CN116174996B - Slag removing agent and preparation method thereof - Google Patents

Slag removing agent and preparation method thereof Download PDF

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Publication number
CN116174996B
CN116174996B CN202310057549.3A CN202310057549A CN116174996B CN 116174996 B CN116174996 B CN 116174996B CN 202310057549 A CN202310057549 A CN 202310057549A CN 116174996 B CN116174996 B CN 116174996B
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Prior art keywords
slag
removing agent
slag removing
acid
tin
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CN116174996A (en
Inventor
郑爱霞
许征峰
王建
王明
李宁成
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Ningcheng New Material Technology Suzhou Co ltd
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Ningcheng New Material Technology Suzhou Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection 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
    • B23K35/3612Selection 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Nonmetallic Welding Materials (AREA)

Abstract

The invention belongs to the technical field of welding flux, and relates to a slag removing agent and a preparation method thereof. The slag remover comprises the following components in percentage by mass: 15-78% of solvent, 20-84% of fatty acid and 1-2% of surfactant. After the slag removing agent is used, the tin slag amount can be effectively reduced, the slag removing efficiency can reach more than 90%, and the problems of low cost, no pollution, no corrosion and easy operation can be solved.

Description

Slag removing agent and preparation method thereof
Technical Field
The invention belongs to the technical field of welding flux, and relates to a slag removing agent and a preparation method thereof.
Background
Wave soldering plays an important role in the soldering quality of electronic products as an important soldering process. During the process, large-area molten solder is exposed to air, and new solder is continuously contacted with oxygen in the air in the welding process to be oxidized to form tin oxide slag. Tin is a very readily oxidizable metal, snO, from the thermodynamic oxidation perspective 2 The standard Gibbs free energy of formation reaches-515.8 KJ/mol. The Sn ratio of the lead-free SnCu solder is much higher than that of the lead-containing solder, and the Sn ratio of the lead-free SnBi solder is not high, but the Sn ratio is higher than that of the lead-containing solder 2 O 3 It can be seen that it oxidizes more readily than Sn and thus lead-free solders oxidize more readily than lead-free solders, as can be seen in the thermodynamic generation standard gibbs free energy-570 KJ/mol. As the lead-free solder gradually replaces the conventional 63Sn37Pb solder, the amount of tin oxide slag is increased, which is continuously generated and accumulated on the surface of the molten solder, not only can the fluidity of the liquid solder be affected to reduce the wettability of the solder, but also the PCBA board can be polluted, and the welding quality and reliability of the product can be affected. Since the solder oxide has a sponge-like network structure, the structure readily encapsulates the useful solder therein, and the agitation of the tin pump, and tumbling of the solder wave, further exacerbates the encapsulation. So we can speak of tin dross that contains not only oxides of the solder but alsoIncluding useful solders encapsulated in oxides. It is counted that this portion of the encapsulated solder may account for more than 90% of the total solder residue.
The slag output of each wave soldering furnace is about 10kg per day, and the economic loss is caused by the waste of the solder. The method for reducing tin dross used in the market at present mainly comprises the following steps: 1. the method of filling nitrogen into the wave soldering furnace can also have the effect, but the cost is high. 2. The method of using a solid powder reducing agent, such solid powder tends to fly off on the plate to cause residue, and a large amount of smoke is generated. 3. The chemical formula of the anti-oxidation reducing agent has lower efficiency, and the strong acid formula is mostly adopted to easily cause corrosion of a tin furnace.
Disclosure of Invention
The invention aims to provide a slag removing agent which can effectively reduce the amount of tin slag after being used, has the slag removing efficiency of more than 90 percent, and can solve the problem of tin slag with low cost, no pollution, no corrosion and easy operation.
The technical scheme adopted for solving the technical problems is as follows:
the slag remover comprises the following components in percentage by mass: 15-78% of solvent, 20-84% of fatty acid and 1-2% of surfactant.
The slag remover has excellent performance of removing solder slag, and can greatly reduce the consumption of solder under the condition of not changing the original process and materials.
Preferably, the solvent is one or more selected from glycerol, fatty alcohol polyoxyethylene ether and polyethylene glycol.
Preferably, the fatty acid is one or more selected from phytic acid, oleic acid and dimer acid. The phytic acid needs to be prepared into an aqueous solution in advance and added into the system.
Preferably, the surfactant is selected from one or two of sodium tripolyphosphate and sodium lignin sulfonate.
Preferably, the solvent consists of two components of glycerin, fatty alcohol polyoxyethylene ether and polyethylene glycol, wherein one component is glycerin, the weight ratio of the glycerin is 10-48% of the total weight of the slag removing agent, and the other component is fatty alcohol polyoxyethylene ether or polyethylene glycol, and the weight ratio of the fatty alcohol polyoxyethylene ether or polyethylene glycol is 5-30% of the total weight of the slag removing agent.
