CN115161724A - Preparation method of nickel sulfamate electroplating solution - Google Patents
Preparation method of nickel sulfamate electroplating solution Download PDFInfo
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- CN115161724A CN115161724A CN202210819168.XA CN202210819168A CN115161724A CN 115161724 A CN115161724 A CN 115161724A CN 202210819168 A CN202210819168 A CN 202210819168A CN 115161724 A CN115161724 A CN 115161724A
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- nickel
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- nickel sulfamate
- solution
- resin
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- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 title claims abstract description 81
- 238000009713 electroplating Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000007747 plating Methods 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 24
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- 229910021585 Nickel(II) bromide Inorganic materials 0.000 claims abstract description 14
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004327 boric acid Substances 0.000 claims abstract description 14
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000000080 wetting agent Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 69
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 38
- 229910001453 nickel ion Inorganic materials 0.000 claims description 32
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 29
- 239000011347 resin Substances 0.000 claims description 28
- 229920005989 resin Polymers 0.000 claims description 28
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 21
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 18
- 239000003456 ion exchange resin Substances 0.000 claims description 18
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 18
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- XQPAPBLJJLIQGV-UHFFFAOYSA-N 4-methoxy-1,3-benzothiazole Chemical compound COC1=CC=CC2=C1N=CS2 XQPAPBLJJLIQGV-UHFFFAOYSA-N 0.000 claims description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims description 11
- WINXNKPZLFISPD-UHFFFAOYSA-M Saccharin sodium Chemical group [Na+].C1=CC=C2C(=O)[N-]S(=O)(=O)C2=C1 WINXNKPZLFISPD-UHFFFAOYSA-M 0.000 claims description 11
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 11
- 238000005342 ion exchange Methods 0.000 claims description 11
- 150000002815 nickel Chemical class 0.000 claims description 11
- ZPIRTVJRHUMMOI-UHFFFAOYSA-N octoxybenzene Chemical compound CCCCCCCCOC1=CC=CC=C1 ZPIRTVJRHUMMOI-UHFFFAOYSA-N 0.000 claims description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims description 11
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 239000012266 salt solution Substances 0.000 claims description 10
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical class NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- UMEWSJNRBXKWKZ-UHFFFAOYSA-M sodium;1,4-dioxo-1,4-dipentoxybutane-2-sulfonate Chemical compound [Na+].CCCCCOC(=O)CC(S([O-])(=O)=O)C(=O)OCCCCC UMEWSJNRBXKWKZ-UHFFFAOYSA-M 0.000 claims description 5
- 230000009466 transformation Effects 0.000 claims description 5
- 150000001768 cations Chemical class 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 239000011152 fibreglass Substances 0.000 claims description 4
- 239000005457 ice water Substances 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- SZHIIIPPJJXYRY-UHFFFAOYSA-M sodium;2-methylprop-2-ene-1-sulfonate Chemical compound [Na+].CC(=C)CS([O-])(=O)=O SZHIIIPPJJXYRY-UHFFFAOYSA-M 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- DGSDBJMBHCQYGN-UHFFFAOYSA-M sodium;2-ethylhexyl sulfate Chemical compound [Na+].CCCCC(CC)COS([O-])(=O)=O DGSDBJMBHCQYGN-UHFFFAOYSA-M 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 14
- 239000002184 metal Substances 0.000 abstract description 13
- 238000005260 corrosion Methods 0.000 abstract description 10
- 230000007797 corrosion Effects 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 6
- 150000003839 salts Chemical class 0.000 abstract description 5
- 230000007935 neutral effect Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 8
- 239000002585 base Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012527 feed solution Substances 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- -1 hydrogen ions Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- DITXJPASYXFQAS-UHFFFAOYSA-N nickel;sulfamic acid Chemical compound [Ni].NS(O)(=O)=O DITXJPASYXFQAS-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 2
- 235000019801 trisodium phosphate Nutrition 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000002828 fuel tank Substances 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000009662 stress testing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
- C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
- C25D3/18—Heterocyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/04—Acids; Metal salts or ammonium salts thereof
- C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention provides a preparation method of nickel sulfamate electroplating solution. The preparation method of the nickel sulfamate electroplating solution comprises the following steps of 1, uniformly mixing high-purity nickel sulfamate and nickel bromide in water; step 2, adding boric acid and adjusting the pH value of the solution; step 3, adding a wetting agent and a stress regulator in sequence, fully stirring and uniformly mixing; and 4, sequentially adding a dispersing agent and the modified nano aluminum oxide particles, fully stirring, and uniformly mixing to obtain the nickel sulfamate electroplating solution. The nickel sulfamate electroplating solution prepared by the preparation method disclosed by the invention effectively removes metal impurities such as Co, cu, fe, zn, mn, ca, mg, cr and the like in the electroplating solution, and the aluminum magnesium alloy base material with the nickel plating layer prepared by the high-purity nickel sulfamate electroplating solution has the advantages of higher neutral salt haze value, better bonding performance, higher hardness value, lower internal stress value, better mechanical property and corrosion resistance, simple preparation method and low cost.
