxide flocculent deposit is identical, but will lead at the raising of acid consumption and waste liquid
Manage increased costs.Therefore the concentration of nitric acid is restricted in the range of 30-50g/L due to dissolubility and economy.
In above-mentioned neutral salt electrolytic cell, current density should be 6A/dm2To 10A/dm2.If in oxide skin cathodic pickling
The current density of period, electrode are less than 6A/dm2, then can not be formed can dissolve oxide skin on PH stainless steel surface
Surface potential, it is thus possible to cause stainless steel watch surface oxidized skin removal effect undesirable.The upper limit of current density is not special
Setting, but due in the actual production process, needing operator visually to decide whether to stop cathodic pickling, and current density mistake
Cause electrode reaction violent greatly, the substrate below oxide skin is likely to be broken.In conjunction with feasibility and economy, the electric current of anode and cathode
Density is limited in 10A/dm2Below.
In ultrasonic cavitation processing, used supersonic frequency is 40kHz.When supersonic frequency is lower, cavitation is not
It obviously, can not effectively assisted electrolysis pickling.When supersonic frequency is excessively high, during cathodic pickling electrode surface generate hydrogen and
Oxygen can acutely shake in the solution, to reduce the contact area of electrode and electrolyte, lead to surface scale cathodic pickling
The reduction of efficiency.Therefore the supersonic frequency used is 40kHz.
During cathodic pickling and ultrasonic cavitation carry out, the electrolyte in electrolytic cell is 25 DEG C -35 DEG C.If electrolyte
Temperature is lower than 25 DEG C, then cathodic pickling reaction speed is slow, it is thus possible to be difficult to efficiently remove the oxide skin of stainless steel surface.Electricity
The upper limit of solution liquid temperature is not set particularly, but verified the method for the present invention can reach higher efficiency at 25 DEG C -35 DEG C,
And electrolyte temperature it is excessively high when reactor stability may reduce.Preferably, the electrolyte in electrolytic cell is 25 DEG C -35
℃。
Alternately, sequencing is that ultrasonic cavitation is handled preceding for ultrasonic cavitation processing and neutral salt electrolysis pickling processes,
Neutral salt electrolysis pickling processes are rear.Ultrasonic cavitation is formed by mechanical shock and accelerates loose stainless steel watch surface oxidized skin
Peeling, ultrasonic wave microjet can be improved electrode surface mass transfer in liquid phase speed, therefore carries out ultrasonic cavitation processing first and can be improved
Cathodic pickling efficiency for the first time.
In these cases, ultrasonic cavitation processing and neutral salt electrolysis pickling processes time are 2-3min.
Embodiment 1:
PH stainless steel room temperature electrolytic pickling method provided in this embodiment includes the following step carried out in order
It is rapid:
1) it prepares and makees containing the neutral salt electrolyte that 150g/L sodium sulphate, 50g/L nitric acid and surplus are water in a cell
For the medium of ultrasonic cavitation and neutral salt electrolysis pickling；The temperature of neutral salt electrolyte is 25 DEG C；
2) PH stainless steel of surface to be processed with oxide skin is immersed in above-mentioned neutral salt electrolyte, so
Supersonic generator is opened afterwards and generates ultrasonic wave, and supersonic frequency 40kHz is stainless to precipitation hardenable using ultrasonic cavitation
Steel carries out ultrasonic cavitation and handles 3min；The weight percent of each component in the PH stainless steel are as follows: Cu:3.0-
5.0%, Cr:15.5-17.5%, Ni:3.0-5.0%, Nb:0.15-0.45%, C:0.07%, remaining is Fe, and solid solubility temperature exists
Between 1030 DEG C to 1050 DEG C；
3) supersonic generator is closed, using PH stainless steel as anode, platinum electrode is as cathode, in 8A/dm2
Current density under to PH stainless steel carry out neutral salt electrolysis pickling processes 3min；
4) step 2)-step 3) is repeated, until the surface non-scale of PH stainless steel remains.
Embodiment 2:
PH stainless steel room temperature electrolytic pickling method provided in this embodiment includes the following step carried out in order
It is rapid:
1) it prepares and makees containing the neutral salt electrolyte that 120g/L sodium sulphate, 40g/L nitric acid and surplus are water in a cell
For the medium of ultrasonic cavitation and neutral salt electrolysis pickling；The temperature of neutral salt electrolyte is 30 DEG C；
2) PH stainless steel of surface to be processed with oxide skin is immersed in above-mentioned neutral salt electrolyte, so
Supersonic generator is opened afterwards and generates ultrasonic wave, and supersonic frequency 40kHz is stainless to precipitation hardenable using ultrasonic cavitation
Steel carries out ultrasonic cavitation and handles 2.5min；The weight percent of each component in the PH stainless steel are as follows: Cu:3.0-
5.0%, Cr:15.5-17.5%, Ni:3.0-5.0%, Nb:0.15-0.45%, C:0.07%, remaining is Fe, and solid solubility temperature exists
Between 1030 DEG C to 1050 DEG C；
3) supersonic generator is closed, using PH stainless steel as anode, platinum electrode is as cathode, in 10A/
dm2Current density under to PH stainless steel carry out neutral salt electrolysis pickling processes 2.5min；
4) step 2)-step 3) is repeated, until the surface non-scale of PH stainless steel remains.
