CN103103541A - Silicon steel acid cleaning stabilizing material and application method thereof - Google Patents
Silicon steel acid cleaning stabilizing material and application method thereof Download PDFInfo
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- CN103103541A CN103103541A CN2013100252239A CN201310025223A CN103103541A CN 103103541 A CN103103541 A CN 103103541A CN 2013100252239 A CN2013100252239 A CN 2013100252239A CN 201310025223 A CN201310025223 A CN 201310025223A CN 103103541 A CN103103541 A CN 103103541A
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Abstract
The invention discloses a silicon steel acid cleaning stabilizing material and an application method thereof. The silicon steel acid cleaning stabilizing material comprises an acid cleaning accelerator and an inhibitor, wherein the acid cleaning accelerator comprises the following components in percentage by weight: 5-20% of surfactant, 5-20% of organic metal chelating agent, 20-40% of reducing agent and 20-40% of water; and the inhibitor comprises the following components in percentage by weight: 10-30% of urotropin, 10-50% of diethylene glycol, 5-15% of o-xylene thiourea, 0-10% of fatty alcohol-polyoxyethylene ether and the balance of water. According to the invention, the silicon steel acid cleaning speed is increased, the speed of hydrogen atom entering strip steel is reduced, the aims of increasing the acid cleaning speed, reducing the acid cleaning temperature, reducing the consumption of hydrochloric acid and reducing brittleness of silicon steel are reached, and stable operation of silicon steel acid cleaning production is realized.
Description
Technical field
The present invention relates to the pickling technology, particularly a kind of silicon-steel pickling stable material and using method thereof.
Background technology
Pickling is the essential operation together in the cold rolled strip steel production process, and the continuity that the quality of pickling is produced quality and the operation of rolling of Cold-strip Steel Surface has important impact.In the cold rolled silicon steel production process, contain the compound of silicon in the oxide skin due to surface of silicon steel, increased the difficulty of pickling.Be to improve the pickling speed of silicon steel, adopt before strip pickling on the one hand shot-peening aspect remove the oxide skin of a part of Surfaces of Hot Rolled Strip, reach by the way that reduces pickling speed the purpose of removing surface scale on the other hand.Obviously before these, a kind of method will improve production cost greatly, a kind of rear method will have influence on the production capacity of unit, these two kinds of methods will make exposed metal directly contact with acid solution simultaneously, the hydrogen atom that forms in metal and acid solution contact process with rapid osmotic in metal body, further increase the fragility of silicon steel, greatly improve the generation that accident is split on broken belt in the belt steel rolling process and limit.
Be the pickling speed of raising with steel, add acid pickling promotor and inhibiter in the strip pickling liquid of being everlasting.Chinese patent CN01133516.5 discloses a kind of acid pickling promotor for iron and steel, its composition and weight proportion are inorganic salt reductive agent (as a kind of in S-WAT, sodium hydrosulfite 90min, pyrosulfurous acid sodium, Sulfothiorine, ammonium thiosulfate or two kinds), 10%～80%; Organo-metallic ion chelating agent (as in gluconic acid and salt, tartrate and salt, citric acid and salt, disodium EDTA a kind of), 1%～20%; Synergistic agent (as in butynediol, ethylene glycol, glycerol a kind of), 1%～20%; Water 10%～50%.CN93115819.2 has invented a kind of de-scaling accelerator for the steel sulfuric acid washing, and this accelerator is by A, B two-component mixture matter.The A component is that one or both components such as oxammonium hydrochloride, hydrazonium sulfate, Sodium Hydrosulphite, oxammonium sulfate, thiocarbamide, formaldehyde, phosphorous acid, thionamic acid, potassiumiodide form, and the add-on of A component is 0.02～0.08% of sulfuric acid pickling solution weight; The B component is that dioctyl sodium sulfosuccinate or 18 alkyl trimethyl ammonium chlorides form, and perhaps adds the compositions such as dibenzo diazole sodium, triamide quaternary amine, and its add-on is 0.019～0.05% of pickle solution weight.A, B two components are put in pickle solution after mixing in 5: 5 to 8: 2 ratios.Aspect the pickling inhibition, it is the aniline aldehyde polymer by main component that Chinese patent CN201010100891.X should invent related inhibiter, is applicable as with the scavenging solution submergence that is added with inhibiter and cleans steel.Chinese patent CN201110122663.7 has announced a kind of restrainer, and its this inhibiter is comprised of alkyl pyridine quaternary ammonium salt, pure and mild nonionogenic tenside.