Description
Technical Field
The invention belongs to the technical field of nickel electroplating, and particularly relates to a preparation method of nickel sulfamate electroplating solution.
Background
The main element of aluminum-magnesium alloys is aluminum, which is strengthened by the incorporation of small amounts of magnesium or other metallic materials. The aluminum is a metal with relatively soft texture, has good plasticity and processability, has weak metallicity, and can easily form a compact oxide film in oxygen, thereby preventing further oxidation of the aluminum metal, being not easy to corrode and having long service life. However, the hardness of pure metal aluminum is not high, which limits the application to a certain extent, therefore, the aluminum is made into alloy, and different kinds of metal elements are added into the electroplating solution of the aluminum, so that the surface coating of the metal aluminum is uniform and is difficult to corrode, thereby further improving the corrosion resistance and the wear resistance and prolonging the service life. The content of magnesium in the magnesium-aluminum alloy is usually between 3 and 5 percent, the magnesium has the advantages of low density, high tensile strength and high elongation, and the weight of the magnesium-aluminum alloy is lower than that of other series of alloys under the same area. It is commonly used in aviation, such as in the manufacture of aircraft fuel tanks. The method is widely applied in the conventional industry, generally adopts continuous casting and rolling manufacturing, belongs to a hot rolling aluminum plate series, and can be used for oxidation deep processing.
However, in practical production applications, the magnesium-aluminum alloy usually needs a certain technology to pretreat and protect the substrate so as to improve various service properties, such as corrosion resistance, abrasion resistance, weldability, conductivity, decorative effect, etc., and the most common technology is metal plating, and the metal plating is mainly realized by electroplating or chemical plating.
The electroplated nickel is widely applied to the field of metal coatings due to the characteristics of simple electroplating process, low cost, good protection performance and the like, and relates to the manufacturing aspects of machines, instruments, medical instruments, household appliances and the like. Compared with other metal nickel electroplating, the traditional nickel electroplating on the surface of the aluminum-magnesium alloy has higher difficulty mainly because the aluminum alloy substrate and a nickel coating have poor bonding force, are easy to foam and delaminate, are easy to generate static electricity, and the thickness of the coating is difficult to control, so that the corrosion resistance effect is poor, and the like. The main reason for this is that aluminum in aluminum magnesium alloy is amphoteric, and it is difficult to use a suitable plating solution. And because of the high porosity of the nickel plating layer, the effect of no pore can be achieved only when the plating thickness exceeds 25 microns. Therefore, the thin nickel plating layer cannot be used alone as a protective plating layer, and therefore, the development of a nickel plating solution with wide applicability and good plating effect is a hot spot of current research.
In recent years, nickel sulfamate is used as an important fine chemical raw material, and other nickel salts are replaced by the nickel sulfamate due to the unique advantages of the nickel sulfamate, so that the nickel sulfamate becomes a widely used electroplating main salt and is widely applied internationally, and the nickel sulfamate solution has the advantages that: the electrodeposition speed is high, the internal stress of the coating is low, and the current efficiency is high; high solubility and no pollution; the plating layer has fine, even and smooth crystallization and bright color. Therefore, nickel sulfamate is better selected as a raw material of the nickel electroplating, but in the process of preparing nickel sulfamate, the use effect of electroplating solution can be seriously influenced because the content of metal impurities such as iron, cobalt, copper and the like in nickel powder is generally high, and the high-purity nickel powder with high purchase price is required for preparing high-purity nickel sulfamate, so that the cost is high.
Therefore, how to obtain a nickel sulfamate electroplating solution with low cost and high purity is a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to: in order to solve the technical problems, the invention provides a preparation method of nickel sulfamate electroplating solution with low cost and high purity.
The technical scheme is as follows: in order to achieve the above object, the present invention provides a method for preparing a nickel sulfamate electroplating solution, comprising the steps of:
step 1, uniformly mixing high-purity nickel sulfamate and nickel bromide in water;
step 2, adding boric acid and adjusting the pH value of the solution;
step 3, adding a wetting agent and a stress regulator in sequence, fully stirring and uniformly mixing;
and 4, sequentially adding a dispersing agent and the modified nano aluminum oxide particles, fully stirring, and uniformly mixing to obtain the nickel sulfamate electroplating solution.
In some embodiments of the invention, in step 1, the high purity nickel sulfamate is added in an amount of 300 to 750g (e.g., 300g, 310g, 320g, 330g, 340g, 350g, 360g, 370g, 380g, 390g, 400g, 410g, 420g, 430g, 440g, 450g, 460g, 470g, 480g, 490g, 500g, 510g, 520g, 530g, 540g, 550g, 560g, 570g, 580g, 590g, 600g, 610g, 620g, 630g, 640g, 650 g) relative to 1L of the plating solution, and the nickel bromide is added in an amount of 10 to 20g (e.g., 10g, 12g, 14g, 16g, 18g, 20 g).
