CN109048121B - Soldering flux for photovoltaic module - Google Patents
Soldering flux for photovoltaic module Download PDFInfo
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- CN109048121B CN109048121B CN201811046784.6A CN201811046784A CN109048121B CN 109048121 B CN109048121 B CN 109048121B CN 201811046784 A CN201811046784 A CN 201811046784A CN 109048121 B CN109048121 B CN 109048121B
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- 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
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- 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
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- 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
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Abstract
The invention discloses a soldering flux for a photovoltaic module, and belongs to the field of solar photovoltaics. According to the invention, rosin is subjected to composite modification, a phenolic resin is used for filling a dimer of the rosin, an ammonium chloride component in a composite auxiliary agent can be subjected to thermal decomposition to generate HCl for providing acidity, the phenomena of decomposition, carbonization and smoking of the rosin due to high temperature are reduced, and full, bright surface and high-expansion-rate welding spots can be formed on a plate surface; the dopamine and aniline components in the auxiliary agent can provide an oxidation self-assembly function, so that an excellent film forming effect can be achieved, the amphiphilic silane coupling agent and lecithin can interact with each other to form an organic silicon-phospholipid double-layer lubricating structure, the contact angle between the organic silicon-phospholipid double-layer lubricating structure and a welding surface is increased, and a welding assisting effect is provided. The invention solves the problem that the treatment effect of the prior common welding flux on the welding surface is poor.
Description
Technical Field
The invention belongs to the field of solar photovoltaics, and particularly relates to a soldering flux for a photovoltaic module.
Background
With the development of economy and social progress, people put forward higher and higher requirements on energy sources, the energy consumption at present mainly comprises fossil fuels such as coal, petroleum and natural gas, and among numerous energy sources, solar photovoltaic power generation is the mode with the most technical content and development prospect in new energy sources and renewable energy sources. Solar energy is a huge energy source without pollution to the environment, and the solar energy obtained by the earth per second is equivalent to the energy generated by burning 500 ten thousand tons of high-quality coal. The solar photovoltaic cell module is a device which combines glass, crystalline silicon cell pieces, wires, wiring devices, bonding materials and the like into an integral structure and converts light energy into electric energy under the irradiation of sunlight. Therefore, the application of the photovoltaic building integration technology which organically integrates the photovoltaic power generation system and the building is more and more extensive. The solar energy dual-purpose solar energy generating set can meet the lighting requirement of buildings, can also fully utilize the existing windows, glass curtain walls or lighting roofs to generate electricity, has dual-purpose effect, and cannot damage the style, the attractiveness and the function of the original buildings. The photovoltaic module (also called solar panel) is a core part in a solar power generation system, and the quality of the photovoltaic module directly determines the solar power generation efficiency, so that the production of the photovoltaic module becomes particularly important.
With the gradual turning of the solar photovoltaic industry to the development of integration and multi-functionalization, the requirement on the performance of the flux is higher and higher. Welding, as a way of connecting parts, which is widely used in daily production, plays an important role in production, and welding often uses solder to connect two parts, so that the performance of the solder greatly determines the quality of the welding performance.
The flux is a mixture of rosin as a main component, and is an auxiliary material for ensuring the smooth operation of a welding process. The soldering is a main process in electronic assembly, the soldering flux is an auxiliary material used in the soldering, and the soldering flux has the main function of removing oxides on the surfaces of solder and a soldered parent metal, so that the metal surface reaches necessary cleanliness, and the firm connection of soldering points can be ensured.
The existing soldering flux comprises: the welding surface is remained too much, which can bond dust and sundries and affect the reliability of the product.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problem that the treatment effect of the conventional flux on the welding surface is poor, the flux for the photovoltaic module is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
the flux for the photovoltaic module comprises the following components: 4-8 parts of polyethylene glycol, 3-7 parts of linolenic acid, 2-5 parts of antioxidant, 3-7 parts of film forming agent, 1-4 parts of preservative, 10-15 parts of surfactant, 6-10 parts of pretreated rice washing water and 1-4 parts of auxiliary agent, and further comprises: 30-50 parts of composite modified rosin and 12-25 parts of composite auxiliary agent.
