CN108655609A - A kind of high wetting water-based scaling powder and preparation method thereof - Google Patents
A kind of high wetting water-based scaling powder and preparation method thereof Download PDFInfo
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- CN108655609A CN108655609A CN201810341465.1A CN201810341465A CN108655609A CN 108655609 A CN108655609 A CN 108655609A CN 201810341465 A CN201810341465 A CN 201810341465A CN 108655609 A CN108655609 A CN 108655609A
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- scaling powder
- ether
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- based scaling
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Classifications
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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
-
- 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
Abstract
The present invention provides a kind of high wetting water-based scaling powders and preparation method thereof, are prepared by the raw material of following parts by weight：9 16 parts of dyhydrobutanedioic acid, 8 14 parts of β hydroxybutyric acids, 6 10 parts of malic acid, 36 parts of D-sorbite, 38 parts of polyoxyethylene lauryl ether, 25 parts of glycol dimethyl ether, 14 parts of polyoxyethylene lauryl ether, 24 parts of oleamide, 2,2,13 parts of 4 trimethyl, 1,3 pentanediol mono isobutyrate, 0.5 2 parts of triethanolamine, 25 parts of ethyl cellulose, 26 parts of corrosion inhibiter, 14 parts of film forming agent, 25 parts of bleeding agent, 47 parts of antioxidant, 8 18 parts of aqueous solution.Scaling powder wetting power prepared by the present invention is strong, while having good shear strength and corrosion resistance, to which the weldering property energy of scaling powder be greatly improved.Therefore the present invention is with a wide range of applications as a kind of high wetting water-based scaling powder.
Description
Technical field
The invention belongs to scaling powder technical fields, and in particular to a kind of high wetting water-based scaling powder and preparation method thereof.
Background technology
Due to environmental protection, prohibit the factors such as lead regulation and market competition and effectively facilitate, the research of novel lead-free solder at
For the hot spot of research.Wherein, Sn-9Zn alloys are since the fusing point with fusing point and tin-lead SnPb63 is closest, mechanical force
The advantages that performance is good, raw material easily obtain, relative low price is learned, one of most promising lead-free brazing is become.However tin zinc
It is that Zn is oxidized easily alloy in the welding process, and the wetability on Cu substrates is poorer than leypewter, this is in certain journey
The practical application of Sn-9Zn systems solder alloy is hindered on degree.Therefore, develop wettability significantly, adapt to environmental requirement and help weldering
Agent becomes the hot subject in pb-free solder field in recent years to improve the wetability of Sn-9Zn brazing filler metals.However existing scaling powder
Do not carry out excessive research on wettability, therefore in order to promote the application of Sn-9Zn alloys and improve weldability
It can, it is necessary to existing flux material further be developed, to improve the wettability of scaling powder.
Invention content
Above of the existing technology in order to solve the problems, such as, the purpose of the present invention is to provide a kind of high wettings water base to help weldering
Agent and preparation method thereof, to improve the wetability of scaling powder.
To achieve the goals above, the present invention provides following technical scheme：
A kind of high wetting water-based scaling powder, is prepared by the raw material of following parts by weight：9-16 parts of dyhydrobutanedioic acid, beta-hydroxy
8-14 parts of butyric acid, 6-10 parts of malic acid, 3-6 parts of D-sorbite, 3-8 parts of polyoxyethylene lauryl ether, glycol dimethyl ether 2-5
Part, 1-4 parts of polyoxyethylene lauryl ether, 2-4 parts of oleamide, 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates 1-3
Part, 0.5-2 parts of triethanolamine, 2-5 parts of ethyl cellulose, 2-6 parts of corrosion inhibiter, 1-4 parts of film forming agent, 2-5 parts of bleeding agent, antioxidant
4-7 parts, 8-18 parts of aqueous solution.
Preferably, a kind of high wetting water-based scaling powder of the present invention, is prepared by the raw material of following parts by weight：Two
12 parts of hydroxysuccinic acid, 9 parts of beta-hydroxy-butanoic acid, 8 parts of malic acid, 4.5 parts of D-sorbite, 5.5 parts of polyoxyethylene lauryl ether, second
3.5 parts of glycol dimethyl ether, 2.5 parts of polyoxyethylene lauryl ether, 3 parts of oleamide, 2,2,4- trimethyl -1,3- pentanediol lists
2 parts of isobutyrate, 1.5 parts of triethanolamine, 3.5 parts of ethyl cellulose, 4 parts of corrosion inhibiter, 2.5 parts of film forming agent, 3.5 parts of bleeding agent,
5.5 parts of antioxidant, 13 parts of aqueous solution.
