CN115091078A - High-temperature halogen-free lead-free soldering flux and preparation method thereof - Google Patents
High-temperature halogen-free lead-free soldering flux and preparation method thereof Download PDFInfo
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- CN115091078A CN115091078A CN202210682985.5A CN202210682985A CN115091078A CN 115091078 A CN115091078 A CN 115091078A CN 202210682985 A CN202210682985 A CN 202210682985A CN 115091078 A CN115091078 A CN 115091078A
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- 238000005476 soldering Methods 0.000 title claims abstract description 51
- 230000004907 flux Effects 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000007716 flux method Methods 0.000 title description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 41
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims abstract description 41
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000003960 organic solvent Substances 0.000 claims abstract description 26
- 150000001412 amines Chemical class 0.000 claims abstract description 17
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 17
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 17
- 230000007797 corrosion Effects 0.000 claims abstract description 17
- 238000005260 corrosion Methods 0.000 claims abstract description 17
- 239000004094 surface-active agent Substances 0.000 claims abstract description 17
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 17
- 239000003112 inhibitor Substances 0.000 claims abstract description 16
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012964 benzotriazole Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 241000779819 Syncarpia glomulifera Species 0.000 claims description 40
- 239000001739 pinus spp. Substances 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 40
- 229940036248 turpentine Drugs 0.000 claims description 40
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 30
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 30
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 20
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000007795 chemical reaction product Substances 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 238000002390 rotary evaporation Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical group CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 5
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 5
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical group CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 claims description 5
- 229940043276 diisopropanolamine Drugs 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 5
- 239000012467 final product Substances 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical group CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical group [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000003466 welding Methods 0.000 abstract description 7
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 231100000956 nontoxicity Toxicity 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000009967 tasteless effect Effects 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000779 smoke Substances 0.000 description 7
- 229910000679 solder Inorganic materials 0.000 description 7
- 230000007480 spreading Effects 0.000 description 5
- 238000003892 spreading Methods 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 4
- -1 bromine compound Chemical class 0.000 description 4
- 229910052794 bromium Inorganic materials 0.000 description 4
- 150000001805 chlorine compounds Chemical class 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- JWVAUCBYEDDGAD-UHFFFAOYSA-N bismuth tin Chemical compound [Sn].[Bi] JWVAUCBYEDDGAD-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical class [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- 239000001293 FEMA 3089 Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052789 astatine Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000011179 visual inspection Methods 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
- B23K35/362—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
- B23K35/22—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
-
- 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 relates to the technical field of soldering flux, and discloses a high-temperature halogen-free lead-free soldering flux and a preparation method thereof, wherein the high-temperature halogen-free lead-free soldering flux is prepared from the following components: organic solvent, modified rosin, benzotriazole, organic amine, thixotropic agent, antioxidant, surfactant and corrosion inhibitor; the high-temperature halogen-free lead-free soldering flux prepared by the invention has the characteristics of no toxicity and no pungent smell, is nontoxic and tasteless at normal temperature, does not generate substances with toxic or pungent smell during welding, and is green and safe.
Description
Technical Field
The invention relates to the technical field of soldering flux, in particular to high-temperature halogen-free lead-free soldering flux and a preparation method thereof.
Background
The halogen compound is usually selected from chlorine compounds or bromine compounds, and after the soldering paste containing the chlorine compound or the bromine compound completes the soldering function, the chlorine compound or the bromine compound still exists in the applied electronic products in the form of residues. As the electronic product is used for a long time, the chlorine compound and the bromine compound can cause certain corrosion to the electronic product, thereby affecting the reliability of the product.
For example, the chinese patent publication No. CN 104858571B discloses a halogen-free soldering flux for tin-bismuth system lead-free solder paste and a preparation method thereof, and the invention provides a halogen-free soldering flux for tin-bismuth system lead-free solder paste and a preparation method thereof. The soldering flux is composed of 20-47% of rosin, 8-20% of tackifier, 0.5-12% of antioxidant, 4-15% of organic acid, 0.2-3% of benzotriazole, 6-14% of organic amine, 0.5-8% of surfactant, 4-10% of thixotropic agent and the balance solvent. The soldering flux disclosed by the invention has the advantages that through the optimized selection of the active system of the soldering flux, the tin paste prepared from the soldering flux and the tin-bismuth lead-free tin powder does not contain any fluorine, chlorine, bromine, iodine and astatine halogen elements, the soldering flux has good solderability in soldering, a soldered joint is full and bright after soldering, no black oxide is generated, the surface insulation resistance is high, and the soldering flux is particularly suitable for assembling and soldering electronic components with low soldering temperature requirements, however, the expansion performance is poor, and the development of the soldering flux is limited.