In some embodiments of the invention, in step 2, the boric acid has a concentration of 30 to 50g/L (e.g., 30g/L, 32g/L, 34g/L, 36g/L, 38g/L, 40g/L, 42g/L, 44g/L, 46g/L, 48g/L, 50 g/L) and a pH of 3 to 4.2 (e.g., 3, 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9, 4.0, 4.1, 4.2).
In some embodiments of the invention, in step 3, the wetting agent is added in an amount of 0.5 to 2g (e.g., 0.5g, 0.7g, 1g, 1.5g, 1.75g, 2 g) and the stress modifier is added in an amount of 5 to 15g (e.g., 5g, 5.5g, 6g, 6.5g, 7g, 7.5g, 8g, 8.5g, 9g, 9.5g, 10g, 10.5g, 11g, 11.5g, 12g, 12.5g, 13g, 13.5g, 14g, 14.5g, 15 g) relative to 1L of the plating solution.
In some embodiments of the present invention, in step 4, the dispersant is added in an amount of 2 to 5g (e.g., 2g, 2.5g, 3g, 3.5g, 4g, 4.5g, 5 g) and the modified nano-alumina particles are added in an amount of 10 to 20g (e.g., 10g, 12g, 14g, 16g, 18g, 20 g) relative to 1L of the plating solution.
In some embodiments of the present invention, the wetting agent is selected from any one of sodium lauryl sulfate, sodium 2-ethylhexyl sulfate, sodium dipentyl sulfosuccinate, sodium methallylsulfonate, or a combination of at least two thereof; preferably, the wetting agent is selected from any one of sodium dodecyl sulfate, sodium dipentyl sulfosuccinate and sodium methallyl sulfonate or the combination of at least two of the above.
In some embodiments of the invention, the dispersant is selected from any one of sodium dodecylbenzene sulfonate, polyethylene glycol octylphenyl ether, or a combination of at least two thereof.
In some embodiments of the present invention, the dispersant is sodium dodecylbenzene sulfonate and polyethylene glycol octyl phenyl ether in a mass ratio of (2-3): (1-2) in a mass ratio of preferably 2:1.
in some embodiments of the invention, the stress modifier is selected from any one of saccharin, sodium naphthalenetrisulfonate, 4-methoxybenzothiazole, or a combination of at least two thereof.
In some embodiments of the invention, the stress modifier is saccharin, sodium naphthalenetrisulfonate, and 4-methoxybenzothiazole in a mass ratio of (0.5-1): (0.65-1): (1-1.5) in a mass ratio of preferably 0.5:0.65:1.
in some embodiments of the invention, the high purity nickel sulfamate is prepared by an ion exchange method, which mainly comprises the following preparation steps:
(1) Column assembling:
filling resin into a glass fiber reinforced plastic ion exchange column, wherein the ion exchange resin is cation resin with macroporous weak acidity, and filling the resin into the exchange column;
(2) Transformation and washing of ion exchange resin:
introducing 5-8% of sodium hydroxide by mass into an exchange column to transform the resin contained in the exchange column, and washing the ion exchange resin with pure water after alkaline washing is finished until the ion exchange resin is washed clean;
(3) Exchange of nickel ions:
introducing a nickel salt solution from the upper end of the treated exchange column until the resin is saturated in adsorption;
(4) Preparation of nickel sulfamate:
introducing saturated sulfamic acid solution from the upper end of the exchange column, collecting effluent liquid, and continuously passing through the column until the exchange is finished;
(5) Concentrating the nickel sulfamate solution:
and carrying out reduced pressure distillation on the nickel sulfamate solution to obtain the high-purity nickel sulfamate.
In some embodiments of the invention, in step (1) packing the column, the ion exchange column has a size of
In some embodiments of the invention, in step (1), the packing height of the resin in the column is from 1/3 to 2/3 of the column.
In some embodiments of the present invention, in the step (2) of transforming and washing the ion exchange resin, the indication that the ion exchange resin is washed clean is that the lye is judged to be washed clean after detecting that the pH of the water is less than 7.
In some embodiments of the present invention, in the exchanging of nickel ions in step (3), the nickel salt solution has a nickel ion concentration of 40g/L to 60g/L.
In some embodiments of the invention, in the exchange of nickel ions in step (3), the saturation of the resin adsorption is marked by the consistency of the concentration of nickel ions in the feed solution and the concentration of nickel ions in the effluent solution.
In some embodiments of the invention, in the preparation of nickel sulfamate in step (4), the indication of completion of the exchange is that the concentration of nickel ions in the feed solution and the concentration of nickel ions in the effluent solution are the same.