Preferably, it is 1 that the corrosion inhibiter, which is mass ratio,:The 2- tolimidazoles and methyltriphenylphospbromide bromide phosphorus of 1-5.
Preferably, the film forming agent is the different octyl ether of ethylene glycol.
Preferably, it is 1-3 that the bleeding agent, which is mass ratio,:2 mannitol, dioctylsulfosuccinat.
Preferably, the antioxidant is butylated hydroxy anisole, di-iso-octyldiphenylamine or tert-butylhydroquinone.
Preferably, the molecular weight of the polyoxyethylene lauryl ether is 2000-8000.
The preparation method of high wetting water-based scaling powder of the present invention, includes the following steps：
（1）By dyhydrobutanedioic acid, beta-hydroxy-butanoic acid, malic acid, D-sorbite, polyoxyethylene lauryl ether, glycol dinitrate
In ether, polyoxyethylene lauryl ether, aqueous solution merging reaction vessel, it is slowly heated to 90-105 DEG C in the state of stirring,
This temperature is kept to continue to be stirred to react 40-60min and obtain mixture A；
（2）70-80 DEG C is cooled the temperature to, oleamide, 2,2,4- trimethyl -1,3- pentanediols are sequentially added into mixture A
Mono isobutyrate, triethanolamine, ethyl cellulose, continue stir 30-60min, be eventually adding corrosion inhibiter, film forming agent, bleeding agent,
Antioxidant is stirred to react 1.5-3h, is cooled to room temperature to obtain the final product.
Preferably, the speed of agitator in the reaction process is 300-500r/min.
Advantageous effect：The present invention provides a kind of high wetting water-based scaling powders and preparation method thereof, and prepared by the present invention helps
The wetting power of solder flux reaches 7.56mN（250℃）, shear strength reaches 65.31MPa, after salt spray corrosion test at solder joint 30 beyond the highest heavens
It sees unchanged, is obtained by the comparison with comparative example, bleeding agent plays an important role the wetability of scaling powder, while polyoxy
Ethylene lauryl ether plays auxiliary wetting effect to the wetability of scaling powder, and bleeding agent and polyoxyethylene lauryl ether are to helping
The wetting power of solder flux plays synergistic effect, while scaling powder has good shear strength and corrosion resistance, to be greatly improved
The weldering property energy of scaling powder.Therefore the present invention is with a wide range of applications as a kind of high wetting water-based scaling powder.
Specific implementation mode
The invention will now be further described with reference to specific embodiments, but examples are merely exemplary, not to this hair
Bright range constitutes any restrictions.It will be understood by those skilled in the art that without departing from the spirit and scope of the invention
Can the details and form of technical solution of the present invention be modified or be replaced, but these modifications and replacement each fall within the present invention's
In protection domain.
Embodiment 1
A kind of high wetting water-based scaling powder, is prepared by the raw material of following parts by weight：12 parts of dyhydrobutanedioic acid, beta-hydroxy fourth
9 parts of acid, 8 parts of malic acid, 4.5 parts of D-sorbite, 5.5 parts of polyoxyethylene lauryl ether, 3.5 parts of glycol dimethyl ether, polyoxy second
2,000 2.5 parts of alkene lauryl ether, 3 parts of oleamide, 2 parts of 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates, three second
It is 1.5 parts of hydramine, 3.5 parts of ethyl cellulose, 4 parts of corrosion inhibiter, 2.5 parts of film forming agent, 3.5 parts of bleeding agent, 5.5 parts of antioxidant, water-soluble
13 parts of liquid.
The corrosion inhibiter is that mass ratio is 1:3 2- tolimidazoles and methyltriphenylphospbromide bromide phosphorus.
The film forming agent is the different octyl ether of ethylene glycol.
The bleeding agent is that mass ratio is 1:1 mannitol, dioctylsulfosuccinat.
The antioxidant is butylated hydroxy anisole.