The preparation method of the composite modified rosin comprises the following steps:
(1) at the temperature of 25-35 ℃, according to the mass ratio of 1: 3-5, mixing and stirring rosin and toluene, heating to 50-60 ℃, adding concentrated sulfuric acid with the mass being 5-8% of that of the rosin, keeping the temperature, adding zinc chloride with the mass being 1-4% of that of the rosin, mixing, keeping the temperature at 100-110 ℃, carrying out reflux reaction to obtain a reactant, washing the reactant, carrying out reduced pressure distillation to obtain polymerized rosin, heating the polymerized rosin to 190-200 ℃, heating phenolic resin with the mass being 3-5 times of that of the polymerized rosin, mixing and stirring, heating to 230-240 ℃, adding pentaerythritol with the mass being 7-15% of that of the polymerized rosin and zinc oxide with the mass being 6-10% of that of the polymerized rosin, keeping the temperature, heating to 260-280 ℃, keeping the temperature, discharging, and cooling to obtain modified rosin;
(2) according to the mass ratio of 5: 4-7: 1-2, mixing maleopimaric acid, a reagent and polyethylene glycol, introducing nitrogen for protection, reacting for 1-3 hours at 200-220 ℃, cooling to 150-160 ℃, discharging to obtain an esterification mixture, and taking the esterification mixture according to a mass ratio of 1: 3-6: 0.01 adding the modified rosin and polyvinylpyrrolidone, mixing and stirring to obtain the composite modified rosin.
The reagent in the step (2): according to the mass ratio of 10-15: 0.1 mixing citric acid solution and concentrated sulfuric acid to obtain the reagent.
The preparation of the compound auxiliary agent comprises the following steps: taking 4-8 parts of microcrystalline paraffin, 3-5 parts of sodium dodecyl benzene sulfonate, 1-4 parts of lecithin, 2-5 parts of cyclohexanol, 4-8 parts of silane coupling agent KH-550 and 20-40 parts of water, mixing and stirring the silane coupling agent KH-550, the sodium dodecyl benzene sulfonate, the lecithin, the cyclohexanol and the water at 30-45 ℃, adding the microcrystalline paraffin, emulsifying at 25-30 ℃ to obtain an emulsion, standing and aging at room temperature to obtain an aging solution, taking the aging solution for rotary evaporation and reduced pressure concentration to obtain a concentrated solution, and taking the concentrated solution according to the mass ratio of 8-12: 1, adding ammonium chloride, mixing and performing ultrasonic action to obtain the composite auxiliary agent.
The preservative is as follows: according to the mass ratio of 1: 4-8: 0.1 mixing sodium benzoate, potassium sorbate, and poly Ɛ -lysine to obtain antiseptic.
The film forming agent is as follows: according to the mass ratio of 10: 2: and 0.1-0.3 mixing the nitrocellulose, the acrylic resin and the OP-10 to obtain the film forming agent.
The antioxidant is as follows: according to the mass ratio of 6-11: 0.1 taking tert-butyl hydroquinone and nano SiO2Mixing to obtain antioxidant.
The surfactant: according to the mass ratio of 1: and 3-6, mixing sodium laureth sulfate and cetyl dimethyl amine oxide to obtain the surfactant.
The auxiliary agent is as follows: according to the mass ratio of 5-8: 1, mixing dopamine hydrochloride and aniline to obtain the auxiliary agent.
The rice washing water pretreatment: according to the mass ratio of 1: and 40-60 taking rice and water, mixing and stirring, filtering, adding NaCl accounting for 3-7% of the mass of the filtrate into the filtrate, mixing, drying in the sun, discharging to obtain a material liquid, adding an acetic acid solution accounting for 10% of the mass of the material liquid into the material liquid, and mixing to obtain the pretreated rice washing water.
Compared with other methods, the method has the beneficial technical effects that:
(1) according to the invention, rosin is subjected to composite modification, a dimer of the rosin is filled with phenolic resin and then mixed with an esterified mixture of maleopimaric acid, the thermal effect during welding use can enable the dimer of the rosin to show acidity and film-forming property, oxidation of a welded surface is effectively eliminated, meanwhile, welding spots are protected from being oxidized, meanwhile, an ammonium chloride component in a composite auxiliary agent can be subjected to thermal decomposition to generate HCl to provide acidity, so that partial oxides are dissolved in acid, and the effect of cleaning the welded surface is achieved, the problem of low fluxing activity caused by the fact that carboxylic acid roasted by the rosin is located on tertiary carbon of a phenanthrene ring structure and the steric hindrance is large is solved through modification, the phenomenon of smoke generation due to decomposition and carbonization of the rosin caused by high temperature is reduced, and full, bright surface and high-expansion rate welding spots can be formed on a plate surface;
(2) the dopamine and aniline components in the auxiliary agent can provide oxidation self-assembly function, and are matched with a nitrocellulose film forming agent, can achieve excellent film forming effect, avoid oxidation, improve the wettability of the soldering flux and the metal surface by using the synergistic effect of the surfactant and other components, the corrosion of the metal surface is reduced, the wettability is obviously improved, the surface tension of the welded material is reduced, the oxidation of the surface of the welded material is prevented, the dispersibility is better provided, the amphiphilic silane coupling agent and lecithin are added to interact to form an organic silicon-phospholipid double-layer lubricating structure, the contact angle with a welding surface is increased, the surface tension is reduced, oxides on the surfaces of the welding flux and the welded parent metal are removed, the metal surface achieves good cleanliness, the metal surface can be continuously protected due to the film forming effect in the using process, and the welding assisting effect is provided.