Preferably, the slag removing agent comprises the following components in percentage by mass: 48% of glycerol, 30% of polyethylene glycol, 2% of sodium tripolyphosphate and 20% of phytic acid.
Preferably, the slag removing agent comprises the following components in percentage by mass: 20% of glycerol, 10% of fatty alcohol polyoxyethylene ether, 1% of sodium lignin sulfonate and 69% of oleic acid.
Preferably, the slag removing agent comprises the following components in percentage by mass: 10% of glycerol, 5% of polyethylene glycol, 1% of sodium tripolyphosphate, 5% of phytic acid, 34% of oleic acid and 45% of dimer acid.
The invention relates to a preparation method of a slag removing agent, which comprises the following steps: mixing surfactant and solvent in the amount of the formula, heating to 120+/-10 ℃ while stirring, adding fatty acid to disperse uniformly, and naturally cooling to obtain pale yellow or colorless liquid.
The beneficial effects of the invention are as follows:
the invention has the advantages that the tin slag amount can be effectively reduced, the slag removing efficiency can reach more than 90 percent, the used solvent has good wetting and penetrating effects, and meanwhile, the used surfactant has the characteristic that one end is completely compatible with the slag removing agent, and the other end can be well adsorbed on the surface of the oxide; meanwhile, the slag remover covers the surface of the molten solder, thereby playing the roles of isolating air and preventing the solder from oxidizing. Because the tin slag reduction process does not involve oxidation-reduction reaction, and the slag remover solution is close to neutral, the corrosion to stainless steel, titanium alloy and cast iron furnace bodies with ceramic coatings can be avoided. The slag removing agent has good thermal stability, does not decompose below 300 ℃ and does not produce smoke pollution.
The slag removing effect of the slag removing agent is verified by two methods: 1. 284.4g of SnBi tin slag is added into a beaker, then 100g of slag removing agent is added, the mixture is placed on a heating table and heated to 180 ℃, heating is stopped when the tin slag is completely melted into metal, the beaker is taken down for cooling, the SnBi alloy which is melted into a whole is taken out of the beaker, and the alloy of 275.3g is obtained by cleaning and weighing with isopropanol. Calculated slag removing efficiency is 96.8%. When SnCu tin slag is used, the slag removal efficiency is slightly lower than about 90%.2. A small tin furnace is used for a simulation experiment, tin bars are added into the small tin furnace, about 30g of slag removing agent is added on the surface of the tin bars after the tin bars are melted, the whole small tin furnace surface is covered, meanwhile, air is blown into the small tin furnace to accelerate alloy oxidation, the amount of tin slag on the surface of the tin furnace is observed after two hours, a large amount of tin slag appears on the surface of the tin furnace without slag removing agent, and the surface of the tin furnace with slag removing agent is added on the surface of the tin furnace, and almost no tin slag is generated except for the viscosity of the slag removing agent due to reaction (see fig. 1 and 2).
Drawings
FIG. 1 is a view of the surface of a small tin furnace without slag remover after 2h of blowing;
FIG. 2 is the surface of a small tin furnace with slag remover added after 2h of blowing;
FIG. 3 is a surface of a tin furnace without slag remover;
FIG. 4 is a surface of a tin furnace with slag remover added.
Detailed Description
The technical scheme of the invention is further specifically described by the following specific examples. It should be understood that the practice of the invention is not limited to the following examples, but is intended to be within the scope of the invention in any form and/or modification thereof.
In the present invention, unless otherwise specified, all parts and percentages are by weight, and the equipment, materials, etc. used are commercially available or are conventional in the art. The methods in the following examples are conventional in the art unless otherwise specified.
The invention provides a slag removing agent, which mainly comprises a solvent, fatty acid and a surfactant.
The slag removing agent prepared by the components comprises the following components in percentage by mass: 5-50% of solvent, 20-95% of fatty acid and 1-10% of surfactant.
The physicochemical properties of the present invention are elucidated as follows:
the slag remover of the invention is colorless or yellowish transparent viscous liquid, has no toxicity and stimulation, and has the relative density of about 0.95+/-0.05 g/cm 3 The plastic container should be protected from direct irradiation of sunlight, and can be stored for 2 years at room temperature.
The product is odorless and pollution-free, and original ventilation equipment is not required to be changed.
The invention is liquid, easy to operate, and can be directly added into a tin furnace, and the specific gravity of the invention is small, and the invention can cover the surface of the tin liquid and can not sink into the molten tin to cause solder pollution. The slag removing agent is consumed along with time and temperature, and when the slag removing agent on the upper layer of the tin material is found to be more viscous, a part of slag removing agent is fished out by a strainer like the process of salvaging tin slag, and then new slag removing agent is added.
The slag reduction principle of the invention is explained as follows:
(1) The slag remover covers the surface of the molten solder to form a layer of protective film, which isolates the contact between the solder and air, thereby playing a role in preventing the oxidation of fresh solder.