Summary of the invention
The object of the present invention is to provide a kind of silicon-steel pickling stablizer and using method, when improving silicon-steel pickling speed, reduce the speed in hydrogen atom flushed zone steel, reach the purpose that improves pickling speed, reduction pickling temperature, the consumption of minimizing hydrochloric acid, reduces the fragility of silicon steel, realize that the stable of silicon-steel pickling production carries out.
Technical scheme of the present invention is:
A kind of silicon-steel pickling stable material, it comprises: the pickling accelerator, its composition weight percent is: tensio-active agent, 5～20%, the organo-metallic sequestrant, 5～20%, reductive agent, 20～40%, water, 20～40%; Inhibitor, its composition weight percent is: urotropine, 10～30%, glycol ether, 10～50%, o-xylene thiourea, 5～15%, fatty alcohol-polyoxyethylene ether, 0～10%, all the other water.
Further, described tensio-active agent is nonionic surfactant, in alkylphenol polyoxyethylene, sodium alkyl benzene sulfonate or fatty alcohol-polyoxyethylene ether more than one.
Described organo-metallic sequestrant be in citric acid, disodium salt disodium, nitrilotriacetic acid(NTA), Amino Trimethylene Phosphonic Acid or ethylenediamine tetramethylene phosphonic acid more than one.
Described reductive agent be in S-WAT, Sulfothiorine, thiourea peroxide, amino imino sulfonic acid or ammonia thiosulfate more than one.
The using method of silicon-steel pickling stable material of the present invention, above-mentioned silicon-steel pickling stable material is added successively the first～the 3rd pickling tank of arranging with reflux type, the band steel is successively through the first～the 3rd pickling tank, and acid solution is from the 3rd pickling tank adverse current to the first pickling tank; Wherein, the ratio of pickling accelerator in the silicon-steel pickling stable material in 0.5～2.0 % by weight of acid cycle amount joined in the second pickling tank, keep the interior concentration of hydrochloric acid of the first pickling tank between 3～5%, temperature is at 80～85 ℃, concentration of hydrochloric acid is between 4～6 quality % in the second pickling tank, 78～83 ℃ of temperature; The ratio of pickling inhibitor in 0.5～2.0 % by weight of acid cycle amount joined in the 3rd pickling tank, keep the interior concentration of hydrochloric acid of the 3rd pickling tank between 8～10%, temperature is at 75～80 ℃.
Cold rolled silicon steel typically refers in soft steel silicone content at the material below 3.0%, owing to containing a large amount of element silicons in material, increases on the one hand the fragility of material, causes on the other hand surface scale dissolve in pickle solution difficult.
The hot rolled steel plate surface oxidation skin is by wustite (FeO), hematite (Fe
2O
3) and magnet body (Fe
3O
4) etc. the mixture of ferriferous oxide, it has been generally acknowledged that outermost layer is Fe
2O
3, the middle layer is Fe
3O
4, and be FeO near the nexine of steel plate, contain element silicon in ferrous materials, also contain Fe SiO in oxide skin
3One class material.When the steel plate with iron scale is immersed in Acidwash solution, according to the constructional feature of iron scale, a series of chemistry and electrochemical reaction process will occur, acid cleaning process can be summarised as three aspects according to the action principle of reacting:
1) solvency action
In the belt steel surface iron scale, the oxide dissolution of various iron in acid solution, generates the ferric iron and the ferrous muriate that are dissolvable in water acid solution, and its reaction formula is:
Fe
2O
3+6HCl＝2FeCl
3+3H
2O
Fe
3O
4+8HCl＝2FeCl
3+FeCl
2+4H
2O
FeO+2HCl＝FeCl
2+H
2O
2) mechanically peel effect
In the belt steel surface iron scale outside the various oxide compounds of deironing, the metallic iron that also is being mingled with part, and iron scale has again porousness, and acid solution just can be by hole and the iron in crack and iron scale or the matrix effect of iron scale so, and a large amount of hydrogen of corresponding generation.The swelling pressure by this part hydrogen produces just can strip down iron scale from belt steel surface, its chemical reaction is:
Fe+HCl＝FeCl
2+H
2↑
Mechanically peel plays a part very large in acid cleaning process.According to the pertinent data introduction, during chlorohydric acid pickling, there is 33% iron scale to be removed by the mechanically peel effect.
