CN108517526B - A method of silicon mud is removed when for silicon-steel pickling online - Google Patents
A method of silicon mud is removed when for silicon-steel pickling online Download PDFInfo
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- CN108517526B CN108517526B CN201810258324.3A CN201810258324A CN108517526B CN 108517526 B CN108517526 B CN 108517526B CN 201810258324 A CN201810258324 A CN 201810258324A CN 108517526 B CN108517526 B CN 108517526B
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- silicon
- sulfonic acid
- water
- high molecular
- molecular polymer
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- 238000005554 pickling Methods 0.000 title claims abstract description 52
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 46
- 239000010703 silicon Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 27
- 229920000642 polymer Polymers 0.000 claims abstract description 46
- 125000000542 sulfonic acid group Chemical group 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000000178 monomer Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 15
- 229920002554 vinyl polymer Polymers 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- 125000002091 cationic group Chemical group 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- -1 acrylyl Chemical group 0.000 claims description 5
- 150000002148 esters Chemical class 0.000 claims description 5
- 229920002521 macromolecule Polymers 0.000 claims description 5
- 239000013049 sediment Substances 0.000 claims description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- ZYASLVDNDXUOMI-UHFFFAOYSA-N n,n-dimethylmethanamine;prop-2-enoic acid Chemical group C[NH+](C)C.[O-]C(=O)C=C ZYASLVDNDXUOMI-UHFFFAOYSA-N 0.000 claims description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 125000003118 aryl group Chemical group 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 claims description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 2
- 239000005977 Ethylene Substances 0.000 claims description 2
- ZDWZXBJFITXZBL-UHFFFAOYSA-N S(=O)(=O)(O)C=CC1=CC=CC=C1.[Na] Chemical compound S(=O)(=O)(O)C=CC1=CC=CC=C1.[Na] ZDWZXBJFITXZBL-UHFFFAOYSA-N 0.000 claims description 2
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical group C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 4
- 239000005864 Sulphur Substances 0.000 claims 4
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 claims 1
- AUZRCMMVHXRSGT-UHFFFAOYSA-N 2-methylpropane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CC(C)CS(O)(=O)=O AUZRCMMVHXRSGT-UHFFFAOYSA-N 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 125000003368 amide group Chemical group 0.000 claims 1
- AVSXGQJYEFAQNK-UHFFFAOYSA-N prop-2-enamide;hydrate Chemical compound O.NC(=O)C=C AVSXGQJYEFAQNK-UHFFFAOYSA-N 0.000 claims 1
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical class CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 claims 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 20
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000001376 precipitating effect Effects 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 description 11
- 229920002401 polyacrylamide Polymers 0.000 description 10
- 125000000129 anionic group Chemical group 0.000 description 9
- 238000004062 sedimentation Methods 0.000 description 9
- 229910000831 Steel Inorganic materials 0.000 description 8
- 239000010959 steel Substances 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 150000001768 cations Chemical group 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000004737 colorimetric analysis Methods 0.000 description 4
- 238000005189 flocculation Methods 0.000 description 4
- 230000016615 flocculation Effects 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000003311 flocculating effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 1
- SYBUMOIKKHDLBN-UHFFFAOYSA-N C(=C)S(=O)(=O)O.C1=CC=CC=C1 Chemical compound C(=C)S(=O)(=O)O.C1=CC=CC=C1 SYBUMOIKKHDLBN-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- 206010027146 Melanoderma Diseases 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000344 molecularly imprinted polymer Polymers 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
- C23G1/085—Iron or steel solutions containing HNO3
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/36—Regeneration of waste pickling liquors
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The method for removing silicon mud online when the present invention provides a kind of for silicon-steel pickling includes the following steps: that the amphoteric water-soluble high molecular polymer containing sulfonic acid group is added in pickling solution, after stirring, is precipitated, the precipitating is removed.The method of the present invention removes that silicon effect is good, and stability is strong online, and most of silicon mud can be removed, and solves the problems, such as silicon mud poor removal effect in silicon steel production.