Detailed Description
Surfactant (b): according to the mass ratio of 1: and 3-6, mixing sodium laureth sulfate and cetyl dimethyl amine oxide to obtain the surfactant.
Film-forming agent: according to the mass ratio of 10: 2: and 0.1-0.3 mixing the nitrocellulose, the acrylic resin and the OP-10 to obtain the film forming agent.
Antioxidant: according to the mass ratio of 6-11: 0.1 taking tert-butyl hydroquinone and nano SiO2Mixing to obtain antioxidant.
Preservative: according to the mass ratio of 1: 4-8: 0.1 mixing sodium benzoate, potassium sorbate, and poly Ɛ -lysine to obtain antiseptic.
Auxiliary agent: according to the mass ratio of 5-8: 1, mixing dopamine hydrochloride and aniline to obtain the auxiliary agent.
Pre-treating rice washing water: according to the mass ratio of 1: and (3) mixing rice and water 40-60, stirring for 5-10 min at a speed of 300-450 r/min, filtering, adding NaCl 3-7% of the mass of the filtrate into the filtrate, mixing, transferring to a sealed transparent glass bottle, sun-drying for 2-4 days, discharging to obtain a feed liquid, adding an acetic acid solution with the concentration of 2mol/L and the mass of 10% of the feed liquid into the feed liquid, and mixing to obtain the pretreated rice washing water.
Reagent: according to the mass ratio of 10-15: 0.1, mixing a citric acid solution with the concentration of 1mol/L and concentrated sulfuric acid with the mass fraction of 85 percent to obtain the reagent.
The preparation method of the composite modified rosin comprises the following steps:
(1) at the temperature of 25-35 ℃, according to the mass ratio of 1: 3-5, mixing rosin and toluene in a container, magnetically stirring for 30-55 min at a speed of 350-600 r/min, heating to 50-60 ℃, adding concentrated sulfuric acid with the mass being 5-8% of that of the rosin, mixing, preserving heat for 1-3 h, adding zinc chloride with the mass being 1-4% of that of the rosin, carrying out heat preservation reflux reaction for 5-7 h at a temperature of 100-110 ℃ to obtain a reactant, cleaning the reactant with deionized water at a temperature of 70-80 ℃, carrying out reduced pressure distillation to obtain polymerized rosin, heating the polymerized rosin in a vessel to 190-200 ℃, heating phenolic resin with the mass being 3-5 times of that of the polymerized rosin, mixing and stirring, heating to 230-240 ℃, adding pentaerythritol with the mass being 7-15% of that of the polymerized rosin and zinc oxide with the mass being 6-10% of that of the polymerized rosin, preserving heat for 1-3 h, heating to 260-280 ℃, preserving heat for 10-15 h, discharging, and;
(2) according to the mass ratio of 5: 4-7: 1-2, mixing maleopimaric acid, a reagent and polyethylene glycol in a reaction kettle, introducing nitrogen for protection, reacting for 1-3 hours at 200-220 ℃, cooling to 150-160 ℃, discharging to obtain an esterification mixture, and taking the esterification mixture according to a mass ratio of 1: 3-6: 0.01 of modified rosin and polyvinylpyrrolidone are added and mixed, and the mixture is magnetically stirred for 1 to 3 hours at the speed of 1000 to 1500r/min, so that the composite modified rosin is obtained.
Preparation of the compound auxiliary agent: taking 4-8 parts of microcrystalline paraffin, 3-5 parts of sodium dodecyl benzene sulfonate, 1-4 parts of lecithin, 2-5 parts of cyclohexanol, 4-8 parts of silane coupling agent KH-550 and 20-40 parts of water, mixing the silane coupling agent KH-550, the sodium dodecyl benzene sulfonate, the lecithin, the cyclohexanol and the water in a reaction kettle at 30-45 ℃, stirring and mixing at 1000-1200 r/min, adding the microcrystalline paraffin, transferring into a homogenizing emulsifying machine, emulsifying at 25-30 ℃ for 30-45 min to obtain an emulsion, standing and aging at room temperature for 3-5 h to obtain an aging solution, taking the aging solution, performing rotary evaporation at 70-90 ℃ and 400-500 kPa, performing reduced pressure concentration to 25-40% of the original volume to obtain a concentrated solution, and taking the concentrated solution according to the mass ratio of 8-12: 1, adding ammonium chloride, mixing, moving to an ultrasonic oscillator, and performing ultrasonic action for 15-25 min at the frequency of 55-65 kHz to obtain the composite auxiliary agent.