Based on the above, we propose a high-temperature halogen-free lead-free soldering flux, and hopefully solve the disadvantages in the prior art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-temperature halogen-free lead-free soldering flux and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
the high-temperature halogen-free lead-free soldering flux is prepared from the following components in parts by weight: 30-50 parts of organic solvent, 20-25 parts of modified rosin, 1-3 parts of benzotriazole, 1.5-2 parts of organic amine, 1.2-1.8 parts of thixotropic agent, 2-3 parts of antioxidant, 1.8-2.6 parts of surfactant and 1-2 parts of corrosion inhibitor.
As a further technical scheme, the preparation method of the modified rosin comprises the following steps:
(1) adding methyl ethylene oxide into a reaction kettle, introducing dried trimethylamine, stirring for reaction for 1-2h after the introduction is finished within 2-3h, controlling the temperature in the reaction kettle to be 20-25 ℃ all the time, performing suction filtration separation after the reaction is finished to obtain a reaction product, washing the reaction product by using acetone, and performing vacuum drying to obtain a white reaction material;
the temperature of the trimethylamine drying treatment is 50-60 ℃, and the drying time is 2-3 h;
(2) sequentially adding rosin, white reaction materials and modified turpentine into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding absolute ethyl alcohol, uniformly stirring, heating to the ethanol reflux temperature, reacting for 2-3h, performing rotary evaporation on the mixed liquid in the reaction kettle, and recovering ethanol to obtain the modified rosin.
As a further technical scheme, the molar ratio of the methyl oxirane to the trimethylamine is 10: 3-4.
As a further technical scheme: the mixing mass ratio of the rosin, the white reaction material, the modified turpentine and the absolute ethyl alcohol is 30-35: 3-5: 5-7:45-50.
As a further technical scheme, the preparation method of the modified turpentine comprises the following steps:
drying turpentine to obtain dried turpentine;
adding dried turpentine and propylene oxide into a reaction kettle in sequence, adding glycerol, stirring for 30-40min, adding a catalyst, adjusting the temperature to 80-88 ℃, keeping the temperature and stirring for 2-3h, cooling to room temperature after the reaction is finished, extracting reactants by using n-hexane for 3 times, combining extract liquor, washing by water for 3 times, drying, and recovering the n-hexane through rotary evaporation to obtain the modified turpentine.
According to a further technical scheme, the mixing mass ratio of the turpentine, the propylene oxide, the glycerol and the catalyst is 20-24:3-7:25-30: 0.8-1.2.
As a further technical scheme: the catalyst is potassium hydroxide.
As a further technical scheme: the organic amine is diisopropanolamine;
the thixotropic agent is N, N-ethylene bis stearamide;
the surfactant is sodium dodecyl benzene sulfonate;
the antioxidant is 2, 6-di-tert-butyl-4-methylphenol;
the corrosion inhibitor is sodium molybdate;
the organic solvent is ethylene glycol.
A preparation method of high-temperature halogen-free lead-free soldering flux comprises the following steps:
(1) weighing the components in parts by weight respectively for later use;
(2) respectively and equally dividing the organic solvent into two parts ab;
(3) sequentially adding benzotriazole and organic amine into a part of organic solvent, adjusting the temperature to 50-60 ℃, keeping the temperature, stirring for 40-50min, and standing;
(4) adding the modified rosin in the step (3), adjusting the temperature to 140 ℃, keeping the temperature and stirring for 35-40min, and naturally cooling to room temperature to obtain an intermediate;
(5) sequentially adding the thixotropic agent, the antioxidant, the surfactant and the corrosion inhibitor into the b parts of the organic solvent, heating to 105-110 ℃, and stirring for 30-35min under heat preservation to obtain a mixed solution;
(6) adding the obtained mixed solution into the intermediate, adjusting the temperature to 80-90 deg.C, stirring for 1-2h under heat preservation, naturally cooling to room temperature, and standing for 40-50min to obtain the final product.