Description
Technical field
The invention belongs to silicon steel production technical field more particularly to it is a kind of for silicon-steel pickling when remove the side of silicon mud online
Method.
Background technique
Currently, work chemically and physically occurs for the oxide skin and pickling solution of surface of steel plate in silicon steel production technology when pickling
With finally obtaining clean surface so that oxide skin be made to fall off from surface of steel plate.Due in oxide skin silicon and its compound exist
Solubility very little in acid, therefore pickling solution has a large amount of silicon mud in cyclic process and generates, silicon mud particle is smaller, is not easy to sink
It forms sediment, often results in the blocking such as pickling system failure, such as graphite heat exchanger, circulating pump, pickling pipeline.Additionally result in the table of steel plate
The problems such as face is of poor quality, easily forms blackspot, point.The desiliconization agent now generallyd use include inorganic (such as: polymeric iron, polymeric aluminum
Deng) and polyacrylamide (such as: polyacrylamide amine cation, polyacrylamide anion, polyacrylamide nonionic), it answers
Used time needs while adding two kinds, i.e. inorganic and polyacrylamide cooperates add simultaneously, and complicated for operation, effect is also paid no attention to
Think.
Summary of the invention
In view of the above-mentioned drawbacks in the prior art, the main purpose of the present invention is to provide one kind be used for silicon-steel pickling when
The method that line removes silicon mud solves the problems, such as silicon mud poor removal effect in silicon steel production online except silicon effect is good.
In order to achieve the above object, the present invention adopts the following technical scheme: a kind of be used to remove silicon online when silicon-steel pickling
The method of mud, includes the following steps:
The amphoteric water-soluble high molecular polymer containing sulfonic acid group is added in pickling solution, after stirring, is precipitated, by institute
State precipitating removal.
As a further preference, the amphoteric water-soluble high molecular polymer containing sulfonic acid group are as follows: sulfonic group will be contained
The amphoteric water-soluble high molecular polymer of group is configured to the solution of 8-12% weight percent with demineralized water.
As a further preference, the amphoteric water-soluble high molecular polymer described in every liter of acid solution containing sulfonic acid group adds
Amount is 1-2 milligrams.
As a further preference, 120-200 revs/min of the mixing speed, the temperature of the pickling solution are 60-90 DEG C.
As a further preference, the preparation method packet of the amphoteric water-soluble high molecular polymer containing sulfonic acid group
It includes: will include the reaction system of water soluble cationic vinyl monomer, the monomer of anionic vinyl containing sulfonic acid group and water, gathered
Reaction is closed, the amphoteric water-soluble high molecular polymer containing sulfonic acid group is obtained；The water soluble cationic vinyl monomer is selected from two
Allyl dimethyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac and acrylic acid trimethylamine groups ester chloride；It is described to contain
Sulfonic acid group anionic vinyl monomer be selected from styrene sulfonic acid or its sulfonate, 2- acrylamide-2-methyl propane sulfonic or its third
Sulfonate.
As a further preference, further include in the reaction system acrylic acid and or acrylamide.
As a further preference, the molar ratio of anionic vinyl monomer and cationic ethylene monomer in the reaction system
Are as follows: 0.1~3:5~99.9.
As a further preference, the preparation method packet of the amphoteric water-soluble high molecular polymer containing sulfonic acid group
It includes: using acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic and water as reaction system, in 75-80
It polymerize 2h at DEG C, synthesis has the amphoteric macromolecule polymer of sulfonic group and strong basicity group.
As a further preference, the preparation method packet of the amphoteric water-soluble high molecular polymer containing sulfonic acid group
It includes: by the polymerisation in solution of styrene sulfonic acid sodium water solution and acrylic acid trimethylamine groups ester chloride, anamorphic zone aromatic sulphonic acid
The amphoteric macromolecule polymer of base.
As a further preference, the molecular weight of the amphoteric water-soluble high molecular polymer containing sulfonic acid group is 200
Between ten thousand -600 ten thousand.
As a further preference, after the precipitating removal, the silicon cement content in the pickling solution is less than 80mg/L.