But in acid cleaning process, we do not wish that Acidwash solution and matrix react, because will make like this loss of acid and matrix too much.Simultaneously, a part of hydrogen that produces in reaction will be diffused into and goes in matrix and cause hydrogen embrittlement.
3) reductive action
Metallic iron and Acidwash solution are done the used time, at first produce hydrogen atom, the part hydrogen atom is by its chemical activity and very strong reducing power, and the oxide compound of high price iron and high price molysite are reduced into the low price ferriferous oxide that is soluble in acid solution and molysite at a low price, the carrying out that is conducive to pickling, its reaction formula is:
Fe
2O
3+2[H]＝2FeO+H
2O
Fe
3O
4+2[H]＝3FeO+H
2O
FeCl
3+[H]＝FeCl
2+HCl
Therefore for improving pickling speed and reducing the negative effect that hydrogen increases material fragility, need to improve pickle solution to the wetting velocity with steel at the initial stage of pickling, reduce the thickness with the fluid boundary layer between steel and pickle solution, thereby realize with the rapid heating of steel and moistening fast, reach the purpose that improves pickling speed.And later stage of pickling due to the oxide skin of belt steel surface seldom, at this moment need to stop the speed of response of metal body and pickle solution, reduce the generation of atomic hydrogen, reach the purpose that reduces metal loss and do not increase the material hydrogen embrittlement.
The pickling unit of cold rolled strip is comprised of three pickling tanks usually, and in each pickling tank, the concentration of hydrochloric acid is different, usually adopts reflux type to arrange, as shown in Figure 1.Band steel 100 enters from the first pickling tank 1, and the band steel is heated by pickle solution in this pickling tank, and this moment, the main and pickle solution of oxide skin of belt steel surface carried out chemical reaction.After the band steel entered into the second pickling tank 2, the acid concentration in acid tank increased, and chemical reaction is more violent, carries out simultaneously the electrochemical reaction between pickle solution and metal body, generated the hydrogen atom of nascent state, accelerated the process of de-scaling process.When the band steel entered into the 3rd pickling tank 3, the most of oxide skin of belt steel surface was eliminated, and at this moment a large amount of metal bodies contacts with pickle solution, and electrochemical reaction occurs, and produces a large amount of hydrogen atoms.For this reason, mainly reach by wettability and the oxidisability two of improving pickle solution the purpose that improves pickling speed for the pickling unit in first, second pickling tank, and in the 3rd pickling tank main metal body and the pickling generation electrochemical reaction of reducing, the hydrogen that reduces nascent state produces, thus the purpose that realizes reducing metal loss and do not increase the material hydrogen embrittlement.
In silicon-steel pickling stable material of the present invention, the Main Function of pickling accelerator is to improve pickle solution to the wettability of silicon steel and the reducing power of pickle solution, joins in the second pickling tank, is overflowed in the first pickling tank by the second pickling tank.Inhibitor is in order to suppressing the speed of metal body and hydrochloric acid reaction, but do not affect the chemical reaction between pickle solution and the residual oxide skin of belt steel surface, joins in the 3rd pickling tank.