In some embodiments of the invention, the high purity nickel sulfamate is prepared by an ion exchange method, which mainly comprises the following preparation steps:
(1) Column assembling:
by using
The glass fiber reinforced plastic ion exchange column with excellent corrosion resistance and higher strength contains resin, wherein the ion exchange resin is polyacrylic acid series macroporous weak acid cation resin, and the resin is filled at the position 1/3-2/3 of the height of the exchange column;
(2) Transformation and washing of ion exchange resin:
introducing 5-8% by mass of sodium hydroxide into the exchange column at a certain flow rate to transform the resin contained in the exchange column, washing the ion exchange resin with pure water again after the alkali washing is finished, detecting the pH value of the water, judging that the alkali liquor is washed clean when the pH value is less than 7, and recovering the washing water;
(3) Exchange of nickel ions:
taking a nickel salt solution with the nickel ion concentration of 40g/L-60g/L, introducing the nickel salt solution from the upper end of the treated exchange column at a certain flow rate, exchanging nickel ions in the exchange column with sodium ions on the resin, and continuously introducing the nickel salt solution until the concentration of the effluent liquid is equal to that of the nickel ions introduced into the solution, which indicates that the resin is saturated by adsorption;
(4) Preparation of nickel sulfamate:
preparing saturated sulfamic acid solution, introducing the saturated sulfamic acid solution from the upper end of an exchange column at a certain flow rate, exchanging hydrogen ions in the exchange column with nickel ions adsorbed on resin at the moment, collecting the effluent liquid which is the nickel sulfamic acid solution, and continuously passing through the column until the concentration of nickel ions in the added liquid is consistent with that of the nickel ions in the effluent liquid, which indicates that the nickel ions are completely exchanged;
(5) Concentrating the nickel sulfamate solution:
and carrying out reduced pressure distillation on the obtained nickel sulfamate solution to finally prepare the high-purity nickel sulfamate.
In some embodiments of the invention, in step (4), the invention increases the concentration of nickel ions from 40g/L to 50g/L to 180g/L to 190g/L by passing the saturated sulfamic acid solution through 3 ion exchange columns which are treated in series.
In some embodiments of the present invention, the preparation method of the modified nano alumina particles comprises the following steps:
preparation of (mono) polymethacrylic acid:
a. adding ammonium persulfate into a flask, and stirring in pure water until the ammonium persulfate is completely dissolved;
b. heating and continuously stirring, and sequentially adding methacrylic acid and isopropanol;
c. ammonium persulfate and methacrylic acid are uniformly mixed in pure water and added into the system through a dropping funnel at the temperature of 60-70 ℃;
d. after the dropwise addition is finished, the reaction is carried out for 0.5 to 2 hours at the temperature of between 80 and 90 ℃;
e. after the reaction is finished, placing the system in an ice-water bath, adding sodium hydroxide while stirring, and adjusting the pH to 5.5-6 to prepare polymethacrylic acid;
(II) preparing modified nano aluminum oxide particles:
uniformly mixing polymethacrylic acid and nano aluminum oxide powder, dispersing for 10-20 min by using a stirrer, and then dispersing for 20-40 min by using an ultrasonic cell crusher to prepare the modified nano aluminum oxide particles.
In some embodiments of the present invention, the preparation method of the modified nano alumina particles comprises the following steps:
preparation of (I) polymethacrylic acid:
a. adding ammonium persulfate into a flask, and stirring in pure water until the ammonium persulfate is completely dissolved;
b. heating and continuously stirring, and sequentially adding methacrylic acid and isopropanol;
c. uniformly mixing ammonium persulfate and methacrylic acid in pure water, adding into the system from a dropping funnel at the temperature of 60-70 ℃, and controlling the dropping time to be 20-40 min;
d. after the dropwise addition is finished, the reaction is carried out for 0.5 to 2 hours at the temperature of between 80 and 90 ℃;
e. after the reaction is finished, placing the system in an ice-water bath, adding sodium hydroxide with the mass fraction of 20-40% while stirring, and adjusting the pH to 5.5-6 to prepare polymethacrylic acid;
(II) preparing modified nano aluminum oxide particles:
uniformly mixing polymethacrylic acid and nano-alumina powder (the mass ratio of the polymethacrylic acid to the nano-alumina powder is (4-8): (6-2)), dispersing for 10-20 min by using a stirrer, and then dispersing for 20-40 min by using an ultrasonic cell crusher to prepare the modified nano-alumina particles.
In some embodiments of the present invention, the modified nano alumina particles have a particle size of about 50 to about 60nm.
On the other hand, the invention provides an application of the nickel sulfamate electroplating solution prepared by the preparation method in nickel plating of aluminum-magnesium alloy.