The halogen-free lead-free soldering flux prepared by the invention can assist solder to spread on a substrate, can promote the smooth operation of a welding process, can directly obstruct the spreading of molten solder on the substrate due to the existence of oxide or impurities on the surface of the welded substrate when electronic packaging is carried out by soldering, can remove the oxide and the impurities to promote the spreading of the molten solder after the halogen-free lead-free soldering flux is adopted, and can form a protective film on the molten solder and the substrate during welding to prevent the molten solder and the substrate from being oxidized again.
The invention can improve the heat transfer efficiency of the soldering flux by introducing the modified rosin, and can better transfer the heat to the area to be welded, thereby greatly improving the welding efficiency, and also has good thermal stability.
The modified turpentine oil is introduced into the preparation of the modified rosin, so that the activity of the modified rosin in a liquid state can be further improved, the modified rosin can react with a metal oxide more quickly to form reaction salt, the effect of removing a metal oxide film is achieved, the modified rosin in a molten state has better fluidity and thermal conductivity, the occurrence of poor welding can be reduced, the secondary oxidation phenomenon of metal can be prevented during welding, and meanwhile, a hydrophobic film formed during welding can play an excellent waterproof and moistureproof role.
Compared with the prior art, the invention provides the high-temperature halogen-free lead-free soldering flux and the preparation method thereof, and the high-temperature halogen-free lead-free soldering flux has the following beneficial effects:
the high-temperature halogen-free lead-free soldering flux prepared by the invention has the characteristics of no toxicity and no pungent smell, is nontoxic and tasteless at normal temperature, does not generate toxic or pungent substances during soldering, is green and safe, is easy to remove residues after soldering, does not generate adverse effects on soldering points, can be stored for a long time at normal temperature, and prolongs the storage life.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following are specific examples:
example 1
The high-temperature halogen-free lead-free soldering flux is prepared from the following components in parts by weight: 30 parts of organic solvent, 20 parts of modified rosin, 1 part of benzotriazole, 1.5 parts of organic amine, 1.2 parts of thixotropic agent, 2 parts of antioxidant, 1.8 parts of surfactant and 1 part of corrosion inhibitor.
As a further technical scheme, the preparation method of the modified rosin comprises the following steps:
(1) adding methyl ethylene oxide into a reaction kettle, introducing dried trimethylamine, stirring for reaction for 1h after the introduction is finished within 2h, controlling the temperature in the reaction kettle to be 20 ℃ all the time, performing suction filtration separation after the reaction is finished to obtain a reaction product, washing the reaction product by using acetone, and performing vacuum drying to obtain a white reaction material;
the temperature of the trimethylamine drying treatment is 50 ℃, and the drying time is 2 h;
(2) sequentially adding rosin, white reaction materials and modified turpentine into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding absolute ethyl alcohol, uniformly stirring, heating to the ethanol reflux temperature, reacting for 2 hours, performing rotary evaporation on the mixed liquid in the reaction kettle, and recovering ethanol to obtain the modified rosin.
According to a further technical scheme, the molar ratio of the methyl oxirane to the trimethylamine is 10:3.
As a further technical scheme: the mixing mass ratio of the rosin, the white reaction material, the modified turpentine and the absolute ethyl alcohol is 30: 3: 5:45.
As a further technical scheme, the preparation method of the modified turpentine comprises the following steps:
drying turpentine to obtain dried turpentine;
adding dried turpentine and propylene oxide into a reaction kettle in sequence, then adding glycerol, stirring for 30min, then adding a catalyst, adjusting the temperature to 80 ℃, keeping the temperature, stirring for 2h, cooling to room temperature after the reaction is finished, extracting reactants by using normal hexane for 3 times, combining extract liquor, washing by water for 3 times, drying, and recovering the normal hexane by rotary evaporation to obtain the modified turpentine.