(2) The solvent and the surfactant in the slag removing agent have good wetting and penetrating effects, so that fatty acid in the slag removing agent reacts with metal oxide to generate a metal salt structure without a wrapping shape, thereby opening a reticular matrix of the tin slag oxide and releasing available metal back into the furnace.
Example 1:
the slag remover consists of the following components in percentage by mass: 48% of glycerol, 30% of polyethylene glycol, 2% of sodium tripolyphosphate and 20% of phytic acid, and the specific formula is shown in table 1.
Because of the solubility, the phytic acid is firstly added with a proper amount of water to prepare a phytic acid solution, and then the phytic acid solution is mixed with other components.
The preparation method of the slag removing agent comprises the following steps:
A. heating glycerol and polyethylene glycol to 120deg.C, stirring while heating, mixing, adding sodium tripolyphosphate, and stirring for 20min.
B. And (c) slowly adding the phytic acid solution into the mixed solution obtained in the step (A), and stirring for 30-50 min to fully evaporate water in the phytic acid solution to obtain a pale yellow clear solution.
C. After full reaction, gradually reducing the temperature to room temperature to obtain the pale yellow slag remover.
Example 2:
the slag remover consists of the following components in percentage by mass: 20% of glycerol, 10% of fatty alcohol polyoxyethylene ether, 1% of sodium lignin sulfonate and 69% of oleic acid.
The preparation method of the slag removing agent comprises the following steps:
A. heating the glycerin and the fatty alcohol-polyoxyethylene ether to 120 ℃, stirring while heating, adding sodium lignin sulfonate after uniformly mixing, and stirring for 20min.
B. And adding oleic acid, and stirring for 30-50 min to obtain colorless clear solution.
C. After sufficient reaction, the temperature was gradually lowered to room temperature to obtain a colorless slag remover solution.
Example 3:
the slag remover consists of the following components in percentage by mass: 10% of glycerol, 5% of polyethylene glycol, 1% of sodium tripolyphosphate, 5% of phytic acid, 34% of oleic acid and 45% of dimer acid.
The preparation method of the slag removing agent comprises the following steps:
A. heating glycerol and polyethylene glycol to 120deg.C, stirring while heating, mixing, adding sodium tripolyphosphate, and stirring for 20min.
B. And (c) slowly adding the phytic acid solution into the mixed solution obtained in the step (A), stirring for 30-50 min, fully evaporating water in the phytic acid solution to obtain a pale yellow clear solution, adding oleic acid and dimer acid, and stirring for 30min.
C. After full reaction, gradually reducing the temperature to room temperature to obtain the pale yellow slag remover.
Table 1 (wt.%)
Example 4:
this example provides an application case of a slag remover, which uses the slag remover prepared in example 3.
1. The using steps are as follows:
on-line test was performed at a company, about 400kg of solder was put into the test, and 500g of slag remover was added after the solder was melted. The test was performed for a total of 2 days. Continuously running for 8 hours on the 1 st day, and shutting down; restarting on the 2 nd day, continuously running for 8 hours, and ending. Every 4 hours, the welding slag is fished out, and then a proper amount of slag removing agent is added. Adding 1kg of slag removing agent in the whole process.
2. Results
1. The surface of the tin furnace added with the slag removing agent has a small amount of tin slag, the welding slag is dissolved in the slag removing agent after being slightly stirred, and 2.34kg of welding slag is fished out after 16 hours; a large amount of tin slag appears on the surface of the tin furnace without slag removing agent, and 50.71kg of tin slag is produced in total after 16 hours. The slag removing efficiency reaches 95 percent.
2. And carrying out equipment corrosion simulation verification experiments by combining the material and actual use conditions of the user tin furnace equipment.
1L of slag remover solution is prepared, the slag remover solution is poured into 3 different beakers to be heated and stabilized at 260 ℃, and a stainless steel plate, a titanium alloy plate and a ceramic plate which are made of the same material as tin furnace equipment are respectively added into the 3 beakers and are completely immersed by the slag remover solution. The sample was taken out after being immersed in 260 ° slag remover solution for one week, washed with isopropyl alcohol, dried and weighed. The weight loss of the three samples before and after soaking does not occur, which indicates that the slag remover cannot cause corrosion to the tin furnace.
FIG. 1 is a view of the surface of a small tin furnace without slag remover after 2h of blowing; FIG. 2 is the surface of a small tin furnace with slag remover added after 2h of blowing; FIG. 3 is a surface of a tin furnace without slag remover; FIG. 4 is a surface of a tin furnace with slag remover added.
3. The slag removing agent does not contain N and P, is environment-friendly, and reduces the environmental protection pressure of users. The smoke is not generated when the air conditioner is heated at high temperature, and original ventilation equipment is not required to be changed.
In this specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, so that the same or similar parts between the embodiments are referred to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The slag removing agent and the preparation method thereof provided by the invention are described in detail. The principles and embodiments of the present invention have been described herein with reference to specific examples, the description of which is intended only to facilitate an understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.