Has the advantages that:
(1) The method for preparing the nickel sulfamate by the ion exchange method has the advantages of simple process, convenient operation, low cost and the like, can prepare the nickel sulfamate with high purity and ultralow metal ion content, and can greatly improve the use effect of the nickel sulfamate in an electroplating solution system;
(2) The aluminum oxide nano particles have a great deal of excellent performances such as large specific surface area, high melting point, good thermal stability, high hardness, excellent water absorption, good electrical insulation performance, acid and alkali corrosion resistance and the like, but have large specific surface area, high surface energy and easy agglomeration, and meanwhile, because the aluminum oxide surface contains abundant-OH groups, hydrogen bonds are easy to form, and a grafting phenomenon is formed among particles under the action of the hydrogen bonds, so that the powder agglomeration is serious;
(3) According to the invention, three stress-removing agents are compounded for use, so that the effect of removing gravitation is better achieved, and the bonding strength between the nickel-plated layer and the base material is better; the composite stress remover is added, so that the effect of reducing or completely eliminating the internal stress of the nickel plating layer is achieved, and the obtained nickel plating layer is fine and uniform and has good brightness effect.
Detailed Description
The invention will be illustrated with reference to specific embodiments. It should be noted that the following examples are illustrative of the present invention, and are not intended to limit the present invention. Other combinations and various modifications within the spirit or scope of the present invention may be made without departing from the spirit or scope of the present invention.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below. In the following embodiments, those whose manipulations are not indicated are carried out according to conventional conditions or conditions recommended by the manufacturer.
Preparation of high-purity nickel sulfamate
(1) Column assembling:
by using
The glass fiber reinforced plastic ion exchange column with excellent corrosion resistance and higher strength contains resin, wherein the ion exchange resin is polyacrylic acid series macroporous weak acid cation resin, and the resin is filled to the position 2/3 of the height of the exchange column;
(2) Transformation and washing of ion exchange resin:
introducing sodium hydroxide with the mass fraction of 5% into an exchange column at a certain flow rate to transform the resin contained in the exchange column, washing the ion exchange resin again by using pure water after the alkali washing is finished, detecting the pH value of water, judging that the alkali liquor is washed clean when the pH value is less than 7, and recovering the washing water;
(3) Exchange of nickel ions:
taking a nickel salt solution with the nickel ion concentration of 50g/L, introducing the nickel salt solution from the upper end of the treated exchange column, exchanging nickel ions in the exchange column with sodium ions on the resin, and continuously introducing the nickel salt solution until the concentrations of the effluent liquid and the nickel ions introduced into the solution are equal, which indicates that the resin is saturated by adsorption;
(4) Preparation of nickel sulfamate:
preparing saturated sulfamic acid solution, introducing the saturated sulfamic acid solution from the upper end of the exchange column, exchanging hydrogen ions in the exchange column with nickel ions adsorbed on the resin, collecting effluent liquid which is nickel sulfamic acid solution, and continuously passing through the column until the concentration of nickel ions in the added liquid is consistent with that of the nickel ions in the effluent liquid, which indicates that the nickel ions are completely exchanged;
(5) Concentrating the nickel sulfamate solution:
and carrying out reduced pressure distillation on the obtained nickel sulfamate solution to finally prepare high-purity nickel sulfamate for later use.
Preparation of modified nano-alumina particles
Preparation of (I) polymethacrylic acid:
a. 2g of ammonium persulfate is added into a flask and stirred in pure water until the ammonium persulfate is completely dissolved;
b. heating and continuously stirring, and sequentially adding 20g of methacrylic acid and 2g of isopropanol until the methacrylic acid and the isopropanol are fully dissolved;
c. uniformly mixing 4g of ammonium persulfate and 160g of methacrylic acid in pure water, heating the system to 65 ℃, adding the mixture into the system through a dropping funnel, and controlling the dropping time to be 30min;
d. after the dropwise addition is finished, reacting for 1h at the temperature of 90 ℃ in a heat preservation manner;
e. after the reaction is finished, placing the system in an ice-water bath, dropwise adding sodium hydroxide with the mass fraction of 30% while stirring, and adjusting the pH to 5.7 to prepare polymethacrylic acid;
(II) preparing modified nano aluminum oxide particles:
uniformly mixing polymethacrylic acid and nano aluminum oxide powder (the mass ratio of the polymethacrylic acid to the nano aluminum oxide powder is 6.
Example 1
Step 1, adding 550g of high-purity nickel sulfamate and 15g of nickel bromide into 1L of water, and uniformly mixing;
step 2, adding 30g/L boric acid, and adjusting the pH of the solution to be =3;
step 3, sequentially adding 1.5g of sodium dodecyl sulfate and 10g of stress regulator (a mixture of saccharin, sodium naphthalenetrisulfonate and 4-methoxybenzothiazole in a mass ratio of 0.5;
and step 4, sequentially adding 3.4g of a dispersing agent (a mixture of sodium dodecyl benzene sulfonate and polyethylene glycol octyl phenyl ether in a mass ratio of 2: 1) and 12g of modified nano aluminum oxide particles, fully stirring, and uniformly mixing to obtain the nickel sulfamate electroplating solution.
Example 2
Step 1, adding 600g of high-purity nickel sulfamate and 10g of nickel bromide into 1L of water, and uniformly mixing in the water;
step 2, adding 35g/L boric acid, and adjusting the pH of the solution to be =3.3;
step 3, sequentially adding 0.6g of sodium dipentyl sulfosuccinate and 15g of a stress regulator (a mixture of saccharin, sodium naphthalenetrisulfonate and 4-methoxybenzothiazole in a mass ratio of 0.5;
and 4, sequentially adding 3g of dispersing agent (a mixture of sodium dodecyl benzene sulfonate and polyethylene glycol octyl phenyl ether in a mass ratio of 2.
