CN117001208B - Zero-halogen no-clean soldering flux - Google Patents
Zero-halogen no-clean soldering flux Download PDFInfo
- Publication number
- CN117001208B CN117001208B CN202311065269.3A CN202311065269A CN117001208B CN 117001208 B CN117001208 B CN 117001208B CN 202311065269 A CN202311065269 A CN 202311065269A CN 117001208 B CN117001208 B CN 117001208B
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- Prior art keywords
- halogen
- zero
- clean
- surfactant
- flux
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- 230000004907 flux Effects 0.000 title claims abstract description 90
- 238000005476 soldering Methods 0.000 title claims abstract description 72
- 229910052736 halogen Inorganic materials 0.000 title claims abstract description 58
- 239000004094 surface-active agent Substances 0.000 claims abstract description 68
- 150000001720 carbohydrates Chemical class 0.000 claims abstract description 43
- 150000001875 compounds Chemical class 0.000 claims abstract description 23
- 230000000694 effects Effects 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 5
- -1 acetyl bromolactose Chemical compound 0.000 claims description 36
- 150000002367 halogens Chemical class 0.000 claims description 28
- 238000002360 preparation method Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- NRLPPGBADQVXSJ-UHFFFAOYSA-N 4-sulfanylbenzaldehyde Chemical compound SC1=CC=C(C=O)C=C1 NRLPPGBADQVXSJ-UHFFFAOYSA-N 0.000 claims description 14
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims description 12
- 239000013543 active substance Substances 0.000 claims description 12
- 230000007797 corrosion Effects 0.000 claims description 12
- 238000005260 corrosion Methods 0.000 claims description 12
- 239000003112 inhibitor Substances 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- 239000006184 cosolvent Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 2
- 238000003466 welding Methods 0.000 abstract description 26
- 230000007480 spreading Effects 0.000 abstract description 10
- 238000003892 spreading Methods 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 7
- 150000002366 halogen compounds Chemical class 0.000 abstract description 4
- 239000004925 Acrylic resin Substances 0.000 description 29
- 229920000178 Acrylic resin Polymers 0.000 description 29
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 26
- 238000012360 testing method Methods 0.000 description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 14
- IGZSSKAOSOCVPH-UHFFFAOYSA-N 2-(morpholin-4-ylmethyl)prop-2-enoic acid Chemical compound OC(=O)C(=C)CN1CCOCC1 IGZSSKAOSOCVPH-UHFFFAOYSA-N 0.000 description 12
- 238000009413 insulation Methods 0.000 description 12
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 12
- ZSZRUEAFVQITHH-UHFFFAOYSA-N 2-(2-methylprop-2-enoyloxy)ethyl 2-(trimethylazaniumyl)ethyl phosphate Chemical compound CC(=C)C(=O)OCCOP([O-])(=O)OCC[N+](C)(C)C ZSZRUEAFVQITHH-UHFFFAOYSA-N 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 8
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 239000000178 monomer Substances 0.000 description 8
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 8
- 239000000523 sample Substances 0.000 description 8
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 7
- 229960004543 anhydrous citric acid Drugs 0.000 description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 7
- 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 6
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 6
- 238000010248 power generation Methods 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 5
- 230000001804 emulsifying effect Effects 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 description 4
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 239000001530 fumaric acid Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 229960004889 salicylic acid Drugs 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000011975 tartaric acid Substances 0.000 description 4
- 235000002906 tartaric acid Nutrition 0.000 description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 4
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- XTDYIOOONNVFMA-UHFFFAOYSA-N dimethyl pentanedioate Chemical compound COC(=O)CCCC(=O)OC XTDYIOOONNVFMA-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229960002598 fumaric acid Drugs 0.000 description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 3
- 229920000053 polysorbate 80 Polymers 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 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 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- 235000019484 Rapeseed oil Nutrition 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- RZXWRJCGZANKDL-UHFFFAOYSA-N azepan-1-ium;benzoate Chemical compound C1CCC[NH2+]CC1.[O-]C(=O)C1=CC=CC=C1 RZXWRJCGZANKDL-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- 239000003729 cation exchange resin Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- CYJMVNWBACJNLK-UHFFFAOYSA-N cyclohexanamine;3-phenylprop-2-enoic acid Chemical compound NC1CCCCC1.OC(=O)C=CC1=CC=CC=C1 CYJMVNWBACJNLK-UHFFFAOYSA-N 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- 238000007405 data analysis Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- DDRPCXLAQZKBJP-UHFFFAOYSA-N furfurylamine Chemical compound NCC1=CC=CO1 DDRPCXLAQZKBJP-UHFFFAOYSA-N 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- NHBKWZCTSMCKDS-UHFFFAOYSA-N undecan-2-amine Chemical compound CCCCCCCCCC(C)N NHBKWZCTSMCKDS-UHFFFAOYSA-N 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000005406 washing Methods 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
- CWLKGDAVCFYWJK-UHFFFAOYSA-N 3-aminophenol Chemical compound NC1=CC=CC(O)=C1 CWLKGDAVCFYWJK-UHFFFAOYSA-N 0.000 description 1
- 229940018563 3-aminophenol Drugs 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229940114081 cinnamate Drugs 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 229960004275 glycolic acid Drugs 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010405 reoxidation reaction Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 1
- 239000001433 sodium tartrate Substances 0.000 description 1
- 229960002167 sodium tartrate Drugs 0.000 description 1
- 235000011004 sodium tartrates Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- WBYWAXJHAXSJNI-VOTSOKGWSA-M trans-cinnamate Chemical compound [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
- B23K35/3613—Polymers, e.g. resins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/362—Selection of compositions of fluxes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention discloses a zero-halogen no-clean soldering flux, which relates to the technical field of soldering fluxes and comprises a compound surfactant; the compound surfactant comprises a saccharide surfactant, and the chemical structure of the compound surfactant is shown as formula I: The zero-halogen no-clean soldering flux provided by the invention has more excellent soldering effect, the spreading capability is obviously improved, the soldering film forming stability is good in a wet and hot environment, no halogen compound is contained, the activity of the welding process is high, the welding spot is full, and the post-welding reliability effect of electronic products is ensured.