The beneficial effects of the present invention are: the method for the present invention is for the first time in production high grade silicon steel acid cleaning process in online desiliconization
Using；Pickling solution of the present invention using the amphoteric water-soluble high molecular polymer containing sulfonic acid group for siliceous mud removes silicon online,
The shortcomings that stability is strong, and effect is good, overcomes polyacrylamide；Amphoteric water-soluble high molecular polymer containing sulfonic acid group point
Anionic group and cation group are had in son, cation group can capture organic suspension negatively charged in pickling solution
Object, anionic group can promote the sedimentation of mineral suspensions in Acidic Liquid, compare due to its structure the characteristics of and are suitable for handling
Other single inorganics or the reluctant occasion of organic desiliconization agent.
Specific embodiment
The present invention by provide it is a kind of for silicon-steel pickling when remove silicon mud online method, solve silicon steel production in silicon
The problem of mud poor removal effect.
In order to solve drawbacks described above, the main thought of the embodiment of the present invention is:
The method that the embodiment of the present invention is used to remove silicon mud online when silicon-steel pickling, includes the following steps:
The amphoteric water-soluble high molecular polymer containing sulfonic acid group is added in pickling solution, after stirring, is precipitated, by institute
State precipitating removal.
Above-mentioned pickling solution is common pickling solution, such as hydrochloric acid, nitric acid or mixed acid etc., type in silicon steel production technology
And the parameters such as concentration, dosage, temperature can refer to common process setting.
The above-mentioned amphoteric water-soluble high molecular polymer containing sulfonic acid group, including anionic group and cation group,
Cation group can capture organic suspended matter negatively charged in pickling solution, and anionic group can promote inorganic in Acidic Liquid
The sedimentation of suspended matter.Sulfonic acid group is a kind of anionic strongly hydrophilic group, above-mentioned polymer can be selected it is specific kind of at
Divide and is obtained by polymerization reaction.
Such as: reversed emulsion polymerization can be used and synthesize the above-mentioned amphoteric water-soluble high molecular polymer containing sulfonic acid group:
Component in reaction system is:
1. or mixtures thereof water soluble cationic vinyl monomer；
2. vinyl monomer containing sulfonic acid group (anion)；
3. water；
Mentioned component is subjected to polymerization reaction, obtains the amphoteric water-soluble high molecular polymer containing sulfonic acid group.
Cationic monomer structural formula in mentioned component are as follows:
A is O or NH in formula；B is C2H4、C3H6、C3H5OH；R1 is H or CH3；R2, R3 are the alkyl of C1~C4；R4 be H or
The alkyl or benzyl of C1~C4；X- is anionic property ion.
Above-mentioned vinyl monomer containing sulfonic acid group can be 2- acrylamide-2-methyl propane sulfonic or its salt (anion) or benzene
Vinyl sulfonic acid or its sulfonate；
Other water-soluble monomers can also be added in above-mentioned polymerization reaction, such as: cationic acrylic acid or acrylamide.
The molar ratio of anions and canons monomer in above-mentioned reaction system are as follows: 0.1~3:5~99.9.
The embodiment of the present invention further grinds other water-soluble monomers and studies carefully discovery, and the above-mentioned amphoteric water-soluble containing sulfonic acid group is high
The molecular weight of Molecularly Imprinted Polymer also has an impact to the sedimentation effect of silicon mud, and effect is preferable when between 2,000,000-600 ten thousand.Molecular weight
When less than 2,000,000, the net laying effect of flocculation sedimentation is small, and when molecular weight is greater than 6,000,000, net laying chain opening time is longer, and net laying is made
With can also become smaller.
The above-mentioned amphoteric water-soluble high molecular polymer containing sulfonic acid group is thick liquid, and water-soluble is fine, and scene is matched
System after being configured to the solution of 8-12% weight percent for example, by using demineralized water, is added in pickling solution and stirs.And
When the solution being configured to is less than 8-12%, solution is too dilute, is easy to happen hydrolysis, causes flocculation sedimentation effect to be deteriorated, is greater than
When 8-12%, solution viscosity is larger, is not easy to add.