According to a further technical scheme, the mixing mass ratio of the turpentine, the propylene oxide, the glycerol and the catalyst is 20:3:25: 0.8.
As a further technical scheme: the catalyst is potassium hydroxide.
As a further technical scheme: the organic amine is diisopropanolamine;
the thixotropic agent is N, N-ethylene bis stearamide;
the surfactant is sodium dodecyl benzene sulfonate;
the antioxidant is 2, 6-di-tert-butyl-4-methylphenol;
the corrosion inhibitor is sodium molybdate;
the organic solvent is ethylene glycol.
A preparation method of high-temperature halogen-free lead-free soldering flux comprises the following steps:
(1) weighing the components in parts by weight respectively for later use;
(2) respectively and equally dividing the organic solvent into two parts ab;
(3) sequentially adding benzotriazole and organic amine into a part of organic solvent, adjusting the temperature to 50 ℃, keeping the temperature, stirring for 40min, and standing;
(4) adding modified rosin into the step (3), adjusting the temperature to 120 ℃, keeping the temperature and stirring for 35min, and naturally cooling to room temperature to obtain an intermediate;
(5) sequentially adding the thixotropic agent, the antioxidant, the surfactant and the corrosion inhibitor into the b parts of the organic solvent, heating to 105 ℃, and stirring for 30min under the condition of heat preservation to obtain a mixed solution;
(6) adding the obtained mixed solution into the intermediate, adjusting the temperature to 80 ℃, keeping the temperature and stirring for 1h, then naturally cooling to room temperature, and standing for 40min to obtain the final product.
Example 2
The high-temperature halogen-free lead-free soldering flux is prepared from the following components in parts by weight: 40 parts of organic solvent, 22 parts of modified rosin, 2 parts of benzotriazole, 1.8 parts of organic amine, 1.5 parts of thixotropic agent, 2.5 parts of antioxidant, 2.3 parts of surfactant and 1.2 parts of corrosion inhibitor.
As a further technical scheme, the preparation method of the modified rosin comprises the following steps:
(1) adding methyl ethylene oxide into a reaction kettle, introducing dried trimethylamine, stirring for reaction for 1.2 hours after the introduction is finished within 2.3 hours, controlling the temperature in the reaction kettle to be 22 ℃ all the time, performing suction filtration and separation after the reaction is finished to obtain a reaction product, washing the reaction product by using acetone, and performing vacuum drying to obtain a white reaction material;
the temperature of the trimethylamine drying treatment is 55 ℃, and the drying time is 2.5 h;
(2) sequentially adding rosin, a white reaction material and modified turpentine into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding absolute ethyl alcohol, uniformly stirring, heating to the ethanol reflux temperature, reacting for 2.5 hours, performing rotary evaporation on the mixed liquid in the reaction kettle, and recovering ethanol to obtain the modified rosin.
According to a further technical scheme, the molar ratio of the methyl oxirane to the trimethylamine is 10: 3.5.
As a further technical scheme: the mixing mass ratio of the rosin, the white reaction material, the modified turpentine and the absolute ethyl alcohol is 32: 4: 6:49.
As a further technical scheme, the preparation method of the modified turpentine comprises the following steps:
drying turpentine to obtain dried turpentine;
adding dried turpentine and propylene oxide into a reaction kettle in sequence, then adding glycerol, stirring for 35min, then adding a catalyst, adjusting the temperature to 82 ℃, keeping the temperature, stirring for 2.5h, cooling to room temperature after the reaction is finished, extracting reactants for 3 times by using n-hexane, combining extract liquor, then washing for 3 times, drying, and recovering the n-hexane through rotary evaporation to obtain the modified turpentine.
According to a further technical scheme, the mixing mass ratio of the turpentine, the propylene oxide, the glycerol and the catalyst is 22:5:28: 0.9.
As a further technical scheme: the catalyst is potassium hydroxide.
As a further technical scheme: the organic amine is diisopropanolamine;
the thixotropic agent is N, N-ethylene bis stearamide;
the surfactant is sodium dodecyl benzene sulfonate;
the antioxidant is 2, 6-di-tert-butyl-4-methylphenol;
the corrosion inhibitor is sodium molybdate;
the organic solvent is ethylene glycol.