Description
Technical Field
The invention belongs to the technical field of soldering fluxes, and particularly relates to a zero-halogen no-clean soldering flux.
Background
In recent years, the national and even global importance is placed on environmental protection problems, and some traditional industries are replaced by environmental protection technologies gradually along with the gradual reduction of market share of the traditional industries, such as solar photovoltaic power generation technology, the occupation ratio of the traditional industries in a national power generation system is heavier and heavier, so that consumption of some non-renewable energy sources can be reduced, and the creation of clean renewable energy sources for human beings is a great trend of future environmental protection; at present, renewable energy sources are focused worldwide, and the development and application of solar photovoltaic power generation technology are exactly renewable energy sources, and solar energy is used as clean, safe and inexhaustible energy sources, can change the energy source structure of human beings, maintains sustainable development, and is a necessary trend and optimal choice for the world energy source convertibility development.
The core in the technical field of solar photovoltaic power generation is a photovoltaic module, and a whole power generation system is assembled by using the photovoltaic module; in the assembly process, the battery piece (monocrystalline silicon and polycrystalline silicon) and the welding strip (bus bar and cross flow bar) are welded together by a series welding machine to form a minimum power generation unit, and the welding strip (bus bar and cross flow bar) is an important component part; the traditional special soldering flux for the photovoltaic solder strip has the problems of high solid content, easiness in residue on the surface of a tin furnace, poor uniformity of a tin surface and large void ratio; the halide content is high, which is extremely harmful to the environment. The existing photovoltaic soldering flux on the market basically takes alcohols as solvents, the soldering flux has low boiling point, is extremely volatile, is flammable and explosive, has a certain harm to the environment and human body, is more crystallized in the actual welding process, has a certain corrosion to a series welding machine, needs to be stopped periodically to clean the crystallization, influences the production efficiency of components, and increases the maintenance cost of the machine. Aiming at the current welding and crystallization situations of the current soldering flux, a soldering flux manufacturer is actively improved, and on the premise of not changing the existing production process and equipment, the environment-friendly solar photovoltaic soldering tape soldering flux which can keep excellent weldability and achieve the best welding effect in extremely short welding time, does not generate residues, or does not corrode a soldering tape after welding, and meets the requirements of related laws and regulations is completely met.
Disclosure of Invention
The invention aims to provide the zero-halogen no-clean soldering flux which has more excellent soldering effect, obviously improves spreading capability, has good soldering film forming stability in a wet and hot environment, does not contain halogen compounds, has high activity in a welding process and full welding spots, and ensures the post-welding reliability effect of electronic products.
The technical scheme adopted by the invention for achieving the purpose is as follows:
A saccharide surfactant has a chemical structure shown in formula I:
The invention adopts acetyl bromolactose, 4-mercaptobenzaldehyde and amino ethyl piperazine to prepare the saccharide surfactant, has a novel chemical structure, obviously improves the surface activity, can effectively reduce the oil-water interfacial tension, and obviously enhances the emulsifying property; the halogen-free no-clean soldering flux is applied to the soldering flux, and the spreading capability of the obtained zero-halogen no-clean soldering flux is effectively enhanced; meanwhile, the soldering flux has more excellent weldability, the welding effect is enhanced, and the change rate of the insulation resistance value of the protective film formed by soldering in a wet and hot environment is obviously reduced. The reason for this may be that the novel saccharide surfactant prepared by the present invention can significantly reduce the surface tension of the flux system during the soldering process, and increase the wettability between the flux and the substrate metal; and the active groups contained in the structure can promote the welding effect, and the active groups are matched with other components such as film forming agents for use, so that the weldability of the soldering flux can be effectively improved, and the welding effect is enhanced.
The preparation method of the carbohydrate surfactant shown in the formula I comprises the following steps:
Step 1: reacting acetyl bromolactose and 4-mercaptobenzaldehyde under the condition of a catalyst, and then removing acetyl for protection under the action of sodium methoxide to obtain an intermediate M;
step 2: and mixing the intermediate M with amino ethyl piperazine to react to obtain the saccharide surfactant.