The flux for the photovoltaic module comprises the following components in parts by mass: 4-8 parts of polyethylene glycol, 3-7 parts of linolenic acid, 2-5 parts of antioxidant, 3-7 parts of film forming agent, 1-4 parts of preservative, 10-15 parts of surfactant, 6-10 parts of pretreated rice washing water, 1-4 parts of auxiliary agent, 30-50 parts of composite modified rosin and 12-25 parts of composite auxiliary agent.
A preparation method of the soldering flux for the photovoltaic module comprises the following steps:
(1) taking 4-8 parts of polyethylene glycol, 3-7 parts of linolenic acid, 2-5 parts of an antioxidant, 3-7 parts of a film forming agent, 1-4 parts of a preservative, 10-15 parts of a surfactant, 6-10 parts of pretreated rice washing water, 1-4 parts of an auxiliary agent, 30-50 parts of composite modified rosin and 12-25 parts of a composite auxiliary agent by weight;
(2) mixing polyethylene glycol, linolenic acid, a composite adjuvant, a surfactant and pretreated rice washing water in a reaction kettle at 35-55 ℃, magnetically stirring for 40-60 min at 350-600 r/min, heating to 90-110 ℃, adding an auxiliary agent, composite modified rosin, an antioxidant, a film forming agent and a preservative, mixing, and stirring for 1-3 h at 700-1000 r/min to obtain the soldering flux for the photovoltaic module.
Surfactant (b): according to the mass ratio of 1: and 3, mixing sodium laureth sulfate and cetyl dimethyl amine oxide to obtain the surfactant.
Film-forming agent: according to the mass ratio of 10: 2: 0.1 mixing the nitrocellulose, the acrylic resin and the OP-10 to obtain the film forming agent.
Antioxidant: according to the mass ratio of 6: 0.1 taking tert-butyl hydroquinone and nano SiO2Mixing to obtain antioxidant.
Preservative: according to the mass ratio of 1: 4: 0.1 mixing sodium benzoate, potassium sorbate, and poly Ɛ -lysine to obtain antiseptic.
Auxiliary agent: according to the mass ratio of 5: 1, mixing dopamine hydrochloride and aniline to obtain the auxiliary agent.
Pre-treating rice washing water: according to the mass ratio of 1: 40 mixing rice and water, stirring for 5min at a speed of 300r/min, filtering, adding 3% of NaCl by mass of the filtrate into the filtrate, mixing, transferring to a sealed transparent glass bottle, drying in the sun for 2 days, discharging to obtain a feed liquid, adding 10% of acetic acid solution with the concentration of 2mol/L by mass of the feed liquid into the feed liquid, and mixing to obtain the pretreated rice washing water.
Reagent: according to the mass ratio of 10: 0.1, mixing a citric acid solution with the concentration of 1mol/L and concentrated sulfuric acid with the mass fraction of 85 percent to obtain the reagent.
The preparation method of the composite modified rosin comprises the following steps:
(1) at 25 ℃, according to the mass ratio of 1: 3, mixing rosin and toluene in a container, magnetically stirring for 30min at 350r/min, heating to 50 ℃, adding concentrated sulfuric acid with the mass of 5% of that of the rosin, mixing, keeping the temperature for 1h, adding zinc chloride with the mass of 1% of that of the rosin, keeping the temperature at 100 ℃, carrying out reflux reaction for 5h to obtain a reactant, cleaning the reactant with deionized water at 70 ℃, carrying out reduced pressure distillation to obtain polymerized rosin, heating the polymerized rosin to 190 ℃ in a vessel, heating phenolic resin with the mass of 3 times of that of the polymerized rosin, mixing and stirring, heating to 230 ℃, adding pentaerythritol with the mass of 7% of that of the polymerized rosin and zinc oxide with the mass of 6% of that of the polymerized rosin, keeping the temperature for 1h, heating to 260 ℃, keeping the temperature for 10h, discharging, and naturally cooling to obtain;
(2) according to the mass ratio of 5: 4: 1, mixing maleopimaric acid, a reagent and polyethylene glycol in a reaction kettle, introducing nitrogen for protection, reacting for 1h at 200 ℃, cooling to 150 ℃, discharging to obtain an esterification mixture, and taking the esterification mixture according to a mass ratio of 1: 3: 0.01 adding the modified rosin and polyvinylpyrrolidone, mixing, and magnetically stirring for 1h at 1000r/min to obtain the composite modified rosin.