The invention has the beneficial effects as follows:
Silicon-steel pickling synergistic agent of the present invention can improve the pickling speed of silicon steel greatly, reduces pickling temperature, avoids belt steel surface to produce over-pickling, improves pickling unit production capacity, improves with the steel lumber recovery and reduce the purpose of pickling energy consumption thereby reach.
Description of drawings
Fig. 1 is the schematic diagram of silicon-steel pickling unit.
In figure, 1,2,3 is the first～the 3rd pickling tank, 4,4 ', 4 " and be well heater, 5,5 ', 5 ", 6,6 ', 6 " and be thermometer, 100 are the band steel.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1: the very pickling of SiClx steel
The pickling accelerator:
Inhibitor:
Ratio in acid cycle amount 2.0% joins the pickling accelerator in the second pickling tank, keep the interior concentration of hydrochloric acid of the first pickling tank between 3～5%, temperature is at 85 ℃, in the second pickling tank, concentration of hydrochloric acid is between 4～6%, 83 ℃ of temperature, ratio in acid cycle amount 0.5% joins inhibitor in the 3rd pickling tank, keeps the interior concentration of hydrochloric acid of the 3rd pickling tank between 8～10%, and temperature is at 80 ℃.
Adopt above-described embodiment silicon-steel pickling stable material and acid cleaning process parameter; can make the unit pickling speed of turbulent pickling unit when normalizing silicon steel is exempted from pickling reach 200 m/mins; belt steel surface after pickling has metalluster, avoids the Hydrogen Brittleness Phenomena that occurs in the strip pickling process.
Embodiment 2: the very pickling of SiClx steel
The pickling accelerator:
Inhibitor:
Ratio in acid cycle amount 2.0% joins the pickling accelerator in the second pickling tank, keep the interior concentration of hydrochloric acid of the first pickling tank between 3.5～6.5%, temperature is at 80 ℃, in the second pickling tank, concentration of hydrochloric acid is between 7～12%, 83 ℃ of temperature, ratio in acid cycle amount 1.5% joins inhibitor in the 3rd pickling tank, keeps the interior concentration of hydrochloric acid of the 3rd pickling tank between 8～14%, and temperature is at 80 ℃.
Adopt above-described embodiment silicon-steel pickling stable material and acid cleaning process parameter; can make the unit pickling speed of turbulent pickling unit when normalizing silicon steel is exempted from pickling reach 200 m/mins; belt steel surface after pickling has metalluster, avoids the Hydrogen Brittleness Phenomena that occurs in the strip pickling process.
Embodiment 3: the pickling of normalizing silicon steel
The pickling accelerator
Inhibitor:
The pickling stablizer that will make by above-mentioned formula, ratio in acid cycle amount 0.5% joins the pickling accelerator in the second pickling tank, keep the interior concentration of hydrochloric acid of the first pickling tank between 3～5%, temperature is at 85 ℃, concentration of hydrochloric acid is between 4～6% in the second pickling tank, and 80 ℃ of temperature join inhibitor in the 3rd pickling tank in the ratio of acid cycle amount 0.5%, keep the interior concentration of hydrochloric acid of the 3rd pickling tank between 8～10%, temperature is at 75 ℃.
Adopt above-described embodiment silicon-steel pickling stable material and acid cleaning process parameter; can make the unit pickling speed of turbulent pickling unit when normalizing silicon steel is exempted from pickling reach 230 m/mins; belt steel surface after pickling has metalluster; avoid the Hydrogen Brittleness Phenomena that occurs in the strip pickling process; can reduce steam usage quantity 20%, reduce metal loss 0.1% in acid cleaning process.
Embodiment 4: the pickling of normalizing silicon steel
The pickling accelerator
Inhibitor:
Ratio in acid cycle amount 2.0% joins the pickling accelerator in the second pickling tank, keep the interior concentration of hydrochloric acid of the first pickling tank between 3.5～6.5%, temperature is at 80 ℃, in the second pickling tank, concentration of hydrochloric acid is between 7～12%, 83 ℃ of temperature, ratio in acid cycle amount 1.5% joins inhibitor in the 3rd pickling tank, keeps the interior concentration of hydrochloric acid of the 3rd pickling tank between 8～14%, and temperature is at 80 ℃.