The catalyst in step 1 includes n-butyllithium.
Further specifically, the preparation method of the saccharide surfactant comprises the following steps:
Step 1: dissolving acetyl bromolactose in CH 3 CN, adding n-butyllithium and 4-mercaptobenzaldehyde, reacting for 3-5 h at room temperature, monitoring the reaction progress by TLC, decompressing and spin-drying after the reaction is finished, adding isopropanol for dilution, filtering with diatomite, spin-evaporating filtrate to remove solvent, dissolving in MeOH, adding CH 3 ONa, reacting for 0.5-1 h at room temperature, monitoring the reaction progress by TLC, regulating pH to weak acid by adopting a proper amount of cation exchange resin after the completion, filtering, concentrating the filtrate, and washing with DCM to obtain an intermediate M;
Step 2: dissolving the intermediate M in CH 3 CN, adding amino ethyl piperazine, dripping glacial acetic acid, reacting at 80-85 ℃, monitoring the reaction progress by TLC, filtering after the reaction, washing a filter cake by DCM, and vacuum drying to obtain the saccharide surfactant.
In the step 1, the solid-to-liquid ratio of acetyl bromolactose to CH 3 CN is 0.04-0.06 g:1mL; the molar ratio of n-butyl lithium to acetyl bromolactose is 0.9-1.1:1; the molar ratio of the 4-mercaptobenzaldehyde to the acetyl bromolactose is 1.3-1.8:1; the solid-to-liquid ratio of MeOH to acetyl bromolactose is 0.05-0.07 g:1mL; the molar ratio of CH 3 ONa to acetyl bromolactose is 2-2.5:1.
The solid-to-liquid ratio of the intermediate M to CH 3 CN is 0.04-0.06 g:1mL; the mol ratio of the amino ethyl piperazine to the intermediate M is 1.4-1.6:1; the ratio of glacial acetic acid to intermediate M used was 1 drop: 0.08-0.12 g.
A zero halogen no-clean soldering flux comprises a compound surfactant; the compound surfactant comprises a saccharide surfactant shown in a formula I.
The zero-halogen no-clean soldering flux comprises a compound organic acid active agent, an acid-base regulator, a film forming agent and a corrosion inhibitor.
The invention also discloses application of the saccharide surfactant in preparing zero-halogen no-clean soldering flux.
The invention also discloses application of the zero-halogen no-clean soldering flux in enhancing a welding effect.
A zero halogen no-clean flux comprising: 1 to 3 percent of compound organic acid active agent, 0.05 to 1 percent of pH regulator, 5 to 20 percent of compound organic cosolvent, 0.1 to 1 percent of compound surfactant, 0.1 to 1 percent of film forming agent, 0.05 to 0.5 percent of corrosion inhibitor and the balance of deionized water.
The compound organic acid active agent comprises at least one of tartaric acid, phthalic acid, anhydrous citric acid, salicylic acid, fumaric acid and glycolic acid; preferably, the compound organic acid active agent comprises tartaric acid, phthalic acid, anhydrous citric acid and glycolic acid, and the mass ratio of the four is 1:0.4-0.6:0.8-1:0.5-0.8.
The pH regulator includes one of triethanolamine or ammonia water.
It should be noted that the compound organic cosolvent includes at least one of ethanol, isopropanol or dimethyl glutarate; preferably, the compound organic cosolvent comprises ethanol and isopropanol, and the volume ratio of the ethanol to the isopropanol is 1:0.5-1.5.
The compound surfactant comprises at least one of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and a saccharide surfactant; preferably, the compound surfactant comprises sodium dodecyl benzene sulfonate and a saccharide surfactant, and the mass ratio of the sodium dodecyl benzene sulfonate to the saccharide surfactant is 1:1-2.
Further, the saccharide surfactant includes 4-mercaptobenzaldehyde and amino ethyl piperazine chemically modified acetyl bromolactose.
The film forming agent comprises one of polyethylene glycol, water-soluble acrylic resin, modified water-soluble acrylic resin, carboxymethyl cellulose and polyvinylpyrrolidone; preferably, the film former comprises a water soluble acrylic resin or a modified water soluble acrylic resin.
Preferably, the modified water-soluble acrylic resin comprises a copolymerization product of methyl methacrylate, acrylic acid, 2-acrylamido-2-methylpropanesulfonic acid, and 2-methacryloyloxyethyl phosphorylcholine.