Preparation of the compound auxiliary agent: taking 4 parts of microcrystalline paraffin, 3 parts of sodium dodecyl benzene sulfonate, 1 part of lecithin, 2 parts of cyclohexanol, 4 parts of silane coupling agent KH-550 and 20 parts of water, mixing the silane coupling agent KH-550, the sodium dodecyl benzene sulfonate, the lecithin, the cyclohexanol and the water in a reaction kettle at 30 ℃, stirring and mixing at 1000r/min, adding the microcrystalline paraffin, moving the mixture into a homogenizing and emulsifying machine, emulsifying at 25 ℃ for 30min to obtain an emulsion, standing and aging at room temperature for 3h to obtain an aging solution, taking the aging solution, performing rotary evaporation at 70 ℃ and 400kPa to obtain a concentrated solution, and concentrating the concentrated solution to 25% of the original volume to obtain the concentrated solution, wherein the mass ratio of the concentrated solution is 8: 1, adding ammonium chloride, mixing, moving to an ultrasonic oscillator, and performing ultrasonic action at 55kHz frequency for 15min to obtain the composite auxiliary agent.
The flux for the photovoltaic module comprises the following components in parts by mass: 4 parts of polyethylene glycol, 3 parts of linolenic acid, 2 parts of antioxidant, 3 parts of film forming agent, 1 part of preservative, 10 parts of surfactant, 6 parts of pretreated rice washing water, 1 part of auxiliary agent, 30 parts of composite modified rosin and 12 parts of composite auxiliary agent.
A preparation method of the soldering flux for the photovoltaic module comprises the following steps:
(1) taking 4 parts of polyethylene glycol, 3 parts of linolenic acid, 2 parts of antioxidant, 3 parts of film forming agent, 1 part of preservative, 10 parts of surfactant, 6 parts of pretreated rice washing water, 1 part of auxiliary agent, 30 parts of composite modified rosin and 12 parts of composite auxiliary agent in parts by weight;
(2) mixing polyethylene glycol, linolenic acid, a composite auxiliary agent, a surfactant and pretreated rice washing water in a reaction kettle at 35 ℃, magnetically stirring for 40min at 350r/min, heating to 90 ℃, adding an auxiliary agent, composite modified rosin, an antioxidant, a film forming agent and a preservative, mixing, and stirring for 1h at 700r/min to obtain the soldering flux for the photovoltaic module.
Surfactant (b): according to the mass ratio of 1: and 5, mixing sodium laureth sulfate and cetyl dimethyl amine oxide to obtain the surfactant.
Film-forming agent: according to the mass ratio of 10: 2: 0.2 mixing the nitrocellulose, the acrylic resin and the OP-10 to obtain the film forming agent.
Antioxidant: according to the mass ratio of 8: 0.1 tert-butyl-p-benzeneDiphenol, nano SiO2Mixing to obtain antioxidant.
Preservative: according to the mass ratio of 1: 6: 0.1 mixing sodium benzoate, potassium sorbate, and poly Ɛ -lysine to obtain antiseptic.
Auxiliary agent: according to the mass ratio of 6: 1, mixing dopamine hydrochloride and aniline to obtain the auxiliary agent.
Pre-treating rice washing water: according to the mass ratio of 1: and 50, mixing rice and water, stirring for 8min at 375r/min, filtering, adding NaCl with the mass of 5% of the filtrate into the filtrate, mixing, transferring to a sealed transparent glass bottle, sun-drying for 3 days, discharging to obtain a feed liquid, adding an acetic acid solution with the concentration of 2mol/L and the mass of 10% of the feed liquid into the feed liquid, and mixing to obtain the pre-treated rice washing water.
Reagent: according to the mass ratio of 13: 0.1, mixing a citric acid solution with the concentration of 1mol/L and concentrated sulfuric acid with the mass fraction of 85 percent to obtain the reagent.
The preparation method of the composite modified rosin comprises the following steps:
(1) at 30 ℃, according to the mass ratio of 1: 4, mixing rosin and toluene in a container, magnetically stirring for 38min at a speed of 425r/min, heating to 55 ℃, adding concentrated sulfuric acid with the mass of 6% of that of the rosin, keeping the temperature for 2h, adding zinc chloride with the mass of 2% of that of the rosin, keeping the temperature at 105 ℃, carrying out reflux reaction for 6h to obtain a reactant, cleaning the reactant with deionized water at 75 ℃, carrying out reduced pressure distillation to obtain polymerized rosin, heating the polymerized rosin to 195 ℃ in a vessel, heating phenolic resin with the mass of 4 times that of the polymerized rosin, mixing and stirring, heating to 235 ℃, adding pentaerythritol with the mass of 11% of that of the polymerized rosin and zinc oxide with the mass of 8% of that of the polymerized rosin, keeping the temperature for 2h, heating to 270 ℃, keeping the temperature for 13h, discharging, and naturally cooling to obtain;
(2) according to the mass ratio of 5: 5: 1.5 taking maleopimaric acid, a reagent and polyethylene glycol to mix in a reaction kettle, introducing nitrogen for protection, reacting for 2 hours at 210 ℃, cooling to 155 ℃, discharging to obtain an esterification mixture, and taking the esterification mixture according to a mass ratio of 1: 5: 0.01 adding the modified rosin and polyvinylpyrrolidone, mixing, and stirring for 2 hours at 1250r/min by magnetic force to obtain the composite modified rosin.