The preparation method of high wetting water-based scaling powder of the present invention, includes the following steps：
（1）By dyhydrobutanedioic acid, beta-hydroxy-butanoic acid, malic acid, D-sorbite, polyoxyethylene lauryl ether, glycol dinitrate
In ether, polyoxyethylene lauryl ether, aqueous solution merging reaction vessel, it is slowly heated to 100 DEG C in the state of stirring, keeps
This temperature, which continues to be stirred to react 50min, obtains mixture A；
（2）75 DEG C are cooled the temperature to, oleamide, 2,2,4- trimethyl -1,3- pentanediol Dan Yi are sequentially added into mixture A
Butyrate, triethanolamine, ethyl cellulose continue to stir 45min, are eventually adding corrosion inhibiter, film forming agent, bleeding agent, antioxidant
It is stirred to react 2.2h, is cooled to room temperature to obtain the final product.
Speed of agitator in the reaction process is 400r/min.
Embodiment 2
A kind of high wetting water-based scaling powder, is prepared by the raw material of following parts by weight：9 parts of dyhydrobutanedioic acid, beta-hydroxy fourth
8 parts of acid, 6 parts of malic acid, 3 parts of D-sorbite, 3 parts of polyoxyethylene lauryl ether, 2 parts of glycol dimethyl ether, polyoxyethylene 12
4,000 1 parts of alkyl ether, 2 parts of oleamide, 1 part of 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates, triethanolamine 0.5
Part, 2 parts of ethyl cellulose, 2 parts of corrosion inhibiter, 1 part of film forming agent, 2 parts of bleeding agent, 4 parts of antioxidant, 8 parts of aqueous solution.
The corrosion inhibiter is that mass ratio is 1:The 2- tolimidazoles and methyltriphenylphospbromide bromide phosphorus of 1-5.
The film forming agent is the different octyl ether of ethylene glycol.
The bleeding agent is that mass ratio is 1:2 mannitol, dioctylsulfosuccinat.
The antioxidant is di-iso-octyldiphenylamine.
The preparation method of high wetting water-based scaling powder of the present invention, includes the following steps：
（1）By dyhydrobutanedioic acid, beta-hydroxy-butanoic acid, malic acid, D-sorbite, polyoxyethylene lauryl ether, glycol dinitrate
In ether, polyoxyethylene lauryl ether, aqueous solution merging reaction vessel, it is slowly heated to 90 DEG C in the state of stirring, keeps
This temperature, which continues to be stirred to react 40min, obtains mixture A；
（2）70 DEG C are cooled the temperature to, oleamide, 2,2,4- trimethyl -1,3- pentanediol Dan Yi are sequentially added into mixture A
Butyrate, triethanolamine, ethyl cellulose continue to stir 30min, are eventually adding corrosion inhibiter, film forming agent, bleeding agent, antioxidant
It is stirred to react 1.5h, is cooled to room temperature to obtain the final product.
Speed of agitator in the reaction process is 300r/min.
Embodiment 3
A kind of high wetting water-based scaling powder, is prepared by the raw material of following parts by weight：12 parts of dyhydrobutanedioic acid, beta-hydroxy fourth
10 parts of acid, 7 parts of malic acid, 4 parts of D-sorbite, 4 parts of polyoxyethylene lauryl ether, 3 parts of glycol dimethyl ether, polyoxyethylene 12
6,000 2 parts of alkyl ether, 2.5 parts of oleamide, 1.5 parts of 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates, triethanolamine 1
Part, 3 parts of ethyl cellulose, 3 parts of corrosion inhibiter, 2 parts of film forming agent, 3 parts of bleeding agent, 5 parts of antioxidant, 10 parts of aqueous solution.
The corrosion inhibiter is that mass ratio is 1:2 2- tolimidazoles and methyltriphenylphospbromide bromide phosphorus.
The film forming agent is the different octyl ether of ethylene glycol.
The bleeding agent is that mass ratio is 1.5:2 mannitol, dioctylsulfosuccinat.
The antioxidant is tert-butylhydroquinone.
The preparation method of high wetting water-based scaling powder of the present invention, includes the following steps：
（1）By dyhydrobutanedioic acid, beta-hydroxy-butanoic acid, malic acid, D-sorbite, polyoxyethylene lauryl ether, glycol dinitrate
In ether, polyoxyethylene lauryl ether, aqueous solution merging reaction vessel, it is slowly heated to 95 DEG C in the state of stirring, keeps
This temperature, which continues to be stirred to react 45min, obtains mixture A；
（2）72 DEG C are cooled the temperature to, oleamide, 2,2,4- trimethyl -1,3- pentanediol Dan Yi are sequentially added into mixture A
Butyrate, triethanolamine, ethyl cellulose continue to stir 40min, are eventually adding corrosion inhibiter, film forming agent, bleeding agent, antioxidant
It is stirred to react 2h, is cooled to room temperature to obtain the final product.