A preparation method of high-temperature halogen-free lead-free soldering flux comprises the following steps:
(1) weighing the components in parts by weight respectively for later use;
(2) respectively and equally dividing the organic solvent into two parts ab;
(3) sequentially adding benzotriazole and organic amine into a part of organic solvent, adjusting the temperature to 55 ℃, keeping the temperature, stirring for 45min, and standing;
(4) adding modified rosin into the step (3), adjusting the temperature to 130 ℃, keeping the temperature and stirring for 38min, and naturally cooling to room temperature to obtain an intermediate;
(5) sequentially adding the thixotropic agent, the antioxidant, the surfactant and the corrosion inhibitor into the b parts of the organic solvent, heating to 107 ℃, and stirring for 32min at the constant temperature to obtain a mixed solution;
(6) adding the obtained mixed solution into the intermediate, adjusting the temperature to 85 ℃, keeping the temperature and stirring for 1.5h, then naturally cooling to room temperature, and standing for 42min to obtain the final product.
Example 3
The high-temperature halogen-free lead-free soldering flux is prepared from the following components in parts by weight: 50 parts of organic solvent, 25 parts of modified rosin, 3 parts of benzotriazole, 2 parts of organic amine, 1.8 parts of thixotropic agent, 3 parts of antioxidant, 2.6 parts of surfactant and 2 parts of corrosion inhibitor.
As a further technical scheme, the preparation method of the modified rosin comprises the following steps:
(1) adding methyl ethylene oxide into a reaction kettle, then introducing dried trimethylamine, stirring for reaction for 2 hours after the introduction is finished within 3 hours, controlling the temperature in the reaction kettle to be 25 ℃ all the time, performing suction filtration separation after the reaction is finished to obtain a reaction product, washing the reaction product by using acetone, and performing vacuum drying to obtain a white reaction material;
the temperature of the trimethylamine drying treatment is 60 ℃, and the drying time is 3 h;
(2) sequentially adding rosin, white reaction materials and modified turpentine into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding absolute ethyl alcohol, uniformly stirring, heating to the ethanol reflux temperature, reacting for 3 hours, performing rotary evaporation on the mixed liquid in the reaction kettle, and recovering ethanol to obtain the modified rosin.
According to a further technical scheme, the molar ratio of the methyl oxirane to the trimethylamine is 10: 4.
As a further technical scheme: the mixing mass ratio of the rosin, the white reaction material, the modified turpentine oil and the absolute ethyl alcohol is 35: 5: 7:50.
As a further technical scheme, the preparation method of the modified turpentine comprises the following steps:
drying turpentine to obtain dried turpentine;
adding dried turpentine and propylene oxide into a reaction kettle in sequence, adding glycerol, stirring for 40min, adding a catalyst, adjusting the temperature to 88 ℃, keeping the temperature and stirring for 3h, cooling to room temperature after the reaction is finished, extracting reactants for 3 times by using n-hexane, combining extract liquor, washing for 3 times, drying, and recovering the n-hexane through rotary evaporation to obtain the modified turpentine.
According to a further technical scheme, the mixing mass ratio of the turpentine, the propylene oxide, the glycerol and the catalyst is 24:7:30: 1.2.
As a further technical scheme: the catalyst is potassium hydroxide.
As a further technical scheme: the organic amine is diisopropanolamine;
the thixotropic agent is N, N-ethylene bis stearamide;
the surfactant is sodium dodecyl benzene sulfonate;
the antioxidant is 2, 6-di-tert-butyl-4-methylphenol;
the corrosion inhibitor is sodium molybdate;
the organic solvent is ethylene glycol.