Preparation of the compound auxiliary agent: taking 6 parts of microcrystalline paraffin, 4 parts of sodium dodecyl benzene sulfonate, 2 parts of lecithin, 3 parts of cyclohexanol, 6 parts of silane coupling agent KH-550 and 30 parts of water, mixing the silane coupling agent KH-550, the sodium dodecyl benzene sulfonate, the lecithin, the cyclohexanol and the water in a reaction kettle at 37 ℃, stirring and mixing at 1100r/min, adding the microcrystalline paraffin, moving the mixture into a homogenizing and emulsifying machine, emulsifying at 28 ℃ for 37min to obtain an emulsion, standing and aging at room temperature for 4h to obtain an aging solution, taking the aging solution, performing rotary evaporation at the temperature of 80 ℃ and the pressure of 450kPa to obtain a concentrated solution, and concentrating the concentrated solution to 33 percent of the original volume to obtain the concentrated solution according to the mass ratio of 10: 1, adding ammonium chloride, mixing, moving to an ultrasonic oscillator, and performing ultrasonic action at 60kHz frequency for 20min to obtain the composite auxiliary agent.
The flux for the photovoltaic module comprises the following components in parts by mass: 6 parts of polyethylene glycol, 5 parts of linolenic acid, 3 parts of antioxidant, 5 parts of film forming agent, 3 parts of preservative, 12 parts of surfactant, 8 parts of pretreated rice washing water, 2 parts of auxiliary agent, 40 parts of composite modified rosin and 18 parts of composite auxiliary agent.
A preparation method of the soldering flux for the photovoltaic module comprises the following steps:
(1) according to the mass parts, taking 6 parts of polyethylene glycol, 5 parts of linolenic acid, 3 parts of antioxidant, 5 parts of film forming agent, 3 parts of preservative, 12 parts of surfactant, 8 parts of pretreated rice washing water, 2 parts of auxiliary agent, 40 parts of composite modified rosin and 18 parts of composite auxiliary agent;
(2) mixing polyethylene glycol, linolenic acid, a composite auxiliary agent, a surfactant and pretreated rice washing water in a reaction kettle at 45 ℃, magnetically stirring for 50min at 475r/min, heating to 100 ℃, adding an auxiliary agent, composite modified rosin, an antioxidant, a film forming agent and a preservative, mixing, and stirring for 2h at 850r/min to obtain the soldering flux for the photovoltaic module.
Surfactant (b): according to the mass ratio of 1: and 6, mixing sodium laureth sulfate and cetyl dimethyl amine oxide to obtain the surfactant.
Film-forming agent: according to the mass ratio of 10: 2: 0.3 mixing the nitrocellulose, the acrylic resin and the OP-10 to obtain the film forming agent.
Antioxidant: according to the mass ratio of 11: 0.1 taking tert-butyl hydroquinone and nano SiO2Mixing to obtain antioxidant.
Preservative: according to the mass ratio of 1: 8: 0.1 mixing sodium benzoate, potassium sorbate, and poly Ɛ -lysine to obtain antiseptic.
Auxiliary agent: according to the mass ratio of 8: 1, mixing dopamine hydrochloride and aniline to obtain the auxiliary agent.
Pre-treating rice washing water: according to the mass ratio of 1: 60, mixing rice and water, stirring for 10min at the speed of 450r/min, filtering, adding NaCl with the mass of 7% of the filtrate into the filtrate, mixing, transferring to a sealed transparent glass bottle, drying for 4 days, discharging to obtain a feed liquid, adding an acetic acid solution with the concentration of 2mol/L and the mass of 10% of the feed liquid into the feed liquid, and mixing to obtain the pre-treated rice washing water.
Reagent: according to the mass ratio of 15: 0.1, mixing a citric acid solution with the concentration of 1mol/L and concentrated sulfuric acid with the mass fraction of 85 percent to obtain the reagent.