Example 3
Step 1, adding 660g of high-purity nickel sulfamate and 13g of nickel bromide into 1L of water, and uniformly mixing;
step 2, adding 33g/L boric acid, and adjusting the pH of the solution to be =3.7;
step 3, sequentially adding 1.2g of sodium dodecyl sulfate and 8.5g of a stress regulator (a mixture of saccharin, sodium naphthalenetrisulfonate and 4-methoxybenzothiazole in a mass ratio of 0.5;
and 4, sequentially adding 3.4g of a dispersing agent (a mixture of sodium dodecyl benzene sulfonate and polyethylene glycol octyl phenyl ether in a mass ratio of 2: 1) and 13g of modified nano aluminum oxide particles, fully stirring, and uniformly mixing to obtain the nickel sulfamate electroplating solution.
Example 4
Step 1, adding 480g of high-purity nickel sulfamate and 20g of nickel bromide into 1L of water, and uniformly mixing;
step 2, adding 30g/L boric acid, and adjusting the pH of the solution to be =4;
step 3, sequentially adding 2g of sodium dipentyl sulfosuccinate and 10g of a stress regulator (a mixture of saccharin, sodium naphthalenetrisulfonate and 4-methoxybenzothiazole in a mass ratio of 0.5;
and 4, sequentially adding 2.3g of a dispersing agent (a mixture of sodium dodecyl benzene sulfonate and polyethylene glycol octyl phenyl ether in a mass ratio of 2: 1) and 18g of modified nano aluminum oxide particles, fully stirring, and uniformly mixing to obtain the nickel sulfamate electroplating solution.
Example 5
Step 1, adding 350g of high-purity nickel sulfamate and 18g of nickel bromide into 1L of water, and uniformly mixing;
step 2, adding 40g/L boric acid, and adjusting the pH of the solution to be =4;
step 3, sequentially adding 2g of sodium methallyl sulfonate and 14g of stress regulator (a mixture of saccharin, sodium naphthalenetrisulfonate and 4-methoxybenzothiazole in a mass ratio of 0.5;
and 4, sequentially adding 3.8g of a dispersing agent (a mixture of sodium dodecyl benzene sulfonate and polyethylene glycol octyl phenyl ether in a mass ratio of 2: 1) and 19g of modified nano aluminum oxide particles, fully stirring, and uniformly mixing to obtain the nickel sulfamate electroplating solution.
Example 6
Step 1, adding 700g of high-purity nickel sulfamate and 15g of nickel bromide into 1L of water, and uniformly mixing;
step 2, adding 45g/L boric acid, and adjusting the pH of the solution to be =4;
step 3, sequentially adding 2g of sodium dodecyl sulfate and 14g of a stress regulator (a mixture of saccharin, sodium naphthalenetrisulfonate and 4-methoxybenzothiazole in a mass ratio of 0.5;
and step 4, sequentially adding 4g of dispersing agent (a mixture of sodium dodecyl benzene sulfonate and polyethylene glycol octyl phenyl ether in a mass ratio of 2 to 1) and 15g of modified nano aluminum oxide particles, fully stirring, and uniformly mixing to obtain the nickel sulfamate electroplating solution.
Example 7
Step 1, adding high-purity nickel sulfamate and nickel bromide into 1L of water, and uniformly mixing;
step 2, adding boric acid and adjusting the pH value of the solution;
step 3, adding a wetting agent and a stress regulator in sequence, fully stirring and uniformly mixing;
and 4, sequentially adding a dispersing agent and the modified nano aluminum oxide particles, fully stirring, and uniformly mixing to obtain the nickel sulfamate electroplating solution.
(2) Dissolving the aluminum-magnesium alloy matrix material by using acetone, ultrasonically cleaning by using ultrasonic waves after dissolving, and washing for 10min at room temperature; using NaOH and Na 3 PO 4 The mixed solution (the volume ratio of NaOH to Na3PO4 is 1) is used for cleaning dirt and grease on the surface of the substrate, and the cleaning time is 10min at 60 ℃; washing with 5% dilute hydrochloric acid for 2min;
(3) Heating nickel sulfamate electroplating solution to 50 ℃;
(4) Aluminum-magnesium alloy base materialPutting the material into nickel sulfamate electroplating solution for nickel plating, wherein the nickel plating time is 1h, and the current density is 1.5A/dm 2 ；
(5) Finally obtaining the aluminum magnesium alloy base material with the nickel plating layer, wherein the size of the aluminum magnesium alloy base material is 150mm multiplied by 25mm multiplied by 1mm, and the thickness of the nickel layer is 1.5 mu m.