Adopt above-described embodiment silicon-steel pickling stable material and acid cleaning process parameter; can make the unit pickling speed of turbulent pickling unit when normalizing silicon steel is exempted from pickling reach 200 m/mins; belt steel surface after pickling has metalluster; avoid the Hydrogen Brittleness Phenomena that occurs in the strip pickling process; can reduce steam usage quantity 20%, reduce metal loss 0.08% in acid cleaning process.
Embodiment 5: the curling pickling with steel of high temperature
The pickling accelerator:
Inhibitor:
Ratio in acid cycle amount 1.0% joins the pickling accelerator in the 3rd pickling tank, keep the interior concentration of hydrochloric acid of the first pickling tank between 3～5%, temperature is at 85 ℃, in the 3rd pickling tank, concentration of hydrochloric acid is between 4～6%, 83 ℃ of temperature, ratio in acid cycle amount 0.5% joins inhibitor in the 3rd pickling tank, keeps the interior concentration of hydrochloric acid of the 3rd pickling tank between 8～10%, and temperature is at 80 ℃.
Adopt above-described embodiment silicon-steel pickling stable material and using method, can make turbulent pickling unit reach 200 m/mins at the curling unit pickling speed during with steel of pickling high temperature, the belt steel surface after pickling has metalluster.
Embodiment 6: the curling pickling with steel of high temperature
The pickling accelerator:
Inhibitor:
Ratio in acid cycle amount 2.0% joins the pickling accelerator in the 3rd pickling tank, keep the interior concentration of hydrochloric acid of the first pickling tank between 3～5%, temperature is at 85 ℃, in the 3rd pickling tank, concentration of hydrochloric acid is between 4～6%, 83 ℃ of temperature, ratio in acid cycle amount 0.5% joins inhibitor in the 3rd pickling tank, keeps the interior concentration of hydrochloric acid of the 3rd pickling tank between 8～10%, and temperature is at 80 ℃.
Adopt above-described embodiment silicon-steel pickling stable material and using method, can make turbulent pickling unit reach 200 m/mins at the curling unit pickling speed during with steel of pickling high temperature, the belt steel surface after pickling has metalluster.Can reduce hydrochloric acid and use consumption 10%, reduce metal loss 0.5% in acid cleaning process.
Claims (5)
1. silicon-steel pickling stable material, it comprises:
The pickling accelerator, its composition weight percent is: tensio-active agent, 5～20%, the organo-metallic sequestrant, 5～20%, reductive agent, 20～40%, water, 20～40%;
Inhibitor, its composition weight percent is: urotropine, 10～30%, glycol ether, 10～50%, o-xylene thiourea, 5～15%, fatty alcohol-polyoxyethylene ether, 0～10%, all the other water.
2. silicon-steel pickling stable material as claimed in claim 1, is characterized in that, described tensio-active agent is nonionic surfactant, in alkylphenol polyoxyethylene, sodium alkyl benzene sulfonate or fatty alcohol-polyoxyethylene ether more than one.
3. silicon-steel pickling stable material as claimed in claim 1, is characterized in that, described organo-metallic sequestrant be in citric acid, disodium salt disodium, nitrilotriacetic acid(NTA), Amino Trimethylene Phosphonic Acid or ethylenediamine tetramethylene phosphonic acid more than one.
4. silicon-steel pickling stable material as claimed in claim 1, is characterized in that, described reductive agent be in S-WAT, Sulfothiorine, thiourea peroxide, amino imino sulfonic acid or ammonia thiosulfate more than one.