Speed of agitator in the reaction process is 350r/min.
Embodiment 4
A kind of high wetting water-based scaling powder, is prepared by the raw material of following parts by weight：16 parts of dyhydrobutanedioic acid, beta-hydroxy fourth
14 parts of acid, 10 parts of malic acid, 6 parts of D-sorbite, 8 parts of polyoxyethylene lauryl ether, 5 parts of glycol dimethyl ether, polyoxyethylene ten
8,000 4 parts of dialkyl ether, 4 parts of oleamide, 3 parts of 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates, triethanolamine 2
Part, 5 parts of ethyl cellulose, 6 parts of corrosion inhibiter, 4 parts of film forming agent, 5 parts of bleeding agent, 7 parts of antioxidant, 18 parts of aqueous solution.
The corrosion inhibiter is that mass ratio is 1:5 2- tolimidazoles and methyltriphenylphospbromide bromide phosphorus.
The film forming agent is the different octyl ether of ethylene glycol.
The bleeding agent is that mass ratio is 3:2 mannitol, dioctylsulfosuccinat.
The antioxidant is butylated hydroxy anisole, di-iso-octyldiphenylamine or tert-butylhydroquinone.
The preparation method of high wetting water-based scaling powder of the present invention, includes the following steps：
（1）By dyhydrobutanedioic acid, beta-hydroxy-butanoic acid, malic acid, D-sorbite, polyoxyethylene lauryl ether, glycol dinitrate
In ether, polyoxyethylene lauryl ether, aqueous solution merging reaction vessel, it is slowly heated to 105 DEG C in the state of stirring, keeps
This temperature, which continues to be stirred to react 60min, obtains mixture A；
（2）80 DEG C are cooled the temperature to, oleamide, 2,2,4- trimethyl -1,3- pentanediol Dan Yi are sequentially added into mixture A
Butyrate, triethanolamine, ethyl cellulose continue to stir 60min, are eventually adding corrosion inhibiter, film forming agent, bleeding agent, antioxidant
It is stirred to react 3h, is cooled to room temperature to obtain the final product.
Speed of agitator in the reaction process is 500r/min.
Comparative example 1
Difference lies in be not added with polyoxyethylene lauryl ether to comparative example 1 in comparative example 1 with embodiment 1.
Comparative example 2
Difference lies in comparative example 2 is not added with bleeding agent to comparative example 2 with embodiment 1.
The scaling powder that embodiment 1-4 and comparative example 1-2 are prepared carries out wetting power, shear strength, corrosion resistance test,
Wetting power test is carried out according to IPC J-STD-004A standards, shear strength, corrosion resistance test are respectively according to national standard GB 11363-
89 soldering joint strength test methods and GB6458-86 metal cladding neutral salt spray test methods carry out.Performance test knot
Fruit is as shown in table 1, is obtained from table 1, and the wetting power of scaling powder prepared by the present invention reaches 7.56mN（250℃）, shear strength
Reach 65.31MPa, 30 days appearances are unchanged at solder joint after salt spray corrosion test, obtained by the comparison with comparative example, bleeding agent
The wetability of scaling powder is played an important role, while polyoxyethylene lauryl ether plays auxiliary to the wetability of scaling powder
Wetting effect, bleeding agent and polyoxyethylene lauryl ether play synergistic effect to the wetting power of scaling powder, to be greatly improved
The weldering property energy of scaling powder.