The above-mentioned serial numbers of the embodiments of the present invention are only for description, and do not represent the advantages and disadvantages of the embodiments.
Comparative example 1
Commercial nickel sulfamate electroplating baths
Comparative example 2
Step 1, adding 550g of high-purity nickel sulfamate and 15g of nickel bromide into 1L of water, and uniformly mixing in the water;
step 2, adding 30g/L boric acid, and adjusting the pH of the solution to be =3;
step 3, sequentially adding 1.5g of sodium dodecyl sulfate and 10g of a stress regulator (a mixture of saccharin, sodium naphthalenetrisulfonate and 4-methoxybenzothiazole in a mass ratio of 0.5;
and step 4, sequentially adding 3.4g of dispersing agent (a mixture of sodium dodecyl benzene sulfonate and polyethylene glycol octyl phenyl ether in a mass ratio of 2 to 1) and 6g of modified nano aluminum oxide particles, fully stirring, and uniformly mixing to obtain the nickel sulfamate electroplating solution.
Comparative example 3
Step 1, adding 550g of high-purity nickel sulfamate and 15g of nickel bromide into 1L of water, and uniformly mixing;
step 2, adding 30g/L boric acid, and adjusting the pH of the solution to be =3;
step 3, sequentially adding 1.5g of sodium dodecyl sulfate and 10g of stress regulator (a mixture of saccharin, sodium naphthalenetrisulfonate and 4-methoxybenzothiazole in a mass ratio of 0.5;
and 4, sequentially adding 3.4g of dispersing agent (a mixture of sodium dodecyl benzene sulfonate and polyethylene glycol octyl phenyl ether in a mass ratio of 2).
The nickel sulfamate baths prepared in examples 1 to 7 were tested for the content of metal impurities using ICPMS as compared to the content of metal impurities in the nickel sulfamate baths of comparative examples 1 to 3 in table 1 below.
TABLE 1 content of metal impurities in the nickel sulfamate used in the comparative examples in the examples
Using the nickel sulfamate plating solutions of examples 1 to 7 and comparative examples 1 to 3, an aluminum magnesium alloy substrate was nickel-plated as follows:
(1) Dissolving the aluminum-magnesium alloy matrix material by using acetone, ultrasonically cleaning by using ultrasonic waves after dissolving, and washing for 10min at room temperature; using NaOH and Na 3 PO 4 The mixed solution (the volume ratio of NaOH to Na3PO4 is 1) is used for cleaning dirt and grease on the surface of the substrate, and the cleaning time is 10min at 60 ℃; washing with 5% dilute hydrochloric acid for 2min;
(2) Heating nickel sulfamate electroplating solution to 50 ℃;
(3) Putting the aluminum-magnesium alloy base material into nickel sulfamate electroplating solution for nickel plating, wherein the nickel plating time is 1h, and the current density is 1.5A/dm 2 ；
(4) Finally obtaining the aluminum magnesium alloy base material with the nickel plating layer, wherein the size of the aluminum magnesium alloy base material is 150mm multiplied by 25mm multiplied by 1mm, and the thickness of the nickel layer is 1.5 mu m.
In the above examples, the sizes of the substrates (aluminum magnesium alloys) used in the comparative examples were all the same, and were 30mm × 50mm × 1mm.
The performance and test method comprises the following steps:
testing the binding force of the composite coating: and (3) carrying out 180-degree bending test according to a test method in the national standard GB 232-2010, and observing whether visible cracks appear on a plating layer on the surface of the aluminum-magnesium alloy by naked eyes, wherein the aluminum-magnesium alloy is qualified if the visible cracks do not appear, and is unqualified if the visible cracks do not appear.
And (3) testing neutral salt spray: and (3) putting the product into a salt spray box, spraying a NaCl solution with neutral pH value through a spraying device, further settling on the surface of the iron sheet, corroding for 10h to observe the corrosion condition of the aluminum-magnesium alloy surface coating, and recording the time (h) when the corrosion points appear on the surface.
And (3) hardness testing: and (3) carrying out a plating hardness test on the product: the hardness test was performed using an HR-150A Rockwell hardness tester.
And (4) internal stress testing: the test method of Zhang Huacheng et al (such as Ying, wangsui, tangji, low-stress high-speed nickel plating, surface technique, 1992, vol21, (1): 25-29) is adopted.
According to the embodiment and the test result of the proportion, the preparation method of the high-purity nickel sulfamate electroplating solution provided by the invention can effectively remove metal impurities such as Co, cu, fe, zn, mn, ca, mg, cr and the like in the electroplating solution, and the aluminum-magnesium alloy matrix material with the nickel plating layer prepared from the high-purity nickel sulfamate electroplating solution has the advantages of higher neutral salt haze value, better bonding performance, higher hardness value, lower internal stress value, better mechanical property and corrosion resistance, simple preparation method and low cost.