And the desiliconization agent that the prior art uses, such as: cationic polyacrylamide, anionic polyacrylamide, nonionic
Polyacrylamide is largely solid, needs scene hydrolysis at that time.Hydrolysis time is longer (2-3 hours), leads to complex process, and go
Except the effect of silicon mud is also bad.
The embodiment of the present invention further study show that, mixing speed also has an impact to the removal effect of silicon mud, stirring speed
At 120-200 revs/min of degree, precipitating removal silicon mud effect is best.
The embodiment of the present invention further study show that, the above-mentioned amphoteric water-soluble high molecular polymer containing sulfonic acid group point
Son amount also has an impact to the sedimentation effect of silicon mud, the above-mentioned amphoteric water-soluble high molecular polymer containing sulfonic acid group in every liter of acid solution
Dosage is 1-2 milligram hour, cost performance highest.And when dosage is less than 1mg/l, dosage is low, and flocculation sedimentation effect is deteriorated, and throws
When dosage is greater than 2mg/l, medicament excess will cause, flocculating effect is deteriorated instead.
Silicon-steel pickling liquid ingredient includes: silicon mud, aluminium oxide, ferric ion, ferrous ion, sodium ion, lead ion, nickel
Several inorganic ions of ion, chromium ion, manganese ion etc. ten, ingredient are very complicated；In addition, the temperature of pickling solution is low, pH high, pickling when
Between it is short, after polymer use of the embodiment of the present invention, effect of settling is good.But it is 90 DEG C that the temperature design of pickling line is constant, pickling
Concentration of hydrochloric acid is designed as 20%, cannot change, pickling time: steel band forward speed is designed as 40-90 ms/min, according to different
Steel grade and coil pickled surface quality are adjusted.It, cannot the flocculating setting from pickling solution in time if it is too many that pickling solution washes the impurity to get off
Get off, will cause coil pickled surface quality variation, the forward speed of steel band can only be reduced, after adding polymer of the embodiment of the present invention,
Pickling solution is become clarifying from muddiness, and under the premise of guaranteeing coil pickled surface quality, steel band forward speed can be improved, opposite to be turned up
Yield.
After present invention method application, after the impurity flocculation sedimentation in silicon-steel pickling liquid, depickling is exhausted, clean acid
Liquid reuse, then pickled plate do not destroy the chemical component of hydrochloric acid, nor affect on the quality of steel plate after pickling.
The removal rate of nephelometer colorimetric method for determining silicon mud can be used in the embodiment of the present invention, with the filtered clear pickling solution of filter paper
Zeroing, confirms through practical application, and present invention method can remove 98% silicon mud, and effect stability.
Below with reference to specific embodiment further illustrate the present invention, the embodiment of the present invention for explaining only the invention,
It is not intended to limit protection scope of the present invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1
Amphoteric water-soluble high molecular polymer containing sulfonic acid group is configured to 10% (weight percent) with demineralized water
Solution is added in acid liquid reaction tank with metering pump by 1mg/l, and after agitated (160 revs/min of mixing speed), a high position flows to heavy
Shallow lake tank, after precipitation, supernatant flows in pickling tank, and the sediments such as silicon mud get to plate and frame filter press with pump and carry out desliming.Using
The removal rate of nephelometer colorimetric method for determining silicon mud, 98% silicon mud are removed.
The preparation method of the above-mentioned amphoteric water-soluble high molecular polymer containing sulfonic acid group includes: to be suspended in reaction system
In butanol, under nitrogen protection with azodiisobutyronitrile in 75-80 DEG C of polymerization 2h, synthesis has sulfonic group and strong basicity group
Amphoteric macromolecule polymer, molecular weight are 3,000,000.
The ingredient of variety classes and different ratio can be used in above-mentioned reaction system, as shown in table 1 below:
Table 1
Embodiment 2
Amphoteric water-soluble high molecular polymer containing sulfonic acid group is configured to 12% (weight percent) with demineralized water
Solution is added in acid liquid reaction tank with metering pump by 2mg/l, and after agitated (200 revs/min of mixing speed), a high position flows to heavy
Shallow lake tank, after precipitation, supernatant flows in pickling tank, and the sediments such as silicon mud get to plate and frame filter press with pump and carry out desliming.Using
The removal rate of nephelometer colorimetric method for determining silicon mud, 96% silicon mud are removed.