5. the using method of silicon-steel pickling stable material as described in any one in claim 1～4, above-mentioned silicon-steel pickling stable material is added the first～the 3rd pickling tank of arranging with reflux type, the band steel is successively through the first～the 3rd pickling tank, and acid solution is from the 3rd pickling tank adverse current to the first pickling tank; Wherein, 0.5～2.0% the ratio of the pickling accelerator in the silicon-steel pickling stable material in the acid cycle amount joined in the second pickling tank, and in overflow to the first pickling tank; Keep concentration of hydrochloric acid in the first pickling tank between 3～5%, temperature is at 80～85 ℃, in the second pickling tank concentration of hydrochloric acid between 4～6%, 78～83 ℃ of temperature; 0.5～2.0% the ratio of pickling inhibitor in the acid cycle amount joined in the 3rd pickling tank, keep concentration of hydrochloric acid in the 3rd pickling tank between 8～10%, temperature is at 75～80 ℃.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103924250A (en) * | 2014-05-04 | 2014-07-16 | 北京爵鑫盛达科技发展有限公司 | Corrosion inhibitor and application thereof |
| CN104775127A (en) * | 2015-04-23 | 2015-07-15 | 衡水京华制管有限公司 | Acid wash for removing ferric oxide on surfaces of steel tubes |
| CN106191947A (en) * | 2015-12-01 | 2016-12-07 | 江苏九天光电科技有限公司 | Before being suitable for steel band plating, quickly defat activates two-in-one inorganic agent collocation method |
| CN106222713A (en) * | 2015-12-01 | 2016-12-14 | 江苏九天光电科技有限公司 | Before being suitable for steel band plating, quickly defat activates two-in-one inorganic agent, collocation method and application |
| CN106222712A (en) * | 2015-12-01 | 2016-12-14 | 江苏九天光电科技有限公司 | Before being suitable for steel band plating, quickly defat activates two-in-one inorganic agent |
| CN106245045A (en) * | 2016-07-19 | 2016-12-21 | 威海翔宇环保科技股份有限公司 | A kind of special rust remover of middle low-pressure boiler and preparation method thereof |
| CN106894027A (en) * | 2017-03-24 | 2017-06-27 | 桥运精密部件（苏州）有限公司 | A kind of STAINLESS STEEL WIRE cleaning agent |
| CN108517526A (en) * | 2018-03-27 | 2018-09-11 | 北京首钢股份有限公司 | A method of it is used to remove silicon mud online when silicon-steel pickling |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103924250A (en) * | 2014-05-04 | 2014-07-16 | 北京爵鑫盛达科技发展有限公司 | Corrosion inhibitor and application thereof |
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| CN104775127A (en) * | 2015-04-23 | 2015-07-15 | 衡水京华制管有限公司 | Acid wash for removing ferric oxide on surfaces of steel tubes |
| CN104775127B (en) * | 2015-04-23 | 2017-03-29 | 衡水京华制管有限公司 | A kind of pickle for removing oxidation ferrum |
| CN106191947A (en) * | 2015-12-01 | 2016-12-07 | 江苏九天光电科技有限公司 | Before being suitable for steel band plating, quickly defat activates two-in-one inorganic agent collocation method |
| CN106222713A (en) * | 2015-12-01 | 2016-12-14 | 江苏九天光电科技有限公司 | Before being suitable for steel band plating, quickly defat activates two-in-one inorganic agent, collocation method and application |
| CN106222712A (en) * | 2015-12-01 | 2016-12-14 | 江苏九天光电科技有限公司 | Before being suitable for steel band plating, quickly defat activates two-in-one inorganic agent |
| CN106245045A (en) * | 2016-07-19 | 2016-12-21 | 威海翔宇环保科技股份有限公司 | A kind of special rust remover of middle low-pressure boiler and preparation method thereof |
| CN106894027A (en) * | 2017-03-24 | 2017-06-27 | 桥运精密部件（苏州）有限公司 | A kind of STAINLESS STEEL WIRE cleaning agent |
| CN108517526A (en) * | 2018-03-27 | 2018-09-11 | 北京首钢股份有限公司 | A method of it is used to remove silicon mud online when silicon-steel pickling |
| CN108517526B (en) * | 2018-03-27 | 2019-11-29 | 北京首钢股份有限公司 | A method of silicon mud is removed when for silicon-steel pickling online |
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