The above embodiments are provided only for illustrating the technical idea and features of the present invention, and the purpose of the present invention is to provide those skilled in the art with understanding and implementing the present invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (10)
1. The preparation method of the nickel sulfamate electroplating solution is characterized by comprising the following steps of:
step 1, uniformly mixing high-purity nickel sulfamate and nickel bromide in water;
step 2, adding boric acid and adjusting the pH value of the solution;
step 3, adding the wetting agent and the stress regulator in sequence, fully stirring and uniformly mixing;
and 4, sequentially adding a dispersing agent and the modified nano aluminum oxide particles, fully stirring, and uniformly mixing to obtain the nickel sulfamate electroplating solution.
2. The production method according to claim 1, wherein in the step 1, the high-purity nickel sulfamate is added in an amount of 300 to 750g and the nickel bromide is added in an amount of 10 to 20g, relative to 1L of the plating solution; in the step 2, the concentration of the boric acid is 30-50g/L; in the step 3, the addition amount of the wetting agent is 0.5-2g, and the addition amount of the stress regulator is 5-15g; in the step 4, the addition amount of the dispersing agent is 2-5g, and the addition amount of the modified nano aluminum oxide particles is 10-20g.
3. The preparation method according to claim 1, wherein the wetting agent is selected from any one of sodium dodecyl sulfate, sodium 2-ethylhexyl sulfate, sodium dipentyl sulfosuccinate, sodium methallyl sulfonate, or a combination of at least two of them.
4. The preparation method according to claim 1, wherein the dispersant is the sodium dodecyl benzene sulfonate and the polyethylene glycol octyl phenyl ether in a mass ratio of (2-3): (1-2).
5. The preparation method according to claim 1, wherein the stress regulator is saccharin, sodium naphthalenetrisulfonate and 4-methoxybenzothiazole in a mass ratio of (0.5-1): (0.65-1): (1-1.5).
6. The preparation method according to claim 1, wherein the high-purity nickel sulfamate is prepared by an ion exchange method, and the preparation method mainly comprises the following steps:
(1) Column assembling:
filling resin into a glass fiber reinforced plastic ion exchange column, wherein the ion exchange column is filled with the resin, and the ion exchange resin is cation resin with macropore and weak acidity;
(2) Transformation and washing of ion exchange resin:
introducing 5-8% of sodium hydroxide by mass into an exchange column to transform the resin contained in the exchange column, and washing the ion exchange resin with pure water after alkaline washing is finished until the ion exchange resin is washed clean;
(3) Exchange of nickel ions:
introducing a nickel salt solution from the upper end of the treated exchange column until the resin is saturated in adsorption;
(4) Preparation of nickel sulfamate:
introducing saturated sulfamic acid solution from the upper end of the exchange column, collecting effluent liquid, and continuously passing through the column until the exchange is finished;
(5) Concentrating the nickel sulfamate solution:
and carrying out reduced pressure distillation on the nickel sulfamate solution to obtain the high-purity nickel sulfamate.
7. The method according to claim 7, wherein in the step (1), the packing height of the resin in the exchange column is 1/3-2/3 of the position of the exchange column; in the step (2), during the transformation and washing of the ion exchange resin, the mark for washing the ion exchange resin is that the alkali liquor is judged to be washed clean after the pH value of the detected water is less than 7; in the exchange of nickel ions in the step (3), the concentration of the nickel ions in the nickel salt solution is 40g/L-60g/L, and the mark of resin adsorption saturation is that the concentration of the nickel ions in the added liquid is consistent with that of the nickel ions in the effluent liquid; in the step (4) of preparing the nickel sulfamate, the sign of the completion of the exchange is that the concentration of the nickel ions in the added liquid is consistent with that of the nickel ions in the effluent liquid.
8. The preparation method according to claim 1, wherein the preparation method of the modified nano alumina particles comprises the following steps:
preparation of (I) polymethacrylic acid:
a. adding ammonium persulfate into a flask, and stirring in pure water until the ammonium persulfate is completely dissolved;
b. heating and continuously stirring, and sequentially adding methacrylic acid and isopropanol;
c. ammonium persulfate and methacrylic acid are uniformly mixed in pure water and added into the system through a dropping funnel at the temperature of 60-70 ℃;
d. after the dropwise addition is finished, reacting for 0.5-2 h at the temperature of 80-90 ℃ in a heat preservation manner;
e. after the reaction is finished, placing the system in an ice-water bath, adding sodium hydroxide while stirring, and adjusting the pH to 5.5-6 to prepare polymethacrylic acid;
(II) preparing modified nano aluminum oxide particles:
uniformly mixing polymethacrylic acid and nano aluminum oxide powder, dispersing for 10-20 min by using a stirrer, and then dispersing for 20-40 min by using an ultrasonic cell crusher to prepare the modified nano aluminum oxide particles.
9. The preparation method according to claim 9, wherein the modified nano alumina particles have a particle size of about 50 to 60nm.
10. Use of a nickel sulfamate electroplating solution prepared by the preparation method of any one of claims 1 to 9 in nickel plating of aluminum magnesium alloys.
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