A preparation method of high-temperature halogen-free lead-free soldering flux comprises the following steps:
(1) weighing the components in parts by weight respectively for later use;
(2) respectively and equally dividing the organic solvent into two parts ab;
(3) sequentially adding benzotriazole and organic amine into a part of organic solvent, adjusting the temperature to 60 ℃, keeping the temperature, stirring for 50min, and standing;
(4) adding modified rosin into the step (3), adjusting the temperature to 140 ℃, keeping the temperature and stirring for 40min, and naturally cooling to room temperature to obtain an intermediate;
(5) sequentially adding the thixotropic agent, the antioxidant, the surfactant and the corrosion inhibitor into the b parts of the organic solvent, heating to 110 ℃, and stirring for 35min under the condition of heat preservation to obtain a mixed solution;
(6) adding the obtained mixed solution into the intermediate, adjusting the temperature to 90 ℃, keeping the temperature and stirring for 2h, then naturally cooling to room temperature, and standing for 50min to obtain the final product.
Comparative example 1: the difference from example 1 is that the modified rosin was replaced by an unmodified rosin;
comparative example 2: the difference from the example 1 is that the modified rosin adopts unmodified turpentine;
and (3) testing:
the size and the irritation of the smoke are judged by means of visual inspection and laboratory smell of the medicine:
TABLE 1
| Smog (big, small) | |
| Example 1 | Less smoke |
| Example 2 | Less smoke |
| Example 3 | Less smoke |
| Comparative example 1 | Big smoke and high smoke |
| Comparative example 2 | Slightly larger smoke |
As can be seen from table 1, the flux prepared according to the present invention has significantly reduced fume generation after use.
TABLE 2
As can be seen from Table 2, the soldering flux prepared by the method of the present invention has no irritating odor.
Storage property comparison of examples and comparative samples:
the mixture is stored in a sealed way at the temperature of 0-10 ℃ for 6 months, and compared, the tackifying rate of each group is changed:
thickening ratio (test viscosity-initial viscosity)/initial viscosity × 100%:
TABLE 3
| Fraction of increase in viscosity% | |
| Example 1 | 2.35 |
| Example 2 | 2.28 |
| Example 3 | 2.33 |
| Comparative example 1 | 10.87 |
| Comparative example 2 | 8.21 |
As can be seen from Table 3, the soldering flux prepared by the method of the present invention has a small viscosity change after a long time storage, and thus has a long storage time, which indicates that the storage property of the soldering flux can be greatly improved by the modification treatment of the rosin.
The spreading performance of the samples of the examples and the comparative examples is tested according to SJ/T11273-2002;
TABLE 4
| Spreading area/mm 2 | |
| Example 1 | 62.34 |
| Example 2 | 63.58 |
| Example 3 | 62.76 |
| Comparative example 1 | 46.27 |
| Comparative example 2 | 55.14 |
As can be seen from Table 4, the flux prepared by the method of the present invention has excellent spreading properties.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The high-temperature halogen-free lead-free soldering flux is characterized by being prepared from the following components in parts by weight: 30-50 parts of organic solvent, 20-25 parts of modified rosin, 1-3 parts of benzotriazole, 1.5-2 parts of organic amine, 1.2-1.8 parts of thixotropic agent, 2-3 parts of antioxidant, 1.8-2.6 parts of surfactant and 1-2 parts of corrosion inhibitor.
2. The high-temperature halogen-free lead-free soldering flux as claimed in claim 1, wherein the preparation method of the modified rosin comprises the following steps:
(1) adding methyl ethylene oxide into a reaction kettle, introducing dried trimethylamine, stirring for reaction for 1-2h after the introduction is finished within 2-3h, controlling the temperature in the reaction kettle to be 20-25 ℃ all the time, performing suction filtration separation after the reaction is finished to obtain a reaction product, washing the reaction product by using acetone, and performing vacuum drying to obtain a white reaction material;
the temperature of the trimethylamine drying treatment is 50-60 ℃, and the drying time is 2-3 h;
(2) sequentially adding rosin, a white reaction material and modified turpentine into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding absolute ethyl alcohol, uniformly stirring, heating to the ethanol reflux temperature, reacting for 2-3 hours, performing rotary evaporation on the mixed liquid in the reaction kettle, and recovering ethanol to obtain modified rosin.
3. The high temperature, halogen-free, lead-free fluxing agent of claim 1, wherein the molar ratio of methyl ethylene oxide to trimethylamine is 10: 3-4.
4. The high temperature, halogen-free, lead-free flux of claim 1, wherein: the mixing mass ratio of the rosin, the white reaction material, the modified turpentine and the absolute ethyl alcohol is 30-35: 3-5: 5-7:45-50.