More preferably, the modified water-soluble acrylic resin includes methyl methacrylate, acrylic acid, 2-acrylamido-2-methylpropanesulfonic acid, 2-methacryloyloxyethyl phosphorylcholine, and 2- (morpholinomethyl) acrylic acid copolymerization products. According to the invention, 2-methacryloyloxyethyl phosphorylcholine and 2- (morpholinomethyl) acrylic acid are adopted as functional polymerization monomers, and are compounded and polymerized with other components to obtain the copolymer, and the copolymer is used as a film forming agent to be applied to a preparation process of soldering flux, so that the obtained zero-halogen no-clean soldering flux has more excellent spreading capability, and the soldering capability is obviously improved, so that a protective film formed after welding has better stability, and the change rate of the insulation resistance value of the protective film is smaller under a damp-heat environment. The reason for this is probably that the invention introduces a new unit structure into the modified water-soluble acrylic resin structure, which has a beneficial effect on the polymer structure and has higher film forming stability; the synergistic effect of the compound and other components obviously reduces the surface tension of the soldering flux, further improves the wettability of the soldering flux, is more conducive to forming a compact organic film after soldering, and reduces the possibility of reoxidation of the solder and the soldered metal.
The moisture and heat resistance can reduce the occurrence of low resistance of the protective film after long-term use.
Specifically, the preparation method of the modified water-soluble acrylic resin comprises the following steps:
And (3) heating the mixed solvent of dimethylbenzene and butyl acetate to 100-120 ℃, sequentially adding methyl methacrylate, acrylic acid, 2-acrylamido-2-methylpropanesulfonic acid, 2-methacryloyloxyethyl phosphorylcholine and 2- (morpholinomethyl) acrylic acid, adding 1/4-1/3 of AIBN, reacting at constant temperature for 1-2 h, adding the rest AIBN, reacting for 3-5 h, cooling and discharging to obtain the modified water-soluble acrylic resin.
The volume ratio of the dimethylbenzene to the butyl acetate is 1:1-3; the solid-liquid ratio of methyl methacrylate and the mixed solvent is 0.3-0.4 g:1mL; the molar ratio of methyl methacrylate, acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, 2-methacryloyloxyethyl phosphorylcholine and 2- (morpholinomethyl) acrylic acid is 1:1:0.3-0.5:0.2-0.4:0.3-0.5; AIBN is added in an amount of 2 to 4wt% based on the total amount of the polymerized monomers.
The corrosion inhibitor is one of cyclohexylamine cinnamate, furfuryl amine, hexamethyleneimine benzoate, urea and 3-aminophenol.
The molecular weight of the modified water-soluble acrylic resin is 10000 to 20000.
The invention also discloses a preparation method of the zero-halogen no-clean soldering flux, which comprises the following steps:
Adding deionized water into a container, sequentially adding an organic cosolvent, an organic acid active agent, a film forming agent, a corrosion inhibitor and a surfactant, and then continuously stirring to prepare the zero-halogen no-clean scaling powder.
Compared with the prior art, the invention has the following beneficial effects:
The invention adopts acetyl bromolactose, 4-mercaptobenzaldehyde and amino ethyl piperazine to prepare the saccharide surfactant, which can effectively reduce the interfacial tension of oil and water and remarkably enhance the emulsifying property; the coating is applied to soldering flux, and the spreading capacity of the coating is obviously improved; meanwhile, the weldability of the soldering flux is obviously improved, the degree of reduction of the insulation resistance value of a protective film formed by soldering in a wet and hot environment is obviously reduced, and the welding effect is enhanced. In addition, the invention adopts 2-methacryloyloxyethyl phosphorylcholine and 2- (morpholinomethyl) acrylic acid as functional polymerization monomers, and the functional polymerization monomers are compounded and polymerized with other components to obtain a film forming agent and are applied to the preparation process of the soldering flux, so that the solid content of the obtained zero-halogen no-clean soldering flux is further improved, the spreading capability is more excellent, the soldering capability is obviously improved, and the change rate of the insulation resistance value of the protective film is smaller under the damp and hot environment. The soldering flux prepared by the invention is colorless transparent liquid, does not contain halogen compounds, has high activity in the welding process, quick tin melting, full welding spots, environmental protection and no harmful smell, and ensures the postwelding reliability effect of electronic products.
Therefore, the zero-halogen no-clean soldering flux provided by the invention has more excellent soldering effect, the spreading capability is obviously improved, the stability of a soldering film in a wet and hot environment is good, no halogen compound exists, the activity of a welding process is high, a welding spot is full, and the reliability effect of an electronic product after welding is ensured.
Drawings
FIG. 1 is the infrared test results of the modified water-soluble acrylic resins of examples 5 and 10 of the present invention;
FIG. 2 is a test result of the spreading ability of the flux in the test example of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the following describes in detail various embodiments of the present application with reference to the embodiments. However, those of ordinary skill in the art will understand that in various embodiments of the present application, numerous technical details have been set forth in order to provide a better understanding of the present application. The claimed application may be practiced without these specific details and with various changes and modifications based on the following embodiments.
Example 1:
a zero halogen no-clean flux comprising: according to mass percentage, 2% of compound organic acid active agent (comprising tartaric acid, phthalic acid, anhydrous citric acid and glycollic acid, the mass ratio of the four is 1:0.5:0.9:0.7), 0.5% of pH regulator triethanolamine, 14% of compound organic cosolvent (comprising ethanol and isopropanol, the volume ratio of the two is 1:1.5), 0.6% of compound surfactant (comprising sodium dodecyl benzene sulfonate and saccharide surfactant, the mass ratio of the two is 1:1.5), 0.5% of film forming agent water-soluble acrylic resin (viscosity 7000 (S), the solid content is 62.8%), 0.3% of corrosion inhibitor cinnamic acid cyclohexylamine, and the balance of deionized water.