Claims (6)

1. The slag removing agent is characterized by comprising the following components in percentage by mass: 15-78% of solvent, 20-84% of fatty acid and 1-2% of surfactant; the solvent is one or more selected from glycerol, fatty alcohol polyoxyethylene ether and polyethylene glycol; the fatty acid is one or more selected from phytic acid, oleic acid and dimer acid; the surfactant is selected from one or two of sodium tripolyphosphate and sodium lignin sulfonate.
2. The slag remover as set forth in claim 1, wherein: the solvent consists of two components of glycerin, fatty alcohol polyoxyethylene ether and polyethylene glycol, wherein one component is glycerin, the weight ratio of the glycerin is 10-48% of the total weight of the slag removing agent, and the other component is fatty alcohol polyoxyethylene ether or polyethylene glycol, and the weight ratio of the glycerin is 5-30% of the total weight of the slag removing agent.
3. The slag remover as set forth in claim 1, wherein: the slag removing agent comprises the following components in percentage by mass: 48% of glycerol, 30% of polyethylene glycol, 2% of sodium tripolyphosphate and 20% of phytic acid.
4. The slag remover as set forth in claim 1, wherein: the slag removing agent comprises the following components in percentage by mass: 20% of glycerol, 10% of fatty alcohol polyoxyethylene ether, 1% of sodium lignin sulfonate and 69% of oleic acid.
5. The slag remover as set forth in claim 1, wherein: the slag removing agent comprises the following components in percentage by mass: 10% of glycerol, 5% of polyethylene glycol, 1% of sodium tripolyphosphate, 5% of phytic acid, 34% of oleic acid and 45% of dimer acid.
6. A process for the preparation of a slag remover according to any of claims 1 to 5, characterized in that it comprises:
mixing surfactant and solvent in the amount of the formula, heating to 120+/-10 ℃ while stirring, adding fatty acid to disperse uniformly, and naturally cooling to obtain pale yellow or colorless liquid.
CN202310057549.3A 2023-01-18 2023-01-18 Slag removing agent and preparation method thereof Active CN116174996B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04228288A (en) * 1990-03-30 1992-08-18 Internatl Business Mach Corp <Ibm> Composite solder/polymer paste and method for producing the same
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
CN101532130A (en) * 2009-01-12 2009-09-16 深圳市堃琦鑫华科技有限公司 Molten metal anti-oxidation reducing agent, preparation method and application thereof
CN101613807A (en) * 2009-08-03 2009-12-30 黄俊凯 Solder dross reducing agent
CN102162039A (en) * 2010-02-24 2011-08-24 诸葛秀英 Super tin slag reducing agent
CN103212921A (en) * 2012-06-26 2013-07-24 深圳市堃琦鑫华科技有限公司 Reductant composition and preparation method thereof, and welding method
CN104057218A (en) * 2013-03-22 2014-09-24 深圳市菲尼的科技有限公司 Novel soldering tin purifying agent

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6540788B1 (en) * 2017-12-29 2019-07-10 千住金属工業株式会社 Flux and solder paste

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04228288A (en) * 1990-03-30 1992-08-18 Internatl Business Mach Corp <Ibm> Composite solder/polymer paste and method for producing the same
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
CN101532130A (en) * 2009-01-12 2009-09-16 深圳市堃琦鑫华科技有限公司 Molten metal anti-oxidation reducing agent, preparation method and application thereof
CN101613807A (en) * 2009-08-03 2009-12-30 黄俊凯 Solder dross reducing agent
CN102162039A (en) * 2010-02-24 2011-08-24 诸葛秀英 Super tin slag reducing agent
CN103212921A (en) * 2012-06-26 2013-07-24 深圳市堃琦鑫华科技有限公司 Reductant composition and preparation method thereof, and welding method
CN104057218A (en) * 2013-03-22 2014-09-24 深圳市菲尼的科技有限公司 Novel soldering tin purifying agent

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Denomination of invention: A slag remover and its preparation method

Effective date of registration: 20231228

Granted publication date: 20231103

Pledgee: Suzhou high tech Industrial Development Zone sub branch of Bank of Communications Co.,Ltd.

Pledgor: Ningcheng New Material Technology (Suzhou) Co.,Ltd.

Registration number: Y2023980074991