The preparation method of the above-mentioned amphoteric water-soluble high molecular polymer containing sulfonic acid group includes: by sodium styrene sulfonate water
The polymerisation in solution of solution and acrylic acid trimethylamine groups ester chloride, the Amphiphatic high polymer polymerization of anamorphic zone aromatic sulphonic acid base
Object.Its molecular weight is 6,000,000.
The ingredient of variety classes and different ratio can be used in above-mentioned reaction system, as shown in table 2 below:
Table 2
Embodiment 3
Amphoteric water-soluble high molecular polymer containing sulfonic acid group is configured to the molten of 8% (weight percent) with demineralized water
Liquid is added in acid liquid reaction tank with metering pump by 2mg/l, and after agitated (120 revs/min of mixing speed), a high position flows to precipitating
Tank, after precipitation, supernatant flow in pickling tank, and the sediments such as silicon mud get to plate and frame filter press with pump and carry out desliming.Using turbid
The removal rate of degree meter colorimetric method for determining silicon mud, 98% silicon mud are removed.
The preparation method of the above-mentioned amphoteric water-soluble high molecular polymer containing sulfonic acid group includes: by 2- acrylamide -2-
Methyl propane sulfonic acid, N- vinyl-N-methylacetaniide and diallyldimethylammonium chloride are suspended in butanol, in nitrogen protection
It is lower to use azodiisobutyronitrile in 75-80 DEG C of polymerization 2h, it has synthesized and has polymerize with the Amphiphatic high polymer of sulfonic group and strong basicity group
Object.Its molecular weight is 2,000,000.
Technical solution in above-mentioned the embodiment of the present application, at least have the following technical effects or advantages:
Present invention method is applied in online desiliconization in production high grade silicon steel acid cleaning process for the first time；The present invention is real
It applies pickling solution of the example using the amphoteric water-soluble high molecular polymer containing sulfonic acid group for siliceous mud and removes silicon, stability online
By force, the shortcomings that effect is good, overcomes polyacrylamide；The above-mentioned amphoteric water-soluble high molecular polymer molecule containing sulfonic acid group
In have anionic group and cation group, cation group can capture organic suspension negatively charged in pickling solution
Object, anionic group can promote the sedimentation of mineral suspensions in Acidic Liquid, compare due to its structure the characteristics of and are suitable for handling
Other single inorganics or the reluctant occasion of organic desiliconization agent.
It should be noted last that the above specific embodiment is only used to illustrate the technical scheme of the present invention and not to limit it,
Although being described the invention in detail referring to example, those skilled in the art should understand that, it can be to the present invention
Technical solution be modified or replaced equivalently, without departing from the spirit and scope of the technical solution of the present invention, should all cover
In the scope of the claims of the present invention.
Claims (9)
1. it is a kind of for silicon-steel pickling when remove silicon mud online method, characterized by the following steps:
The amphoteric water-soluble high molecular polymer containing sulfonic acid group is added in pickling solution, after stirring, is precipitated, it will be described heavy
It forms sediment and removes；
The preparation method of the amphoteric water-soluble high molecular polymer containing sulfonic acid group includes: will be including water-soluble cationic second
The reaction system of alkene monomer, the monomer of anionic vinyl containing sulfonic acid group and water carries out polymerization reaction, obtains containing sulfonic acid group
Amphoteric water-soluble high molecular polymer；The water soluble cationic vinyl monomer is selected from diallyldimethylammonium chloride, propylene
Acyloxyethyl trimethyl ammonium chloride and acrylic acid trimethylamine groups ester chloride；The monomer of anionic vinyl containing the sulfonic acid group choosing
From styrene sulfonic acid or its sulfonate, 2- acrylamide-2-methyl propane sulfonic or its propane sulfonic acid salt.