Preparation of saccharide surfactant:
Step 1: the solid-liquid ratio is 0.05g:1mL of acetyl bromolactose (CAS No. 5160-10-1) was dissolved in CH 3 CN, then n-butyllithium (molar ratio to acetyl bromolactose is 1:1) and 4-mercaptobenzaldehyde (molar ratio to acetyl bromolactose is 1.5:1) were added, the reaction was carried out at room temperature for 4h, TLC was monitored for the progress of the reaction, dried under reduced pressure after completion of the reaction, isopropanol was added for dilution, then the mixture was filtered with celite, the filtrate was distilled off with solvent, then dissolved in MeOH (solid to acetyl bromolactose ratio: 0.06g:1 mL), CH 3 ONa (molar ratio to acetyl bromolactose: 2.3:1) was added, the reaction was carried out at room temperature for 0.5h, TLC was monitored for the progress of the reaction, an appropriate amount of cation exchange resin (IR-120) was used for adjusting pH to weak acid after completion of the reaction, the filtrate was concentrated and washed with DCM to obtain an intermediate M;1H NMR(400MHz,CDCl3)：δ：9.90(s,1H,-CHO),7.78、7.55(4H,Ar-H),5.41、4.98、3.6～4.1、3.32(10H,-CH),3.5～3.6(4H,-CH2);
Step 2: the solid-liquid ratio is 0.05g:1mL of intermediate M is taken and dissolved in CH 3 CN, aminoethylpiperazine (the mol ratio of the intermediate M to the intermediate M is 1.5:1), glacial acetic acid (the dosage ratio of the intermediate M to the intermediate M is 1 drop: 0.1 g) is added dropwise for reaction at 80 ℃, TLC is used for monitoring the reaction progress, suction filtration is carried out after the reaction is finished, filter cakes are washed by DCM, and the saccharide surfactant (the chemical structure is as follows) is obtained by vacuum drying );1H NMR(400MHz,D2O)：δ：8.74(s,1H,-CH),7.70、7.23(4H,Ar-H),5.38、4.99、3.6～4.1、3.30(10H,-CH),3.5～3.6(4H,-CH2),3.68、2.73、2.64、2.33(12H,-CH2).
The preparation method of the zero-halogen no-clean soldering flux comprises the following steps:
Adding deionized water into a container, sequentially adding an organic cosolvent, an organic acid active agent, a film forming agent, a corrosion inhibitor and a surfactant, and then continuously stirring to prepare the zero-halogen no-clean scaling powder.
Example 2:
A zero halogen no-clean flux comprising: according to mass percentage, 1.8% of compound organic acid active agent (phthalic acid, anhydrous citric acid, salicylic acid and fumaric acid, the mass ratio of the phthalic acid to the anhydrous citric acid, the salicylic acid to the fumaric acid is 1:1.5:1.2:0.8), 0.07% of pH regulator triethanolamine, 7% of compound organic cosolvent (comprising isopropyl alcohol and dimethyl glutarate, the volume ratio of the isopropyl alcohol to the dimethyl glutarate is 1:1), 0.2% of compound surfactant (sodium dodecyl sulfate and saccharide surfactant, the mass ratio of the sodium dodecyl sulfate to the saccharide surfactant is 1:2), 0.2% of film forming agent carboxymethyl cellulose, 0.08% of corrosion inhibitor furfuryl amine and the balance deionized water.
The saccharide surfactant was prepared as in example 1.
The preparation method of the zero-halogen no-clean soldering flux is the same as that of the example 1.
Example 3:
A zero halogen no-clean flux comprising: according to mass percentage, 2.7% of compound organic acid active agent (comprising anhydrous citric acid, salicylic acid, fumaric acid and glycollic acid, the mass ratio of the four is 1:2:0.5:0.7), 0.8% of pH regulator triethanolamine, 18% of compound organic cosolvent (comprising isopropyl alcohol and isopropyl alcohol, the volume ratio of the two is 1:2), 0.8% of compound surfactant (comprising sodium dodecyl benzene sulfonate and sodium dodecyl sulfate, the mass ratio of the two is 1:1), 0.9% of film forming agent polyvinylpyrrolidone, 0.4% of corrosion inhibitor hexamethyleneimine benzoate and the balance of deionized water.
The saccharide surfactant was prepared as in example 1.
The preparation method of the zero-halogen no-clean soldering flux is the same as that of the example 1.