Table 1
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 |
| Wetting power | 7.56 | 5.04 | 5.62 | 6.53 | 4.89 | 4.28 |
| Shear strength（MPa） | 65.31 | 42.57 | 46.95 | 53.26 | 63.84 | 62.45 |
| Salt air corrosion（NaCl aqueous solutions, 5g/L） | Appearance is unchanged within 30 days | Appearance is unchanged within 30 days | Appearance is unchanged within 30 days | Appearance is unchanged within 30 days | Appearance is unchanged within 30 days | Appearance is unchanged within 30 days |
Claims (9)
1. a kind of high wetting water-based scaling powder, which is characterized in that be prepared by the raw material of following parts by weight：Dyhydrobutanedioic acid
9-16 parts, 8-14 parts of beta-hydroxy-butanoic acid, 6-10 parts of malic acid, 3-6 parts of D-sorbite, 3-8 parts of polyoxyethylene lauryl ether, second two
2-5 parts of diethylene glycol dimethyl ether, 1-4 parts of polyoxyethylene lauryl ether, 2-4 parts of oleamide, 2,2,4- trimethyl -1,3- pentanediol lists
1-3 parts of isobutyrate, 0.5-2 parts of triethanolamine, 2-5 parts of ethyl cellulose, 2-6 parts of corrosion inhibiter, 1-4 parts of film forming agent, bleeding agent
2-5 parts, 4-7 parts of antioxidant, 8-18 parts of aqueous solution.
2. a kind of high wetting water-based scaling powder according to claim 1, which is characterized in that by the raw material system of following parts by weight
It is standby to form：12 parts of dyhydrobutanedioic acid, 9 parts of beta-hydroxy-butanoic acid, 8 parts of malic acid, 4.5 parts of D-sorbite, polyoxyethylene lauryl
5.5 parts of ether, 3.5 parts of glycol dimethyl ether, 2.5 parts of polyoxyethylene lauryl ether, 3 parts of oleamide, trimethyl -1 2,2,4-,
2 parts of 3- pentanediol mono isobutyrates, 3.5 parts of ethyl cellulose, 4 parts of corrosion inhibiter, 2.5 parts of film forming agent, ooze 1.5 parts of triethanolamine
Saturating 3.5 parts of agent, 5.5 parts of antioxidant, 13 parts of aqueous solution.
3. a kind of high wetting water-based scaling powder according to claim 1, which is characterized in that the corrosion inhibiter is that mass ratio is
1:The 2- tolimidazoles and methyltriphenylphospbromide bromide phosphorus of 1-5.
4. a kind of high wetting water-based scaling powder according to claim 1, which is characterized in that the film forming agent is that ethylene glycol is different
Octyl ether.
5. a kind of high wetting water-based scaling powder according to claim 1, which is characterized in that the bleeding agent is that mass ratio is
1-3:2 mannitol, dioctylsulfosuccinat.
6. a kind of high wetting water-based scaling powder according to claim 1, which is characterized in that the antioxidant is butylhydroxy
Anisole, di-iso-octyldiphenylamine or tert-butylhydroquinone.
7. a kind of high wetting water-based scaling powder according to claim 1, which is characterized in that the polyoxyethylene lauryl base
The molecular weight of ether is 2000-8000.
8. claim 1-7 any one of them height soaks the preparation method of water-based scaling powder, which is characterized in that including following step
Suddenly：
（1）By dyhydrobutanedioic acid, beta-hydroxy-butanoic acid, malic acid, D-sorbite, polyoxyethylene lauryl ether, glycol dinitrate
In ether, polyoxyethylene lauryl ether, aqueous solution merging reaction vessel, it is slowly heated to 90-105 DEG C in the state of stirring,
This temperature is kept to continue to be stirred to react 40-60min and obtain mixture A；
（2）70-80 DEG C is cooled the temperature to, oleamide, 2,2,4- trimethyl -1,3- pentanediols are sequentially added into mixture A
Mono isobutyrate, triethanolamine, ethyl cellulose, continue stir 30-60min, be eventually adding corrosion inhibiter, film forming agent, bleeding agent,
Antioxidant is stirred to react 1.5-3h, is cooled to room temperature to obtain the final product.
9. the preparation method of high wetting water-based scaling powder according to claim 8, which is characterized in that in the reaction process
Speed of agitator be 300-500r/min.
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| CN107186387A (en) * | 2017-06-28 | 2017-09-22 | 合肥市闵葵电力工程有限公司 | A kind of cleaning-free lead-free solder soldering fluid and preparation method thereof |
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2018
- 2018-04-17 CN CN201810341465.1A patent/CN108655609A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350599A (en) * | 2011-08-25 | 2012-02-15 | 华南理工大学 | Halogen-free high-impedance water-based washing-free scaling powder as well as preparation method and application thereof |
| CN103521952A (en) * | 2012-07-06 | 2014-01-22 | 重庆微世特电子材料有限公司 | Welding-bonding dual-purpose halogen-free electronic addition agent and preparation method thereof |
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