2. the method according to claim 1 for being used to remove silicon mud online when silicon-steel pickling, it is characterised in that: described to contain sulphur
The amphoteric water-soluble high molecular polymer of acid groups are as follows: by the amphoteric water-soluble high molecular polymer demineralized water containing sulfonic acid group
It is configured to the solution of 8-12% weight percent.
3. the method according to claim 1 or 2 for being used to remove silicon mud online when silicon-steel pickling, it is characterised in that: every liter
Amphoteric water-soluble high molecular polymer dosage described in acid solution containing sulfonic acid group is 1-2 milligrams.
4. the method according to claim 1 or 2 for being used to remove silicon mud online when silicon-steel pickling, it is characterised in that: described
120-200 revs/min of mixing speed, the temperature of the pickling solution is 60-90 DEG C.
5. the method according to claim 1 for being used to remove silicon mud online when silicon-steel pickling, it is characterised in that: the reaction
Further include in system acrylic acid and or acrylamide.
6. the method according to claim 1 for being used to remove silicon mud online when silicon-steel pickling, it is characterised in that: the reaction
The molar ratio of anionic vinyl monomer and cationic ethylene monomer in system are as follows: 0.1~3:5~99.9.
7. the method according to claim 1 for being used to remove silicon mud online when silicon-steel pickling, it is characterised in that: described to contain sulphur
The preparation method of the amphoteric water-soluble high molecular polymer of acid groups includes: by acrylyl oxy-ethyl-trimethyl salmiac, 2- third
Acrylamide -2- methyl propane sulfonic acid and water polymerize 2h, synthesis has sulfonic group and strong basicity as reaction system at 75-80 DEG C
The amphoteric macromolecule polymer of group.
8. the method according to claim 1 for being used to remove silicon mud online when silicon-steel pickling, it is characterised in that: described to contain sulphur
The preparation method of the amphoteric water-soluble high molecular polymer of acid groups includes: by styrene sulfonic acid sodium water solution and acrylic acid front three
The polymerisation in solution of amido ester chloride, the amphoteric macromolecule polymer of anamorphic zone aromatic sulphonic acid base.
9. the method according to claim 1 for being used to remove silicon mud online when silicon-steel pickling, it is characterised in that: described to contain sulphur
The molecular weight of the amphoteric water-soluble high molecular polymer of acid groups is between 2,000,000-600 ten thousand.
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| CN1100759A (en) * | 1993-09-22 | 1995-03-29 | 鞍山钢铁公司 | Sulfuric acid pickling descaling accelerator |
| CN1408901A (en) * | 2001-09-29 | 2003-04-09 | 华中科技大学 | Acid pickling promotor for iron and steel |
| CN102677076A (en) * | 2011-03-18 | 2012-09-19 | 宝山钢铁股份有限公司 | Method for removal of silicon impurities in silicon steel pickling waste liquor without dissolving process |
| CN103103541A (en) * | 2013-01-24 | 2013-05-15 | 宝山钢铁股份有限公司 | Silicon steel acid cleaning stabilizing material and application method thereof |
| CN103526215A (en) * | 2013-10-11 | 2014-01-22 | 武汉科技大学 | Silicon steel pickling promoter and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7722841B2 (en) * | 2006-04-25 | 2010-05-25 | General Electric Company | Polymeric chelant and coagulant to treat metal-containing wastewater |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100759A (en) * | 1993-09-22 | 1995-03-29 | 鞍山钢铁公司 | Sulfuric acid pickling descaling accelerator |
| CN1408901A (en) * | 2001-09-29 | 2003-04-09 | 华中科技大学 | Acid pickling promotor for iron and steel |
| CN102677076A (en) * | 2011-03-18 | 2012-09-19 | 宝山钢铁股份有限公司 | Method for removal of silicon impurities in silicon steel pickling waste liquor without dissolving process |
| CN103103541A (en) * | 2013-01-24 | 2013-05-15 | 宝山钢铁股份有限公司 | Silicon steel acid cleaning stabilizing material and application method thereof |
| CN103526215A (en) * | 2013-10-11 | 2014-01-22 | 武汉科技大学 | Silicon steel pickling promoter and preparation method thereof |
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