Example 4:
A zero halogen no-clean flux comprising: 1.4% of compound organic acid active agent (including tartaric acid, phthalic acid, anhydrous citric acid and glycolic acid, the mass ratio of the four is 1:0.56:0.82:0.52), 0.76% of pH regulator triethanolamine, 15% of compound organic cosolvent (including ethanol and isopropanol, the volume ratio of the two is 1:2), 0.43% of compound surfactant (including sodium dodecyl benzene sulfonate and saccharide surfactant, the mass ratio of the two is 1:1.8), 0.57% of film forming agent water-soluble acrylic resin, 0.36% of corrosion inhibitor cinnamic acid cyclohexylamine, and the balance of deionized water.
The saccharide surfactant was prepared as in example 1.
The preparation method of the zero-halogen no-clean soldering flux is the same as that of the example 1.
Example 5:
The zero halogen no-clean flux differs from example 1 in that: the film forming agent is the modified water-soluble acrylic resin prepared in the embodiment.
Preparation of modified water-soluble acrylic resin:
Mixing dimethylbenzene and butyl acetate (volume ratio is 1:2), heating to 110 ℃, and sequentially adding methyl methacrylate, acrylic acid, 2-acrylamido-2-methylpropanesulfonic acid, 2-methacryloyloxyethyl phosphorylcholine and 2- (morpholinomethyl) acrylic acid (molar ratio is 1:1:0.4:0.3:0.4), wherein the solid-liquid ratio of the methyl methacrylate to the mixed solvent is 0.35g:1mL; adding 1/3 of AIBN, reacting at constant temperature for 1h, and adding the rest AIBN, wherein the total AIBN addition amount is 3wt% of the total polymerized monomer; and (3) continuously reacting for 4 hours, and cooling and discharging to obtain the modified water-soluble acrylic resin with the molecular weight of 11200.
The saccharide surfactant was prepared as in example 1.
The preparation method of the zero-halogen no-clean soldering flux is the same as that of the example 1.
Example 6:
The zero halogen no-clean flux differs from example 5 in that: the film forming agent is the modified water-soluble acrylic resin prepared in the embodiment.
The modified water-soluble acrylic resin was prepared differently from example 5:
In the preparation process, the 2- (morpholinomethyl) acrylic acid is replaced by the butyl acrylate with the same molar quantity.
The preparation method of the zero-halogen no-clean soldering flux is the same as that of the example 5.
Example 7:
the zero halogen no-clean flux differs from example 5 in that: among the surfactants, the saccharide surfactants were prepared in this example.
The saccharide surfactant was prepared differently from example 5: in the preparation process, the step 2 is adopted to replace aminoethylpiperazine with 2-aminoundecane with equal molar weight.
The zero halogen no-clean flux was prepared as in example 5.
Example 8:
the zero halogen no-clean flux differs from example 5 in that: among the surfactants, the saccharide surfactants are replaced with equimolar amounts of alkyl glycosides.
The zero halogen no-clean flux was prepared as in example 5.
Example 9:
The zero halogen no-clean flux differs from example 7 in that: the film forming agent is the modified water-soluble acrylic resin prepared in the embodiment.
The modified water-soluble acrylic resin was prepared differently from example 7: in the preparation process, the 2- (morpholinomethyl) acrylic acid is replaced by the butyl acrylate with the same molar quantity.
The zero halogen no-clean flux was prepared as in example 7.
Example 10:
The zero halogen no-clean flux differs from example 7 in that: the film forming agent is the modified water-soluble acrylic resin prepared in the embodiment.
The modified water-soluble acrylic resin was prepared differently from example 7: in the preparation process, the equimolar amount of butyl acrylate is used for replacing 2-methacryloyloxyethyl phosphorylcholine and 2- (morpholinomethyl) acrylic acid.
The zero halogen no-clean flux was prepared as in example 7.
Example 11:
the zero halogen no-clean flux differs from example 1 in that: among the surfactants, the saccharide surfactants were prepared in this example.
The saccharide surfactant was prepared differently from example 1: in the preparation process, the step 2 is adopted to replace aminoethylpiperazine with 2-aminoundecane with equal molar weight.
The zero halogen no-clean flux was prepared as in example 1.
Example 12:
The zero halogen no-clean flux differs from example 1 in that: among the surfactants, the saccharide surfactants are replaced with equimolar amounts of alkyl glycosides.
The zero halogen no-clean flux was prepared as in example 1.
Test example 1:
Infrared sign
The testing is carried out by adopting a Fourier infrared spectrometer, and the testing range is 500-4000 cm -1 by adopting a potassium bromide tabletting method.
The above-described test was conducted on the modified water-soluble acrylic resins prepared in example 5 and example 10, and the results are shown in FIG. 1. From the analysis in the figure, compared with the infrared test result of the modified water-soluble acrylic resin prepared in example 10, in the infrared spectrum of the modified water-soluble acrylic resin prepared in example 5, a characteristic absorption peak of the phosphate group appears at 1215cm -1、1058cm-1, and a characteristic absorption peak of the epoxy group appears near 910cm -1, indicating that the modified water-soluble acrylic resin prepared in example 5 was successfully prepared.