5. The high temperature, halogen-free, lead-free soldering flux of claim 4, wherein the modified turpentine is prepared by the steps of:
drying turpentine to obtain dried turpentine;
adding dried turpentine and propylene oxide into a reaction kettle in sequence, adding glycerol, stirring for 30-40min, adding a catalyst, adjusting the temperature to 80-88 ℃, keeping the temperature and stirring for 2-3h, cooling to room temperature after the reaction is finished, extracting reactants by using n-hexane for 3 times, combining extract liquor, washing by water for 3 times, drying, and recovering the n-hexane through rotary evaporation to obtain the modified turpentine.
6. The high-temperature halogen-free lead-free soldering flux as claimed in claim 5, wherein the mixing mass ratio of the turpentine, the propylene oxide, the glycerol and the catalyst is 20-24:3-7:25-30: 0.8-1.2.
7. The high temperature, halogen-free, lead-free flux of claim 6, wherein: the catalyst is potassium hydroxide.
8. The high temperature, halogen-free, lead-free flux of claim 1, wherein: the organic amine is diisopropanolamine;
the thixotropic agent is N, N-ethylene bis stearamide;
the surfactant is sodium dodecyl benzene sulfonate;
the antioxidant is 2, 6-di-tert-butyl-4-methylphenol;
the corrosion inhibitor is sodium molybdate;
the organic solvent is ethylene glycol.
9. The method for preparing a high temperature, halogen-free, lead-free soldering flux according to any one of claims 1 to 8, comprising the steps of:
(1) weighing the components in parts by weight respectively for later use;
(2) respectively and equally dividing the organic solvent into two parts ab;
(3) sequentially adding benzotriazole and organic amine into a part of organic solvent, adjusting the temperature to 50-60 ℃, keeping the temperature, stirring for 40-50min, and standing;
(4) adding the modified rosin in the step (3), adjusting the temperature to be 140 ℃, keeping the temperature and stirring for 35-40min, and naturally cooling to room temperature to obtain an intermediate;
(5) sequentially adding a thixotropic agent, an antioxidant, a surfactant and a corrosion inhibitor into the b parts of organic solvent, heating to 105-110 ℃, and stirring for 30-35min under heat preservation to obtain a mixed solution;
(6) adding the obtained mixed solution into the intermediate, adjusting the temperature to 80-90 deg.C, stirring for 1-2h under heat preservation, naturally cooling to room temperature, and standing for 40-50min to obtain the final product.
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|---|---|---|---|---|
| JPS63278695A (en) * | 1986-11-04 | 1988-11-16 | Harima Chem Inc | Creamy solder |
| JPH1110388A (en) * | 1997-06-18 | 1999-01-19 | Asahi Chem Res Lab Ltd | Water base flux composition |
| CN1543385A (en) * | 2001-06-29 | 2004-11-03 | 富士电机株式会社 | Solder composition |
| CN104175024A (en) * | 2014-04-30 | 2014-12-03 | 江苏博迁新材料有限公司 | High-performance lead-free halogen-free soldering flux for soldering paste and preparing method of soldering flux |
| JP2016002553A (en) * | 2014-06-13 | 2016-01-12 | 荒川化学工業株式会社 | Lead-free solder paste |
-
2022
- 2022-06-16 CN CN202210682985.5A patent/CN115091078A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63278695A (en) * | 1986-11-04 | 1988-11-16 | Harima Chem Inc | Creamy solder |
| JPH1110388A (en) * | 1997-06-18 | 1999-01-19 | Asahi Chem Res Lab Ltd | Water base flux composition |
| CN1543385A (en) * | 2001-06-29 | 2004-11-03 | 富士电机株式会社 | Solder composition |
| CN104175024A (en) * | 2014-04-30 | 2014-12-03 | 江苏博迁新材料有限公司 | High-performance lead-free halogen-free soldering flux for soldering paste and preparing method of soldering flux |
| JP2016002553A (en) * | 2014-06-13 | 2016-01-12 | 荒川化学工業株式会社 | Lead-free solder paste |
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