Claims (5)
1. a kind of PH stainless steel room temperature electrolytic pickling method, it is characterised in that: the PH stainless steel
Room temperature electrolytic pickling method includes the following steps carried out in order:
1) neutral salt electrolyte containing 100-150g/L sodium sulphate, 30-50g/L nitric acid and surplus for water is prepared in a cell
Medium as ultrasonic cavitation and neutral salt electrolysis pickling；
2) PH stainless steel of surface to be processed with oxide skin is immersed in above-mentioned neutral salt electrolyte, is then opened
It opens supersonic generator and generates ultrasonic wave, ultrasonic cavitation processing is carried out to PH stainless steel using ultrasonic cavitation；
3) supersonic generator is closed, using PH stainless steel as anode, platinum electrode is as cathode, to precipitation hardenable
Stainless steel carries out neutral salt electrolysis pickling processes；
4) step 2)-step 3) is repeated, until the surface non-scale of PH stainless steel remains.
2. PH stainless steel room temperature electrolytic pickling method according to claim 1, it is characterised in that: in step 2)
With in step 3), the temperature range of the neutral salt electrolyte is 25-35 DEG C.
3. PH stainless steel room temperature electrolytic pickling method according to claim 1, it is characterised in that: in step 2)
In, supersonic frequency used by the supersonic generator is 40kHz.
4. PH stainless steel room temperature electrolytic pickling method according to claim 1, it is characterised in that: in step 3)
In, whens described neutral salt electrolysis pickling processes, used current density was 6-10A/dm2。
5. PH stainless steel room temperature electrolytic pickling method according to claim 1, it is characterised in that: in step 2)
With in step 3), the ultrasonic cavitation processing and neutral salt electrolysis pickling processes time are 2-3min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811123266.XA CN109267142A (en) | 2018-09-26 | 2018-09-26 | A kind of PH stainless steel room temperature electrolytic pickling method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811123266.XA CN109267142A (en) | 2018-09-26 | 2018-09-26 | A kind of PH stainless steel room temperature electrolytic pickling method |
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| CN109267142A true CN109267142A (en) | 2019-01-25 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110965116A (en) * | 2019-11-27 | 2020-04-07 | 中国民航大学 | Electrolysis ultrasonic cooperative device suitable for precipitation hardening stainless steel descaling |
| WO2022091049A1 (en) * | 2020-11-01 | 2022-05-05 | Bholanda Dipakkumar | Novel process for descaling or pickling of steels and stainless steels |
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| JP2003027295A (en) * | 2001-07-23 | 2003-01-29 | Sumitomo Metal Ind Ltd | Method for pickling stainless steel strip |
| CN1900384A (en) * | 2006-07-05 | 2007-01-24 | 北京航空航天大学 | Process for removing part surface oxidized skin using supersonic wave and electrolytic combination |
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| CN103403230A (en) * | 2010-12-28 | 2013-11-20 | Posco公司 | Eco-friendly high-speed pickling process for producing a low-chrome ferrite-based cold-rolled stainless steel sheet having superior surface quality |
| CN105332043A (en) * | 2015-11-24 | 2016-02-17 | 苏州盖德精细材料有限公司 | Normal-temperature electropolishing solution and preparation method thereof |
| CN107245671A (en) * | 2017-06-21 | 2017-10-13 | 合肥市旺友门窗有限公司 | A kind of stainless steel manufacture craft for plastic-steel door and window |
| CN108360058A (en) * | 2018-03-23 | 2018-08-03 | 中山大学 | A kind of electrolyte and stainless steel engraving method for etching stainless steel |
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2018
- 2018-09-26 CN CN201811123266.XA patent/CN109267142A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5130000A (en) * | 1990-07-27 | 1992-07-14 | Andritz-Patentverwaltungs-Gesellschaft M.B.H. | Pickling high-grade steel |
| CN1261630A (en) * | 1998-12-22 | 2000-08-02 | 安德里茨-专利管理有限公司 | Acid washing process for stainless steel |
| JP2002348700A (en) * | 2001-03-23 | 2002-12-04 | Sumitomo Metal Ind Ltd | DESCALING METHOD FOR COLD-ROLLED AND ANNEALED Cr-BASED STAINLESS STEEL SHEET |
| JP2003027295A (en) * | 2001-07-23 | 2003-01-29 | Sumitomo Metal Ind Ltd | Method for pickling stainless steel strip |
| CN1900384A (en) * | 2006-07-05 | 2007-01-24 | 北京航空航天大学 | Process for removing part surface oxidized skin using supersonic wave and electrolytic combination |
| CN101165223A (en) * | 2007-08-15 | 2008-04-23 | 山西太钢不锈钢股份有限公司 | Acid pickling method for stainless steel surface |
| CN103403230A (en) * | 2010-12-28 | 2013-11-20 | Posco公司 | Eco-friendly high-speed pickling process for producing a low-chrome ferrite-based cold-rolled stainless steel sheet having superior surface quality |
| CN105332043A (en) * | 2015-11-24 | 2016-02-17 | 苏州盖德精细材料有限公司 | Normal-temperature electropolishing solution and preparation method thereof |
| CN107245671A (en) * | 2017-06-21 | 2017-10-13 | 合肥市旺友门窗有限公司 | A kind of stainless steel manufacture craft for plastic-steel door and window |
| CN108360058A (en) * | 2018-03-23 | 2018-08-03 | 中山大学 | A kind of electrolyte and stainless steel engraving method for etching stainless steel |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110965116A (en) * | 2019-11-27 | 2020-04-07 | 中国民航大学 | Electrolysis ultrasonic cooperative device suitable for precipitation hardening stainless steel descaling |
| WO2022091049A1 (en) * | 2020-11-01 | 2022-05-05 | Bholanda Dipakkumar | Novel process for descaling or pickling of steels and stainless steels |
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