Test example 2:
characterization of saccharide surfactant Performance
1. Measurement of oil-water interfacial tension
The test was performed using a BZY-1 type automatic interfacial tensiometer. The specific test method comprises the following steps: an aqueous solution of the test sample was first prepared at a concentration of 0.2wt%, and then the interfacial tension was measured with a platinum ring (radius 9.55 mm). And (3) cleaning the surface of the platinum ring by ultrapure water, burning the platinum ring by an alcohol lamp until the surface turns red, cooling the platinum ring to room temperature, placing the platinum ring in the water solution of the test sample, adding an equal amount of rapeseed oil, slowly lifting the platinum ring upwards, and simultaneously reading the maximum tension required by the platinum ring on the instrument passing through an oil-water interface, namely the oil-water interface tension.
2. Determination of the emulsifying Properties
10ML of a test sample aqueous solution with the concentration of 0.2wt% and 10mL of a control sample Tween 80 aqueous solution with the concentration of 0.2wt% are taken and respectively placed in a centrifuge tube, 10mL of rapeseed oil is added, the mixture and stirring are carried out to enable oil and water to be fully mixed, the mixture is kept stand for 1h, and then the corresponding volumes of an aqueous phase, an emulsion phase and an organic phase are recorded (the larger volume of the emulsion layer represents stronger emulsifying property).
The saccharide surfactants prepared in example 1 and example 7 were subjected to the above test, and the results are shown in table 1:
TABLE 1 surfactant Performance test results
| Sample of | Interfacial tension (mN/m) | Emulsion volume (mL) |
| Example 1 | 2.7 | 18.6 |
| Example 7 | 4.5 | 16.2 |
| Tween 80 | -- | 14.7 |
From the data analysis in table 1, the oil-water interface Zhang Liming of the saccharide surfactant prepared in example 1 is significantly lower than that of example 7, which shows that the saccharide surfactant prepared by adopting 4-mercaptobenzaldehyde and aminoethylpiperazine to chemically modify acetyl bromolactose has better interfacial action performance and can effectively enhance the action effect of the saccharide surfactant on reducing the oil-water interfacial tension. Meanwhile, the emulsion volume treated by the saccharide surfactant prepared in the example 1 is obviously higher than that of the emulsion prepared in the example 7 and tween 80, which shows that the saccharide surfactant prepared by chemically modifying acetyl bromolactose by using 4-mercaptobenzaldehyde and amino ethyl piperazine has better emulsifying property on the surface.
Test example 3:
Flux performance measurement
Spreadability assay
The test was carried out according to the requirements specified in GB113 test method and SJ/T11273, and the spread area of the sample was measured by CAD measurement.
The above test was performed on the zero halogen no-clean flux prepared in examples 1 to 12, and the results are shown in fig. 2. From the analysis of the figure, the spreading area of the zero-halogen no-clean soldering flux prepared in the example 1 is obviously higher than that of the examples 11 and 12, which shows that the application of the soldering flux can be effectively improved and the application performance of the soldering flux can be enhanced by adopting 4-mercaptobenzaldehyde and aminoethylpiperazine to chemically modify acetyl bromolactose to prepare the saccharide surfactant. Example 5 is slightly better than example 1 and example 6, example 6 is slightly better than example 1, example 7 is better than example 11, example 8 is better than example 12, and example 7 is better than example 9 and example 10, example 9 is slightly better than example 10 and example 11, indicating that the use of 2-methacryloyloxyethyl phosphorylcholine or 2- (morpholinomethyl) acrylic acid as a polymeric monomer, in combination with other components to prepare a modified water-soluble acrylic resin, as a film former, can also significantly improve the spreading ability of the flux when applied in a zero halogen no-rinse flux.
Measurement of insulation resistance value
The test was performed with reference to the standard specified in GB/T9494, and the insulation resistance value of the flux test sample was measured. Then, each test sample was placed at 45℃under 93% humidity for 96 hours, then placed in a desiccator having a humidity of 90% adjusted with a saturated solution of sodium tartrate at 20℃for 1 hour, and then taken out to measure the insulation resistance again, and the rate of decrease in the insulation resistance was calculated.
The zero halogen no-clean soldering fluxes prepared in examples 1 to 12 of the present invention were subjected to the above test, and the results are shown in table 2:
TABLE 2 insulation resistance test results
| Sample of | Insulation resistance value (x 10 11 Ω) | Percent decrease (%) |
| Example 1 | 6.3 | 5.2 |
| Example 2 | 6.2 | 5.7 |
| Example 3 | 6.1 | 6.4 |
| Example 4 | 6.4 | 5.0 |
| Example 5 | 7.5 | 2.1 |
| Example 6 | 6.9 | 3.8 |
| Example 7 | 6.6 | 4.8 |
| Example 8 | 6.4 | 5.5 |
| Example 9 | 6.0 | 6.4 |
| Example 10 | 5.5 | 7.5 |
| Example 11 | 5.3 | 7.9 |
| Example 12 | 5.0 | 8.7 |
From the data analysis in table 2, the insulation resistance values of the zero halogen no-clean soldering flux prepared in example 1 are higher than those of the soldering flux prepared in examples 11 and 12, which shows that the soldering performance of the soldering flux can be effectively improved by using the 4-mercaptobenzaldehyde and the aminoethylpiperazine to chemically modify the acetyl bromolactose to prepare the saccharide surfactant. Example 5 is slightly better than example 1 and example 6, example 6 is slightly better than example 1, example 7 is better than example 11, example 8 is better than example 12, and example 7 is better than example 9 and example 10, example 9 is slightly better than example 10 and example 11, indicating that the use of 2-methacryloyloxyethyl phosphorylcholine or 2- (morpholinomethyl) acrylic acid as a polymeric monomer, in combination with other components, to prepare a modified water-soluble acrylic resin, as a film former, can be applied in a zero halogen no-rinse flux, and can also improve the flux ability of the flux to some extent.