The preparation method of the composite modified rosin comprises the following steps:
(1) at 35 ℃, according to the mass ratio of 1: 5, mixing rosin and toluene in a container, magnetically stirring for 55min at a speed of 600r/min, heating to 60 ℃, adding concentrated sulfuric acid accounting for 8% of the mass of the rosin, mixing, preserving heat for 3h, adding zinc chloride accounting for 4% of the mass of the rosin, preserving heat, refluxing for 7h at 110 ℃ to obtain a reactant, cleaning the reactant with deionized water at 80 ℃, distilling under reduced pressure to obtain polymerized rosin, heating the polymerized rosin to 200 ℃ in a container, heating phenolic resin accounting for 5 times of the mass of the polymerized rosin, mixing and stirring, heating to 240 ℃, adding pentaerythritol accounting for 15% of the mass of the polymerized rosin and zinc oxide accounting for 10% of the mass of the polymerized rosin, preserving heat for 3h, heating to 280 ℃, preserving heat for 15h, discharging, and naturally cooling to obtain modified rosin;
(2) according to the mass ratio of 5: 7: 2, mixing maleopimaric acid, a reagent and polyethylene glycol in a reaction kettle, introducing nitrogen for protection, reacting for 3 hours at 220 ℃, cooling to 160 ℃, discharging to obtain an esterification mixture, and taking the esterification mixture according to a mass ratio of 1: 6: 0.01 adding the modified rosin and polyvinylpyrrolidone, mixing, and magnetically stirring for 3h at 1500r/min to obtain the composite modified rosin.
Preparation of the compound auxiliary agent: taking 8 parts of microcrystalline paraffin, 5 parts of sodium dodecyl benzene sulfonate, 4 parts of lecithin, 5 parts of cyclohexanol, 8 parts of silane coupling agent KH-550 and 40 parts of water, mixing the silane coupling agent KH-550, the sodium dodecyl benzene sulfonate, the lecithin, the cyclohexanol and the water in a reaction kettle at 45 ℃, stirring and mixing at 1200r/min, adding the microcrystalline paraffin, moving the mixture into a homogenizing and emulsifying machine, emulsifying at 30 ℃ for 45min to obtain an emulsion, standing and aging at room temperature for 5h to obtain an aging solution, taking the aging solution, performing rotary evaporation at 90 ℃ and 500kPa to obtain a concentrated solution, and concentrating the concentrated solution to 40% of the original volume to obtain the concentrated solution according to the mass ratio of 12: 1, adding ammonium chloride, mixing, moving to an ultrasonic oscillator, and performing ultrasonic action at 65kHz frequency for 25min to obtain the composite auxiliary agent.
The flux for the photovoltaic module comprises the following components in parts by mass: 8 parts of polyethylene glycol, 7 parts of linolenic acid, 5 parts of antioxidant, 7 parts of film forming agent, 4 parts of preservative, 15 parts of surfactant, 10 parts of pretreated rice washing water, 4 parts of auxiliary agent, 50 parts of composite modified rosin and 25 parts of composite auxiliary agent.
A preparation method of the soldering flux for the photovoltaic module comprises the following steps:
(1) according to the mass parts, taking 8 parts of polyethylene glycol, 7 parts of linolenic acid, 5 parts of antioxidant, 7 parts of film forming agent, 4 parts of preservative, 15 parts of surfactant, 10 parts of pretreated rice washing water, 4 parts of auxiliary agent, 50 parts of composite modified rosin and 25 parts of composite auxiliary agent;
(2) mixing polyethylene glycol, linolenic acid, a composite auxiliary agent, a surfactant and pretreated rice washing water in a reaction kettle at 55 ℃, magnetically stirring for 60min at 600r/min, heating to 110 ℃, adding an auxiliary agent, composite modified rosin, an antioxidant, a film forming agent and a preservative, mixing, and stirring for 3h at 1000r/min to obtain the soldering flux for the photovoltaic module.
Comparative example 1: the procedure was essentially the same as in example 1 except that the complex modified rosin was absent.
Comparative example 2: the procedure was essentially the same as in example 1 except that the auxiliary composition was absent.
Comparative example 3: flux for photovoltaic modules produced by a company in Dongguan.
The flux for photovoltaic modules obtained in the examples and the comparative examples was tested according to the GB/T15829 standard, and the test results are shown in Table 1.
TABLE 1
| Test items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Conductivity (W/mk) | 45 | 43 | 44 | 39 | 40 | 22 |
| Expansion ratio (%) | 90.1 | 89.4 | 89.7 | 81.5 | 82.6 | 69.9 |
| Degree of ionic contamination (. mu.g/cm)2） | 0.7 | 0.9 | 0.8 | 1.2 | 1.6 | 3.1 |
In conclusion, compared with the commercial product, the soldering flux for the photovoltaic module has better effect and is worthy of great popularization.