Meanwhile, the reduction rate of the insulation resistance value of the zero-halogen no-clean soldering flux prepared in the embodiment 1 is obviously lower than that of the embodiment 11 and the embodiment 12, and the fact that the saccharide surfactant is prepared by adopting 4-mercaptobenzaldehyde and aminoethylpiperazine to chemically modify acetyl bromolactose is shown, so that the soldering flux can be effectively improved in weldability, enhanced in soldering effect and higher in stability when the zero-halogen no-clean soldering flux is applied to the preparation of the soldering flux. Example 5 is slightly better than example 1 and example 6, example 6 is slightly better than example 1, example 7 is better than example 11, example 8 is better than example 12, and example 7 is better than example 9 and example 10, example 9 is slightly better than example 10 and example 11, indicating that 2-methacryloyloxyethyl phosphorylcholine or 2- (morpholinomethyl) acrylic acid is used as a polymerization monomer to prepare a modified water-soluble acrylic resin by compounding and copolymerizing with other components, and is used as a film former in a zero halogen no-rinse flux to further improve the solderability of the flux and enhance the soldering effect.
The conventional technology in the above embodiments is known to those skilled in the art, and thus is not described in detail herein.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. A saccharide surfactant has a chemical structure shown in formula I:
I。
2. the preparation method of the carbohydrate surfactant shown in the formula I comprises the following steps:
step 1: reacting acetyl bromolactose and 4-mercaptobenzaldehyde under the condition of a catalyst, and then removing acetyl for protection under the action of sodium methoxide to obtain an intermediate M; the catalyst in the step 1 comprises n-butyllithium, wherein the molar ratio of the n-butyllithium to the acetyl bromolactose is 0.9-1.1:1, the molar ratio of the 4-mercaptobenzaldehyde to the acetyl bromolactose is 1.3-1.8:1, and the molar ratio of the sodium methoxide to the acetyl bromolactose is 2-2.5:1;
Step 2: mixing intermediate M with aminoethylpiperazine and glacial acetic acid for reaction to obtain a saccharide surfactant, wherein the molar ratio of the aminoethylpiperazine to the intermediate M is 1.4-1.6:1, and the dosage ratio of the glacial acetic acid to the intermediate M is 1 drop: 0.08-0.12 g.
3. A zero halogen no-clean soldering flux comprises a compound surfactant; the built surfactant comprises the saccharide surfactant of claim 1.
4. A zero-halogen no-clean flux according to claim 3, wherein: the zero-halogen no-clean soldering flux comprises a compound organic acid active agent, an acid-base regulator, a film forming agent and a corrosion inhibitor.
5. The zero-halogen no-clean flux of claim 4, wherein: the zero-halogen no-clean soldering flux comprises: 1 to 3 percent of compound organic acid active agent, 0.05 to 1 percent of pH regulator, 5 to 20 percent of compound organic cosolvent, 0.1 to 1 percent of compound surfactant, 0.1 to 1 percent of film forming agent, 0.05 to 0.5 percent of corrosion inhibitor and the balance of deionized water.
6. Use of the saccharide surfactant of claim 1 in the preparation of a zero halogen no-clean flux.
7. Use of the zero-halogen no-clean flux of claim 3 to enhance the soldering effect.
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| CN114589433A (en) * | 2022-03-21 | 2022-06-07 | 广东省科学院化工研究所 | Soldering flux and preparation method and application thereof |
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2023
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| WO2001058639A1 (en) * | 2000-02-08 | 2001-08-16 | Showa Denko K.K. | Solder paste, soldering method using said solder paste and jointed product prepared by said soldering method |
| JP2007216296A (en) * | 2006-01-17 | 2007-08-30 | Mitsubishi Materials Corp | Flux for solder, solder paste using the flux and method for producing substrate mounted with electronic parts |
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| CN102581521A (en) * | 2012-02-03 | 2012-07-18 | 深圳市兴时达科技产品有限公司 | Halogen-free, lead-free and clean-free scaling powder and preparation method thereof |
| CN107175430A (en) * | 2017-07-04 | 2017-09-19 | 合肥安力电力工程有限公司 | A kind of environment protection soldering fluid |
| CN114589433A (en) * | 2022-03-21 | 2022-06-07 | 广东省科学院化工研究所 | Soldering flux and preparation method and application thereof |
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