Claims (5)
1. The flux for the photovoltaic module comprises the following components in parts by mass: 4~8 parts of polyethylene glycol, 3~7 parts of linolenic acid, 2~5 parts of antioxidant, 3~7 parts of film-forming agent, 1~4 parts of preservative, 10~15 parts of surfactant, 6~10 parts of pretreatment rice washing water, 1~4 parts of auxiliary agent, and its characterized in that still includes: 30-50 parts of composite modified rosin and 12-25 parts of composite auxiliary agent;
the preparation method of the composite modified rosin comprises the following steps:
(1) at the temperature of 25-35 ℃, according to the mass ratio of 1: 3-5, mixing and stirring rosin and toluene, heating to 50-60 ℃, adding concentrated sulfuric acid with the mass being 5-8% of that of the rosin, keeping the temperature, adding zinc chloride with the mass being 1-4% of that of the rosin, mixing, keeping the temperature at 100-110 ℃, carrying out reflux reaction to obtain a reactant, washing the reactant, carrying out reduced pressure distillation to obtain polymerized rosin, heating the polymerized rosin to 190-200 ℃, heating phenolic resin with the mass being 3-5 times of that of the polymerized rosin, mixing and stirring, heating to 230-240 ℃, adding pentaerythritol with the mass being 7-15% of that of the polymerized rosin and zinc oxide with the mass being 6-10% of that of the polymerized rosin, keeping the temperature, heating to 260-280 ℃, keeping the temperature, discharging, and cooling to obtain modified rosin;
(2) according to the mass ratio of 5: 4-7: 1-2, mixing maleopimaric acid, a reagent and polyethylene glycol, introducing nitrogen for protection, reacting for 1-3 hours at 200-220 ℃, cooling to 150-160 ℃, discharging to obtain an esterification mixture, and taking the esterification mixture according to a mass ratio of 1: 3-6: 0.01 adding the modified rosin and polyvinylpyrrolidone, mixing and stirring to obtain the composite modified rosin; the reagent is as follows: according to the mass ratio of 10-15: 0.1, mixing citric acid solution and concentrated sulfuric acid to obtain a reagent;
the preparation of the compound auxiliary agent comprises the following steps: taking 4-8 parts of microcrystalline paraffin, 3-5 parts of sodium dodecyl benzene sulfonate, 1-4 parts of lecithin, 2-5 parts of cyclohexanol, 4-8 parts of silane coupling agent KH-550 and 20-40 parts of water, mixing and stirring the silane coupling agent KH-550, the sodium dodecyl benzene sulfonate, the lecithin, the cyclohexanol and the water at 30-45 ℃, adding the microcrystalline paraffin, emulsifying at 25-30 ℃ to obtain an emulsion, standing and aging at room temperature to obtain an aging solution, taking the aging solution for rotary evaporation and reduced pressure concentration to obtain a concentrated solution, and taking the concentrated solution according to the mass ratio of 8-12: 1, adding ammonium chloride, mixing and performing ultrasonic action to obtain a composite auxiliary agent;
the auxiliary agent is as follows: according to the mass ratio of 5-8: 1, mixing dopamine hydrochloride and aniline to obtain an auxiliary agent;
the rice washing water pretreatment: according to the mass ratio of 1: and 40-60 taking rice and water, mixing and stirring, filtering, adding NaCl accounting for 3-7% of the mass of the filtrate into the filtrate, mixing, drying in the sun, discharging to obtain a material liquid, adding an acetic acid solution accounting for 10% of the mass of the material liquid into the material liquid, and mixing to obtain the pretreated rice washing water.
2. The flux for photovoltaic modules according to claim 1, wherein the preservative: according to the mass ratio of 1: 4-8: 0.1 mixing sodium benzoate, potassium sorbate, and poly Ɛ -lysine to obtain antiseptic.
3. The flux for a photovoltaic module according to claim 1, wherein the film-forming agent: according to the mass ratio of 10: 2: and 0.1-0.3 mixing the nitrocellulose, the acrylic resin and the OP-10 to obtain the film forming agent.
4. The flux for photovoltaic modules according to claim 1, wherein the antioxidant: according to the mass ratio of 6-11: 0.1 taking tert-butyl hydroquinone and nano SiO2Mixing to obtain antioxidant.
5. The flux for photovoltaic modules according to claim 1, wherein the surfactant: according to the mass ratio of 1: and 3-6, mixing sodium laureth sulfate and cetyl dimethyl amine oxide to obtain the surfactant.
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| CN104084714B (en) * | 2014-07-30 | 2016-08-24 | 广西众昌树脂有限公司 | Rosin flux |
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